A polyolefin composition suitable for preparing single ply roofing membranes, comprising:

The present invention concerns polyolefin compositions having improved tenacity, while retaining softness and good mechanical properties, which can be advantageously used in flat sheet material, such as single ply roofing membranes for covering industrial and commercial flat roofs, and in other roofing applications. These compositions may be obtained by a sequential polymerization process.
Traditionally, the building industry has utilized conventional built-up asphalt or fiber glass roofing as a preferred material in roofing construction. More recently, however, membrane roofing materials have displaced the conventional materials as a preferred material due to their cold cracking resistance, ease of installation, and overall improved and increased leak protection over time. Further, the membrane systems are easier and safer to install and are therefore more desirable to the contractor as well as the consumer.
Two membrane types are utilized in this field: thermoplastic and elastomeric.
Thermoplastic membranes, such as those formed from polyvinyl chloride (PVC), chlorinated polyethylene (CPE), chlorosulfonated polyethylene and the like, can be heat sealed or solvent welded to provide dependable seals of higher strength; however, these membranes also have serious disadvantages. For example, the thermoplastic material must be plasticized to provide the flexibility necessary for a roofing membrane, and plasticizers are quite expensive and leach out of the membrane over time thus resulting in the loss of flexibility, embrittlement and decreased cold crack resistance of the membrane. Further, the capacity of the thermoplastic materials to accept fillers is limited.
Moreover, there is a need for a PVC sheeting alternative, in view of the trend toward a chlorine-free environment.
Elastomeric membranes, such as vulcanized ethylene/propylene/diene terpolymers EPDM rubbers, has been rapidly gaining acceptance, because of outstanding weathering resistance and flexibility. This material normally is prepared by vulcanizing the composition in the presence of sulfur or sulfur containing compounds.
However, these membranes are difficult to seal, due to the lack of adhesion of EPDM, especially cured EPDM, to itself, and require an adhesive for seaming the membrane in order to provide a leak-free, continuous roofing cover. These adhesives add a significant material cost and are difficult and time-consuming to apply. Further, the adhesives often weaken over time, causing delamination of the membranes and subsequent leaks in the roofing cover. Elastomeric membranes also require an additional costly curing step.
In order to avoid the curing procedure, in the state of the art it was proposed to use sheeting materials for roofing applications comprising an EPDM in combination with highly crystalline thermoplasticity promoters, such as high density polyethylene (HDPE), low density polyethylene (LDPE) and other similar olefin type polymers. For instance, U.S. Pat. No. 5,256,228 discloses a heat seamable sheet material for roofing, prepared from an uncured polymeric composition which comprises 100 parts by weight of a polymer blend comprising from 50 to 90 parts by weight of polyolefins having up to 2 percent by weight crystallinity, and from 10 to 50 parts by weight of a highly crystalline thermoplasticity promoter such as HDPE or LDPE; 50-250 parts by weight of a filler; and 20-150 parts by weight of a processing material.
Nevertheless, the presence of crystalline polyethylene resins have many disadvantages. For instance, higher crystallinity levels result in less thermal dimensional stability, expansion or contraction over large temperature ranging observed in the field; this may result in bucking or stress on the sheet. Moreover, the lower melting characteristics of polyethylene result in limitations for applications at elevated temperatures, such as in dark colored sheet. Finally, polyethylene has a narrow melting point range, which results in a narrow heat welding process window.
Polyolefin compositions having good mechanical properties have been used in many application fields, due to the characteristics which are typical of polyolefins (such as chemical inertia, mechanical properties and nontoxicity); moreover, these compositions show outstanding cost/performance ratios. In the state of the art, these compositions have been obtained by way of sequential copolymerization of propylene, optionally containing minor quantities of olefin comonomers, and then ethylene/propylene or ethylene/alpha-olefin mixtures. Catalysts based on halogenated titanium compounds supported on magnesium chloride are commonly used for this purpose.
For instance, U.S. Pat. No. 5,286,564, in the name of the same Applicants, describes flexible polyolefin compositions comprising, in parts by weight:
A) 10-50 parts of an isotactic propylene homopolymer or copolymer;
B) 5-20 parts of an ethylene copolymer, insoluble in xylene at room temperature; and
C) 40-80 parts of an ethylene/propylene copolymer containing less than 40% by weight of ethylene and being soluble in xylene at room temperature; the intrinsic viscosity of said copolymer is preferably from 1.7 to 3 dl/g.
Said compositions have flexural modulus values of less than 150 MPa and Shore D hardness between 20 and 35. Although these mechanical properties are advantageous for certain applications, the compositions prepared in Examples 1-5 show values of Tensile Strength at Break ranging from 13.8 to 17.3 MPa; for many applications, such as in roofing sheets, these polymers do not show a satisfactory tenacity, which is a property strictly related to tensile strength at break and to elongation at break properties. Tenacity is fundamental in roofing applications, wherein there is the tendency of roofing to break under the action of the wind.
As it is well known in the art, the strength and flexibility of thermoplastic polyolefin compositions may be enhanced decreasing the rubber content; nevertheless, to the increase in strength is usually associated an increase in stiffness that causes various drawbacks. For instance, the increase in stiffness of a flexible membrane limits the installation of the membrane around corner, chimneys, vents etc., where the membrane must be flexible to bend around the obstruction.
The European Patent Application No. 1202876.7, in the name of the same Applicants, describes a polyolefin composition comprising:
(A) from 8 to 25% by weight of a crystalline propylene homopolymer or copolymer; and
(B) from 75 to 92% by weight of an elastomeric fraction comprising a first elastomeric copolymer of propylene with 15-32% wt ethylene, the intrinsic viscosity of the xylene soluble fraction ranging from 3.0 to 5.0 dl/g; and a second elastomeric copolymer of propylene with more than 32% up to 45% wt. of ethylene, the intrinsic viscosity of the xylene soluble fraction ranging from 4.0 to 6.5 dl/g.
These polyolefin compositions have flexural modulus values lower than 60 MPa and very good hardness values (Shore A hardness lower than 90); nevertheless, they exhibit low tenacity values. In fact, the polyolefin compositions prepared in Examples 1-3 of the above-mentioned application show values of Tensile Strength at Break equal to 5.5, 11.7 and 11.2 MPa respectively. As reported above, such values are not fully satisfactory for roof sheeting, since the increase in flexibility is associated to an enhanced stiffniess.
A strong need therefore exists for softer materials which are easier to install, and at the same time possess a satisfactory tenacity, strength, and tear and puncture resistance. In other words, it is felt the need for polyolefin compositions which exhibit a good balance of flexibility over a variable temperature range, and tenacity, as well as good mechanical properties; moreover, these compositions must be heat-sealable and oil-resistant and must not undergo degradation when exposed to the elements.
The present invention concerns a polyolefin composition comprising:
(A) from about 15 to about 40% by weight of a crystalline copolymer of propylene with at least one alpha-olefin of formula H2Cxe2x95x90CHR1, where R1 is H or a C2xe2x88x928 linear or branched alkyl, containing at least about 90% by weight of propylene, and having solubility in xylene at room temperature lower than about 15% by weight;
(B) from about 60 to about 85% by weight of an elastomeric fraction comprising:
(1) a copolymer of propylene with ethylene, optionally containing about 0.5 to 5% by weight of a diene, containing from about 20 to about 35% by weight ethylene, and having solubility in xylene at room temperature greater than about 70% by weight, the intrinsic viscosity of the xylene soluble fraction being higher than about 3.0 dl/g up to about 6.0 dl/g; and
(2) a copolymer of ethylene with at least one alpha-olefin of formula H2Cxe2x95x90CHR2, where R2 is a C2xe2x88x928 linear or branched alkyl, optionally containing about 0.5 to 5% by weight of a diene, containing about 15% to 40% by weight alpha-olefin, and having solubility in xylene at room temperature greater than about 25% by weight, the intrinsic viscosity of the xylene soluble fraction ranging from about 0.5 to about 5.0 dl/g;
the (1)/(2) weight ratio ranging from about 1:5 to about 5:1.
The present invention further concerns a process for the preparation of the polyolefin composition reported above, comprising at least three sequential polymerization stages, with each subsequent polymerization being conducted in the presence of the polymeric material formed in the immediately preceding polymerization reaction, wherein the crystalline copolymer (A) is prepared in a first stage, and the elastomeric fraction (B) is prepared in at least two subsequent stages. According to a preferred embodiment, all the polymerization stages are carried out in the presence of a catalyst comprising a trialkylaluminum compound, optionally an electron donor, and a solid catalyst component comprising a halide, or halogen-alcoholate of Ti, and an electron donor compound supported on anhydrous magnesium chloride, said solid catalyst component having a surface area (measured by BET) of less than about 200 m2/g, and a porosity (measured by BET) higher than about 0.2 ml/g.
The polyolefin compositions of the present invention show a significant improvement in strength and toughness, without sacrificing stiffness; on the opposite, applicants have surprisingly found that the stiffness of the compositions of the invention is reduced with respect to prior art compositions containing lower amounts of rubber content. More specifically, the compositions of the invention are endowed with high tenacity, as evidenced by the values of tensile strength at break and elongation at break much higher than the ones of the prior art thermoplastic resins used in flexible roofing membranes, at the same time showing a remarkable reduction in stiffness.
The compositions of the invention exhibit a very good balance of flexibility and mechanical properties, and in particular of flexural modulus values and Shore D hardness, at the same time retaining good elastomeric properties. These soft compositions, easier to install even around corners and chimneys, show better strength and tear resistance, as well as improved wind uplift and puncture resistance; moreover, they are endowed with long term weldability.
The polyolefin compositions of the present invention comprise from about 15 to about 40% by weight, preferably from about 15 to about 35%, and even more preferably from about 20 to about 30%, of a crystalline copolymer of propylene (A), and from about 60 to about 85% by weight, preferably from about 65 to about 85%, and even more preferably from about 70 to about 80% by weight of an elastomeric fraction (B).
In the present description, by xe2x80x9croom temperaturexe2x80x9d is meant approximately 25xc2x0 C.
The crystalline copolymer (A) of the compositions of the invention is a copolymer of propylene with an alpha-olefin H2Cxe2x95x90CHR1, where R1 is H or a C2xe2x88x928 linear or branched alkyl, containing at least about 90% by weight of propylene, preferably at least about 95% propylene. This copolymer has solubility in xylene at room temperature lower than about 15% by weight, preferably lower than about 10%, and even more preferably lower than about 8%. Said alpha-olefin is preferably ethylene, 1-butene, 1-pentene, 4-methylpentene, 1-hexene, 1-octene or combinations thereof, and even more preferably it is ethylene.
The elastomeric fraction (B) of the polyolefin compositions of the invention comprises a copolymer of propylene with ethylene, and a copolymer of ethylene with an alpha-olefin H2Cxe2x95x90CHR2, where R2 is a linear or branched C2xe2x88x928 alkyl. By xe2x80x9celastomenrcxe2x80x9d is meant herein a polymer having low cristallinity or amorphous, and having a solubility in xylene at room temperature greater than about 40% by weight.
The copolymer (1) of propylene with ethylene contains from about 20 to about 35% by weight of ethylene, preferably from about 25 to about 30%, and has a solubility in xylene at room temperature greater than about 70% by weight, preferably greater than about 75%; the intrinsic viscosity of the xylene soluble fraction ranges from about 3.0 to about 6.0 dl/g, more preferably from about 3.5 to about 5.0 dl/g, and even more preferably from about 4.0 to about 4.5 dl/g.
The copolymer (2) is a copolymer of ethylene with at least one alpha olefin of formula H2Cxe2x95x90CHR2, where R2 is a C2xe2x88x928 linear or branched alkyl, optionally containing about 0.5 to 5% by weight of a diene; said alpha-olefin is preferably 1-butene, 1-hexene or 1-octene, and even more preferably is 1-butene. The alpha-olefin content ranges from about 15% to about 40% by weight, and preferably from about 20 to about 35%. The copolymer (2) has solubility in xylene at room temperature greater than about 25% by weight, preferably greater than about 30%, and the intrinsic viscosity of the xylene soluble fraction ranges from about 0.5 to about 5.0 dl/g, preferably from about 1.0 to about 4.5 dl/g.
As previously reported, the copolymers (1) and (2) of the elastomeric fraction (B) may contain a diene, conjugated or not, such as butadiene, 1,4-hexadiene, 1,5-hexadiene and ethylidene-norbornene-1. The diene, when present, is contained in an amount of from about 0.5 to about 5% by weight, with respect to the weight of the fraction (B).
The weight ratio of the elastomeric copolymers (1)/(2) ranges from about 1:5 to about 5:1, and preferably from about 1:2 to about 2:1.
The polyolefin composition of the invention, preferably prepared by sequential polymerization in at least three stages, shows high tenacity, and in particular has tensile strength at break 25 MPa (ASTM D 882, on a 100 xcexcm film), more preferably xe2x89xa728 MPa; elongation at break 700 MPa (ASTM D 882, on a 100 xcexcm film), more preferably xe2x89xa7750 MPa; and toughness 150 MPa (ASTM D 638, on a 1 mm sheet), more preferably 170 MPa.
Moreover, said composition has a flexural modulus 130 MPa, preferably 100 MPa, and more preferably 80 MPa; Shore D hardness 40xc2x0 S, and preferably ranging from about 25 to about 35; and MFR  less than 1.0 g/10 min, preferably  less than 0.8 g/10 min, and even more preferably  less than 0.6 g/10 min.
According to a preferred embodiment of the invention, the polyolefin composition is in the form of spherical particles having an average diameter of about 250 to about 7,000 microns, a flowability of less than about 30 seconds and a bulk density (compacted) greater than about 0.4 g/ml.
The polyolefin composition of the invention may be prepared by sequential polymerization in at least three stages; according to a preferred embodiment, the sequential polymerization is carried out in the presence of a catalyst comprising a trialkylaluminum compound, optionally an electron donor, and a solid catalyst component comprising a halide or halogen-alcoholate of Ti, and an electron-donor compound supported on anhydrous magnesium chloride.
The present invention is further directed to a process for the preparation of the polyolefin compositions as reported above, said process comprising at least three sequential polymerization stages with each subsequent polymerization being conducted in the presence of the polymeric material formed in the immediately preceding polymerization reaction, wherein the crystalline copolymer (A) is prepared in at least one first stage, and the elastomeric fraction (B) is prepared in at least two sequential stages. The polymerization stages may be carried out in the presence of a Ziegler-Natta and/or a metallocene catalyst.
Suitable Ziegler-Natta catalysts are described in EP-A-45 977 and U.S. Pat. No. 4,399,054, incorporated herein by reference; other examples can be found in U.S. Pat. No. 4,472,524, incorporated herein by reference.
The solid catalyst components used in said catalysts comprise, as electron-donors (internal donors), compounds selected from the group consisting of ethers, ketones, lactones, compounds containing N, P and/or S atoms, and esters of mono- and dicarboxylic acids.
Particularly suitable electron-donor compounds are phthalic acid esters, such as diusobutyl, dioctyl, diphenyl and benzylbutyl phthalate.
Other suitable electron-donors are 1,3-diethers of formula:
wherein RI and RII, the same or different from each other, are C1-C18 alkyl, C3-C18 cycloalkyl or C7-C18 aryl radicals; RIII and RIV, the same or different from each other, are C1-C4 alkyl radicals; or are the 1,3-diethers in which the carbon atom in position 2 belongs to a cyclic or polycyclic structure made up of 5, 6 or 7 carbon atoms and containing two or three unsaturations.
Ethers of this type are described in EP-A-361 493 and EP-A-728 769.
Representative examples of said dieters are 2-methyl-2-isopropyl-1,3-dimethoxypropane, 2,2-diisobutyl-1,3-dimethoxypropane, 2-isopropyl-2-cyclopentyl-1,3-dimethoxypropane, 2-isopropyl-2-isoamyl-1,3-dimethoxypropane, and 9,9-bis(methoxymethyl)fluorene.
The preparation of the above mentioned catalyst components is carried out according to various methods.
According to a preferred method of preparation, a MgCl2.nROH adduct (in particular in the form of spheroidal particles) wherein n is generally from 1 to 3 and ROH is ethanol, butanol or isobutanol, is reacted with an excess of TiCl4 containing the electron-donor compound. The reaction temperature is generally from 80 to 120xc2x0 C. The solid is then isolated and reacted once more with TiCl4, in the presence or absence of the electron-donor compound, after which it is separated and washed with aliquots of a hydrocarbon until all chlorine ions have disappeared.
In the solid catalyst component the titanium compound, expressed as Ti, is generally present in an amount from about 0.5 to about 10% by weight. The quantity of electron-donor compound which remains fixed on the solid catalyst component generally is about 5 to 20% by moles with respect to the magnesium dihalide.
The titanium compounds which can be used in the preparation of the solid catalyst component are the halides and the halogen alcoholates of titanium. Titanium tetrachloride is the preferred compound.
The reactions described above result in the formation of a magnesium halide in active form. Other reactions are known in the literature, which cause the formation of magnesium halide in active form starting from magnesium compounds other than halides, such as magnesium carboxylates.
The Al-alkyl compounds used as co-catalysts comprise Al-trialkyls, such as Al-triethyl, Al-triisobutyl, Al-tri-n-butyl, and linear or cyclic Al-alkyl compounds containing two or more Al atoms bonded to each other by way of O or N atoms, SO4 or SO3 groups. The Al-alkyl compound is generally used in such a quantity that the Al/Ti ratio be from about 1 to about 1000.
The electron-donor compounds that can be used as external donors include aromatic acid esters such as alkyl benzoates, and in particular silicon compounds containing at least one Sixe2x80x94OR bond, where R is a hydrocarbon radical. Examples of silicon compounds are (tert-butyl)2Si(OCH3)2, (cyclohexyl)(methyl)Si(OCH3)2, (phenyl)2Si(OCH3)2 and (cyclopentyl)2Si(OCH3)2. 1,3-diethers having the formulae described above can also be used advantageously. If the internal donor is one of these dieters, the external donors can be omitted.
The solid catalyst component have preferably a surface area (measured by BET) of less than about 200 m2/g, and more preferably ranging from about 80 to about 170 m2/g, and a porosity (measured by BET) preferably greater than about 0.2 ml/g, and more preferably from about 0.25 to about 0.5 ml/g.
The catalysts may be precontacted with small quantities of olefin (prepolymerization), maintaining the catalyst in suspension in a hydrocarbon solvent, and polymerizing at temperatures from ambient to 60xc2x0 C., thus producing a quantity of polymer from about 0.5 to about 3 times the weight of the catalyst. The operation can also take place in liquid monomer, producing, in this case, a quantity of polymer 1000 times the weight of the catalyst.
By using the above-mentioned catalysts, the polyolefin compositions are obtained in spheroidal particle form, the particles having an average diameter from about 250 to about 7,000 microns, a flowability of less than about 30 seconds and a bulk density (compacted) greater than about 0.4 g/ml.
Other catalysts that may be used in the process according to the present invention are metallocene-type catalysts, as described in EP-A-0 129 368 and U.S. Pat. No. 5,324,800, incorporated herein by reference; particularly advantageous are bridged bis-indenyl metallocenes, for instance as described in EP-A-0 485 823 and U.S. Pat. No. 5,145,819, incorporated herein by reference. Another class of suitable catalysts are the so-called constrained geometry catalysts, as described in EP-A-0 416 815, EP-A-0 420 436, EP-A-0 671 404, EP-A-0 643 066 and WO 91/04257. These metallocene compounds may be used to produce the copolymers (1) and (2) of the elastomeric fraction (B).
According to a preferred embodiment, the polymerization process of the invention comprises three stages, all carried out in the presence of Ziegler-Natta catalysts, where: in the first stage the relevant monomer(s) are polymerized to form the crystalline copolymer (A); in the second stage a mixture of propylene and ethylene, and optionally a diene are polymerized to form the copolymer (B)(1); and in the third stage a mixture of ethylene and an alpha-olefin H2Cxe2x95x90CHR2, and optionally a diene, are polymerized to form the copolymer (B)(2).
The polymerization stages may occur in liquid phase, in gas phase or liquid-gas phase. Preferably, the polymerization of the crystalline copolymer fraction (A) is carried out in liquid monomer (e.g. using liquid propylene as diluent), while the copolymerization stages of the copolymers (B)(1) and (B)(2) are carried out in gas phase, without intermediate stages except for the partial degassing of the propylene. According to a most preferred embodiment, all the three sequential polymerization stages are carried out in gas phase.
The reaction temperature in the polymerization stage for the preparation of the crystalline copolymer (A) and in the preparation of the copolymers (B)(1) and (B)(2) can be the same or different, and is preferably from about 40xc2x0 C. to about 90xc2x0 C.; more preferably, the reaction temperature ranges from about 50 to about 80xc2x0 C. in the preparation of the fraction (A), and from about 40 to about 80xc2x0 C. for the preparation of components (B)(1) and (B)(2).
The pressure of the polymerization stage to prepare the fraction (A), if carried out in liquid monomer, is the one which competes with the vapor pressure of the liquid propylene at the operating temperature used, and is possibly modified by the vapor pressure of the small quantity of inert diluent used to feed the catalyst mixture, and the overpressure of the monomers and the hydrogen optionally used as molecular weight regulator.
The polymerization pressure preferably ranges from about 33 to about 43 bar, if done in liquid phase, and from about 5 to about 30 bar if done in gas phase. The residence times of the three stages depend on the desired ratio between the fractions, and can range from about 15 minutes to 8 hours. Conventional molecular weight regulators known in the art, such as chain transfer agents (e.g. hydrogen or ZnEt2), may be used.
The compositions of the invention may be used in combination with other elastomeric polymers, such as ethylene/propylene copolymers (EPR), ethylene/ propylene/diene terpolymers (EPDM), copolymers of ethylene with C4-C12 alpha-olefins (e.g. ethylene/octene-1 copolymers, such as the ones commercialized under the name Engage(copyright)) and mixtures thereof. Such elastomeric polymers may be present in an amount of 5 to 80% by weight on the total composition.
In addition to its polymer components, the composition of the present invention can be blended with common additives, such as reinforcing and non-reinforcing fillers, pigments, nucleating agents, extension oils, mineral fillers, flame retardants (e.g. aluminum trihydrate), antioxidants, UV resistants (e.g. titanium dioxide), UV stabilizers, lubricants (e.g., oleamide), antiblocking agents, antistatic agents, waxes, coupling agents for fillers and other processing aids known in the polymer compounding art. The pigments and other additives may comprise up to about 50 weight percent of the total composition based on polymer components plus additives; preferably pigments and fillers comprise above about 0 to about 30 weight percent of the total composition.
In view of the properties described above, the polyolefin compositions of the present invention are valuable in the production of roofing membranes for covering industrial and commercial flat roofs, and in other roofing applications. In fact, they possess a high tenacity, while retaining softness and good mechanical properties.
Moreover, the roofing membranes obtained with the polyolefin compositions of the invention are weatherproof, inexpensive to manufacture, and durable, having an average life far greater than that of current commercial roofing shingles which are made using fiberglass or asphalt.
Roofing membranes formed from the polyolefin compositions of the present invention may be produced by any method conventionally used for producing roofing membranes from filled polymer compositions. For example, the membranes may be formed by conventional milling, calendering or extrusion techniques. Other methods, including spray coating and roller die forming, may be used. According to a preferred embodiment, the polymeric compositions of the invention are sheeted to thickness ranging from about 5 to about 200 mils. The sheeting can be cut to desired length and width dimensions at this time.
Roofing membranes formed from the compositions of the present invention may optionally be scrim reinforced. Besides roofing membranes, the polyolefin compositions of this invention may be used to produce underlay materials, used as replacements for roofing felt.
Roofing membranes can be applied in the same manner and circumstances as conventional asphaltic or fiberglass membranes. They have light weight, providing potential cost savings in the design of structural roof supports, as well as ease of application. They provide outstanding strength and durability, together with excellent temperature stability, weatherability and resiliency.
A method for covering a roof comprises the steps of applying sheets of the polymeric material of the invention to the roof being covered; overlapping adjacent edges of the layers; heating the overlapped areas to slightly above the softening point of the sheet material and seaming the overlapped areas using heat and under sufficient pressure to provide an acceptable seam strength. The polymeric compositions have sufficient self-adhesion without the use of an adhesive.
The following analytical methods have been used to determine the properties reported in the detailed description and in the examples.
Determination of Xylene Solubility at Room Temperature (% by weight):
2.5 g of polymer were dissolved in 250 ml of xylene, at 135xc2x0 C., under agitation. After 20 minutes, the solution was cooled to 25xc2x0 C. under stirring, and then it was allowed to settle for 30 minutes.
The precipitate was filtered with filter paper; the solution was evaporated under a nitrogen current, and the residue dried under vacuum at 80xc2x0 C. until reached constant weight. The weight percentage of polymer soluble in xylene at room temperature was then calculated. The percent by weight of polymer insoluble in xylene at room temperature was considered the isotactic index of the polymer. This value corresponded substantially to the isotactic index determined by extraction with boiling n-heptane, which by definition constitutes the isotactic index of polypropylene.
Unless otherwise specified, the samples to be subjected to the various physical-mechanical analyses were molded by use of a Negri and Bossi injection press 90, after stabilizing the sample with IRGANOX R 1010 hindered phenolic stabilizer (0.05% by weight), and IRGAFOS 168 phosphite stabilizer (0.1% by weight), and pelletizing the sample with a twin-screw Berstorff extruder (barrel diameter 25 mm) at 210xc2x0 C.
The conditions were as follows:
temperature of the melt: 220xc2x0 C.;
temperature of the mold: 60xc2x0 C.;
injection time: 9 sec;
cooling time: 15 sec.
The dimensions of the plaques for the tests were 127xc3x97127xc3x972.5 mm. From these plaques, C-type dumbbells were cut and submitted to tensile strength tests with a head speed of 500 mm/min. Also the specimens for the flexural modulus and hardness Shore D were cut from these plaques. All the specimens were cut parallel to the advancement front and consequently perpendicular to the flow direction.

Polyolefin compositions having high tenacity

Abstract: (A) from about 15 to about 40% by weight of a crystalline copolymer of propylene with at least one alpha-olefin of formula H2Cxe2x95x90CHR1, where R1 is H or a C2xe2x88x928 linear or branched alkyl, containing at least about 90% by weight of propylene, having solubility in xylene at room temperature lower than about 15% by weight;

Abstract: (1) a copolymer of propylene with ethylene containing about 20 to about 35% by weight ethylene, and having solubility in xylene at room temperature greater than about 70% by weight, the intrinsic viscosity of the xylene soluble fraction being higher than about 3.0 dl/g up to about 6.0 dl/g; and

Abstract: (2) a copolymer of ethylene with at least one alpha-olefin of formula H2Cxe2x95x90CHR2, where R2 is a C2xe2x88x928 linear or branched alkyl, containing about 15% to 40% by weight alpha-olefin, and having solubility in xylene at room temperature greater than about 25% by weight, the intrinsic viscosity of the xylene soluble fraction ranging from about 0.5 to about 5.0 dl/g;

Abstract: The polyolefin composition of the invention, preferably prepared by sequential polymerization in at least three stages, has tensile strength at break xe2x89xa725 MPa, elongation at break xe2x89xa7700 MPa and toughness xe2x89xa7150 MPa.


Disclosed is a terahertz wave generator which includes a dual mode semiconductor laser device configured to generate at least two laser lights having different wavelengths and to beat the generated laser lights; and a photo mixer formed on the same chip as the dual mode semiconductor laser device and to generate a continuous terahertz wave when excited by the beat laser light.

Exemplary embodiments relate to a semiconductor device, and more particularly, relate to a terahertz wave generator.
A terahertz (THz) wave may be an electromagnetic wave between a microwave and an infra ray, and may have a frequency within a range of 0.1 THz to 30 THz. The terahertz wave may have both wave-like characteristics (e.g., the dielectric penetrability of a radio wave) and the particle-like characteristics (e.g., the propagation direction of a light wave). The terahertz wave with absorption is applicable to image, spectrum, and communication fields as a new technology. It is possible to penetrate the interior of a substance or to analyze a body mechanism of a molecule motion energy level and a space signal, using the terahertz wave. Further, an ultrahigh-speed short-range wireless communication can be made more excellently using the terahertz wave as compared with a microwave and a millimeter wave.
The THz wave technology with the above-described applicability may have been limited due to a trouble of development of a light source and a detector. However, development of semiconductor and laser technologies may enable the appearance of various light sources. Hitherto developed pulse light source technologies may include a photoconductive antenna manner, an optical rectification manner, and the like. Continuous wave light sources for generating a THz wave may include a photo mixer, a hot-hole laser, a free electron laser, a quantum cascade laser, and the like.
The photo mixer may be considered as a terahertz technology with a relatively high commercialization probability as compared with other technologies. The reason may be because the photo mixer is driven at a room temperature, freely varies a frequency, and is implemented by a low-cost, small-sized system.
The photo mixer may generate or detect a THz wave using a photoconductive material whose carrier lifetime is within a range of hundreds femtoseconds (fs) to several pico-seconds (ps) and an antenna formed on the photoconductive material. The photoconductive material may be a material whose resistance varies by a carrier excited by an exciting light. The photoconductive material may play a role of a switch which enables a current to flow to an integrated antenna. The antenna and a photoconductive switch may constitute a photo mixer.
A femtosecond pulse laser may be mainly used to generate a terahertz wave. Since the intensity of light is large, the femtosecond pulse laser may generate a pulse terahertz wave having a relatively large intensity at a wide frequency region. In case of generating a continuous terahertz wave, two laser beams of different wavelengths may be beat and a resultant may be used as an excited wave. Upon generating of a continuous THz wave with a variable frequency, two continuous waves output from two distributed feedback lasers (DFBs) or a continuous light source laser may be used. If one or all (two) wavelengths are varied, a frequency of a beat signal may be varied, so that a frequency of a produced THz wave is changed. The intensity of the exciting light may be maintained largely while a wavelength is changed.
In recent, needs for portable terahertz generator/detector may increase. However, a bulky femtosecond laser generator may be used as a light source of an exciting light used at a terahertz generator/detector. Accordingly, there may be required a technology of implementing terahertz generator and detector with a low cost and a small size.

Electronics and Telecommunications Research Institute


A method of synthesizing rottlerin analogs is described. The synthesis methods described are the first known method of synthesizing rottlerin analogs from commercially-available materials to produce cost effective analogs. Rottlerin analog structures made by the synthesis methods and methods of use for treating a neurological or inflammatory response mediated by protein kinase C (PKC) are further described.

Various neurodegenerative disorders are characterized by selective degeneration of nigral dopaminergic neurons in the brain, including Parkinson's disease (PD). PD is the second most common neurodegenerative disorder after Alzheimer disease and affects more than 1.5 million people in the U.S. with approximately 50,000 to 60,000 new cases diagnosed each year. The disease is characterized by the cardinal motor symptoms of rigidity, bradykinesia, tremors and postural instability. Existing treatment options for neurodegenerative disorders fail to prevent the progression of the degeneration. As a result, development of neuroprotective agents to delay progression of the disease is needed. The apoptotic cell death pathway mediated by protein kinase C is a viable treatment pathway.
Protein kinase C (PKC) belongs to a family of serine threonine protein kinases. To date, twelve isoforms in the PKC subfamily have been identified (Kanthasamy et al., Antioxidants & Redox Signaling, 5: 609-620, 2003). One such isoform is protein kinase C delta (PKCδ) (Martelli et al., Eur. J. Histochem., 48(1):89-94, 2004).
PKCδ was originally discovered by Gschwendt et al. (Biochem. Biophys. Res. Commun., 137: 766-74, 1986) and cloned from a rat brain cDNA library the following year (Kurkinen et al., Gene 242: 115-23, 2000; Ono et al., Identification of three additional members of rat protein kinase C family: delta-, epsilon- and zeta-subspecies. FEBS Lett., 226: 125-8, 1987). The PKCδ gene is localized on human chromosome 3 (Huppi et al., Assignment of the protein kinase C delta polypeptide gene (PKCδ) to human chromosome 3 and mouse chromosome 14. Genomics 19: 161-2, 1994), rat chromosome 16 (Kurkinen et al., Genomic structure and chromosomal localization of the rat protein kinase C delta gene. Gene 242: 115-23, 2000), and mouse chromosome 14 (Huppi et al., Assignment of the protein kinase C delta polypeptide gene (PKCδ) to human chromosome 3 and mouse chromosome 14. Genomics. 19: 161-62, 1994).
Rottlerin exhibits biological activity, including selectively inhibiting protein kinase C delta (PKCδ). Rottlerin is a natural product that is isolated from the seeds of the fruit Mallotus philippinensis, most commonly produced in India, Philippines, Southeast Asia, and Australia. The IUPAC name for rottlerin is (E)-1-[6-[(3-acetyl-2,4,6-trihydroxy-5-methylphenyl)methyl]-5,7-dihydroxy-2,2-dimethylchromen-8-yl]-3-phenylprop-2-en-1-one. The molecular formula for the structure is C30H28O8 and the structure has a molecular weight of 516.53852 g/mol. The chemical structure of rottlerin is shown below:

Rottlerin selectively inhibits PKCδ with an IC50 of 3-6 μM. Although rottlerin is widely used as a specific inhibitor of PKCδ (McCormack et al., Neurobiol. Dis., 10(2): 119-27, 2002; Kanthasamy et al., Brain Res., 759(1): 1-8, 1997; Przedborski et al., Proc. Natl. Acad. Sci., 93(10): 4565-71, 1996), rottlerin has also been shown to inhibit PRAK, MAP kinases, and CAMKII kinases at higher concentrations (Turmel et al., Mov. Disord., 16(2): 185-9, 2001; Jackson-Lewis et al., Neurodegeneration, 4(3): 257-69, 1995).
Synthesis of rottlerin has not been reported. No studies of the scope and limitations of the preparation of rottlerin and/or any synthetic analogs have been reported. Similarly, there is a lack of detailed studies of the molecular mechanism of action of rottlerin; it is unknown what segments of the rottlerin structure are biologically active. However, documented uses of the rottlerin structure are known (see e.g., Kanthasamy et al. U.S. patent application Ser. Nos. 11/479,173 and 61/240,906) but are significantly restricted due to the limited natural abundance of the substance. Due to such limited abundance, rottlerin is cost prohibitive for use as a drug therapy, despite its identified beneficial actions as a PKCδ inhibitor. Accordingly, methods of rottlerin synthesis in large quantities are desirable in order to obtain sufficient quantities of the analog for future studies. Further, synthetic rottlerin that are PKCδ inhibitors with better selectivity and more affinity are desirable and an objective of the present invention.
Accordingly, it is an objective of the present invention to develop methods and means of synthesizing PKCδ inhibitor analogs from the rottlerin base structure.
It is a further objective of the present invention to develop rottlerin analogs having simplified chemical structures in order to identify analogs with enhanced biological activity compared to natural rottlerin.
It is a further objective of the present invention to develop methods of rottlerin analog synthesis from commercially-available materials comprising minimal synthesis steps, namely four or fewer synthesis steps.
The method and means of accomplishing each of the above objectives as well as others will become apparent from the detailed description of the invention which follows hereafter.

Design, synthesis and functional characterization of rottlerin analogs

Iowa State University Research Foundation, Inc.


Embodiments of the invention describe heterogeneous photonic integrated circuits (PIC) wherein a first silicon region is separated from the heterogeneous semiconductor material by a first distance, and a second silicon region is separated from the heterogeneous semiconductor material by a second distance greater than the first distance.

The efficiency of an optical device (e.g., the aspects of the drive voltage or power requirement of the device) is fundamentally determined by the electro-optic materials used to construct the device. Silicon materials are more easily processed and more readily available, but are not as efficient at light emission or absorption as non-silicon materials (such as III-V materials), nor do they possess other desirable optical properties present in materials such as, magneto-optic materials, and other crystal substrate materials. Attempts have been made to create photonic devices utilizing these materials in addition to silicon, wherein the device's optical waveguide is formed and included silicon semiconductor material and non-silicon material (and, in some cases, the bonding layer combining both materials). These devices are referred to herein as heterogeneous photonic integrated circuits (PICs).
Heterogeneous PICs on silicon-on-insulator (SOI) substrates require a method of controlling the confinement factor of the optical mode in the heterogeneously integrated material. It is desirable to be able to achieve a wide range of optical confinement factors in the heterogeneous material, nearly spanning 0 to 100%, in order to efficiently transfer light between Si-only modes and heterogeneous modes, to avoid interaction of light with absorbing or scattering materials and structures, and to optimize optical and optoelectronic devices for characteristics dependent upon confinement factor of the mode in the heterogeneous material such as gain, saturation, absorption coefficient, nonlinear coefficients, and modulation efficiency per unit distance.
Current solutions rely on controlling the optical confinement in the heterogeneous material by laterally varying the dimension of either the silicon waveguide, the heterogeneous material, or both. The drawback of these approaches is that the flexibility to change confinement in the heterogeneous integrated material is dependent on the range of widths for which one can define the structures. The range of widths is restricted by lithography for both silicon waveguides and the heterogeneous integrated materials. In the case of active devices, the range of widths is additionally restricted by device design considerations such as the maximum width permissible to obtain the desired capacitance and current density, and the minimum width permitted to create electrical contacts and current channels.
Descriptions of certain details and implementations follow, including a description of the figures, which may depict some or all of the embodiments described below, as well as discussing other potential embodiments or implementations of the inventive concepts presented herein. An overview of embodiments of the invention is provided below, followed by a more detailed description with reference to the drawings.

Heterogeneous semiconductor photonic integrated circuit with multiple offset heights

Abstract: Thus embodiments of the invention may be described as, in heterogeneous regions of a heterogeneous PIC, silicon waveguides using multiple heights of the silicon waveguide, or other structures with multiple offset heights between silicon and heterogeneous materials (as described herein).


An apparatus for archiving robust channel estimation in a communication system includes a training sequence generator to generate a training sequence. A formatter inserts the training sequence to a frame. A transmitting module is employed to transmit the frame. The training sequence generator further includes a symbol generator to generate a plurality of training symbols satisfying a predetermined constraint such that the training symbols are insensitive to synchronization error and a training sequence forming unit that forms the training sequence from the training symbols generated by the training symbol generator.

In wireless communication, OFDM (Orthogonal Frequency Division Multiplexing) has been viewed as a popular technical solution with high spectrum efficiency for realizing high data rate, especially in 4G (4th Generation) wireless communication systems, because of its effective use of frequency band and simple implementation. Typically in an OFDM system, available bandwidth is divided into a number of discrete channels, which are overlapping and orthogonal to each other. Each discrete channel is defined as a subcarrier and has a well-defined frequency. Each subcarrier carries modulated symbols, the amplitude and/or phase of which represent encoded information. At receiver end, received OFDM symbols can be demodulated only after the starting time of each OFDM symbol is identified. Therefore, time synchronization is required to identify the timing of the symbol. However, synchronization error exists due to channel fading, interference, noise and so on.
There are two kinds of synchronization error, early synchronization error and late synchronization error. The impacts of the early synchronization error to subsequent blocks can be ignored as long as the estimated starting time lies in the range of cyclic prefix of the symbol. The late synchronization error is more harmful than the early synchronization error, as there is no effective protection provided against this kind of synchronization error.
In practice, the estimated symbol starting time is typically shifted backwards a certain amount within the cyclic prefix to reduce the probability of the late synchronization error. However, for an OFDM system with multi-path fading channel, the late synchronization error is more likely to occur. This is due to the fact that the starting time of the signal transmitted through the strongest path (rather than the starting time of the signal transmitted through the weaker path with the smallest propagation delay) is typically taken as the starting time of the received symbol for time synchronization. Thus, the above-mentioned method of shifting the estimated symbol starting time can provide little help in this situation, because the strongest path may have much larger propagation delay than the first path.
In order to avoid the above-mentioned problem, prior solutions focus on special designed training sequences in the preamble field or longer cyclic prefix. However, such solutions are disadvantageous in that modification of the format of preamble field or data field is needed and the modification may have conflict with specifications in communication standards.
Another prior solution focuses on joint synchronization and channel estimation. Joint estimation can obtain more accurate result than separate estimation, but the computation complexity of joint estimation is much more than that of separate estimation. More complexity results in higher cost. An improved joint estimation is proposed to improve channel estimation by weighted averaging multiple training sequences based on estimated power of interference. But, in the system with the late synchronization error, all the received training sequences involve great interference, and therefore, the method of weighted averaging will not bring improvement.
MIMO (Multiple Input Multiple Output) OFDM system is more sensitive to synchronization error than SISO (Single Input Single Output) OFDM system, because synchronization error in one receiver can not only introduce interference to it own but also confuse other receivers. Because there are different timing offsets between multiple transmitters and a single receiver, ideal synchronization or early synchronization for signal from one transmitter often becomes late synchronization for signal from another transmitter. So synchronization error is difficult to avoid in MIMO OFDM system even if the clocks of some transmitter and receiver are perfectly synchronized.

Robust channel estimation in communication systems


A weatherseal employing a magnetic appendage for enhancing the sealing with a mounting surface. The weatherseal includes an elastomeric base that conforms to and engages the mounting surface. The seal portion extends from the base for selective engagement with a second surface, such as a door of a vehicle. An appendage is fabricated from a magnetic elastomer that is sufficiently flexible to conform to irregularities in the mounting surface. Preferably, only the appendage is formed of the magnetic elastomer to achieve an effective seal with only a small amount of the expensive magnetic elastomer to enhance the seal with the mounting surface and avoid, for example, the use of more expensive welded mounting channels that add undesired weight to the vehicle.

1. Field of the Invention
This invention relates to sealing systems, and more particularly to a weatherseal or weatherstrip employed with a vehicle door that enhances the seal between the weatherstrip and a surface to which it is attached.
2. Discussion of the Art
It is well known in the art to use an extruded weatherseal that seals the gap between a door and a body of a vehicle. Under conventional practice, a mounting region or base of the seal is secured to the door with a metal C-channel that is spot welded to the door. Enclosing edges retain the weatherseal in position in the C-channel. Moreover, by spot welding the C-channel to the door, water is prevented from running or passing beneath the weatherseal. Although a continuous water tight seal is obtained, it is an expensive assembly and thus adds to both the cost and the weight of the vehicle. Using a C-channel requires a vehicle manufacturer to roll form, stretch-bend, cut-to-length, and spot weld the C-channel. Numerous problems are associated with this assembly and it still does not provide a foolproof manner of preventing water ingress into the vehicle. Flange mounted seals are another area where water intrusion between the seal and the seal mounting region, i.e., the flange, is a concern.
Door mounted weatherseals or weatherstrips are designed to fit to and seal the vehicles. Compliancy of the weatherseal is important in order to adequately seal the vehicle. That is, the weatherseal must be sufficiently flexible so that it will fit many irregular surfaces or curved surfaces, and still maintain a seal. Thus, any proposed solution to the water ingress problem along the mounting surface must still adequately address the need for compliancy in the remainder of the weatherseal.
Although others have suggested using a magnetic rubber formulation as a part of a door mounted weatherseal, the desired savings in the manufacturing costs and weight do not outweigh the increased costs of using an expensive magnetic rubber formulation. That is, others have suggested magnetic sealing where the target is the sealing surface, i.e., in the case of a door mounted seal, the vehicle body is the target and the magnetic seal enhances the sealing contact with the body.
Accordingly, a need exists for an effective weatherseal in the vehicle door environment that is effective and provides increased savings.
An improved weatherseal includes a base that conforms to and engages an associated first surface. A seal portion extends from the base and selectively engages a second surface or target when the first and second surfaces are disposed in close proximity. An appendage is fabricated from a magnetic elastomer and is sufficiently flexible to conform to irregularities in the first surface.
The base, seal portion, and magnetic appendage are preferably coextruded.
The weatherseal is secured to the first surface at spaced locations via attachment members or pegs which eliminate use of a welded C-channel.
A corrosion resistant layer is preferably added to the magnetic appendage.
A primary benefit of the invention relates to the significant savings to the vehicle manufacturer as a result of reduced weight and costs.
Another benefit of the invention resides in the continuous water tight seal formed between the weatherseal and the mounting surface to which it is attached.
Another benefit of the invention resides in the ability of the weatherseal to conform to irregularities in the mounting surface and prevent water from running beneath the seal and leaking into the interior of the vehicle.
Yet another advantage of the invention is realized by the flexibility of the weatherseal to fit normal variations in sheet metal contours of the mounting surface.
Still other advantages and benefits will become apparent to those skilled in the art upon reading and understanding the following detailed description.


Tobacco products suitable for oral ingestion are provided. The tobacco products include a tobacco composition and at least one edible film. The edible film can include one or more of (i) a fruit or vegetable puree and (ii) a denatured protein. A multi-layer tobacco product is provided that includes a tobacco composition in the form of a compressed sheet layer and at least one edible film adjacent to the tobacco composition layer, wherein the edible film includes a puree of at least one fruit, vegetable, or a combination thereof. A process for preparing a tobacco product is also provided, such as a process that includes receiving a tobacco composition and an edible film; applying the edible film to the tobacco composition; and compressing the edible film and tobacco composition together to form a multi-layer tobacco product.

Tobacco may be enjoyed in a so-called "smokeless" form. Particularly popular smokeless tobacco products are employed by inserting some form of processed tobacco or tobacco-containing formulation into the mouth of the user. See, for example, the types of smokeless tobacco formulations, ingredients, and processing methodologies set forth in U.S. Pat. No. 1,376,586 to Schwartz; U.S. Pat. No. 3,696,917 to Levi; U.S. Pat. No. 4,513,756 to Pittman et al.; U.S. Pat. No. 4,528,993 to Sensabaugh, Jr. et al.; U.S. Pat. No. 4,624,269 to Story et al.; U.S. Pat. No. 4,991,599 to Tibbetts; U.S. Pat. No. 4,987,907 to Townsend; U.S. Pat. No. 5,092,352 to Sprinkle, III et al.; U.S. Pat. No. 5,387,416 to White et al.; U.S. Pat. No. 6,668,839 to Williams; U.S. Pat. No. 6,834,654 to Williams; U.S. Pat. No. 6,953,040 to Atchley et al.; U.S. Pat. No. 7,032,601 to Atchley et al.; U.S. Pat. No. 7,694,686 to Atchley et al.; U.S. Pat. No. 7,810,507 to Dube et al.; U.S. Pat. No. 7,819,124 to Strickland et al.; U.S. Pat. No. 7,861,728 to Holton, Jr. et al.; and U.S. Pat. No. 7,946,296 to Wrenn et al.; US Pat. Pub. No. 2004/0020503 to Williams; US Pat. Pub. No. 2005/0115580 to Quinter et al.; US Pat. Pub. No. 2005/0244521 to Strickland et al.; US Pat. Pub. No. 2006/0191548 to Strickland et al.; US Pat. Pub. No. 2007/0062549 to Holton, Jr. et al.; US Pat. Pub. No. 2007/0261707 to Winterson et al.; US Pat. Pub. No. 2008/0029110 to Dube et al.; US Pat. Pub. No. 2008/0029116 to Robinson et al.; US Pat. Pub. No. 2008/0029117 to Mua et al.; US Pat. Pub. No. 2008/0173317 to Robinson et al.; US Pat. Pub. No. 2008/0196730 to Engstrom et al.; US Pat. Pub. No. 2008/0209586 to Neilsen et al.; US Pat. Pub. No. 2008/0305216 to Crawford et al.; US Pat. Pub. No. 2009/0065013 to Essen et al.; US Pat. Pub. No. 2009/0293889 to Kumar et al.; US Pat. Pub. No. 2010/0170522 to Sun et al.; US Pat. Pub. No. 2010/0291245 to Gao et al.; US Pat. Pub. No. 2010/0300463 to Chen et al.; US Pat. Pub. No. 2010/0300464 to Gee et al.; US Pat. Pub. No. 2010/0303969 to Sengupta et al.; US Pat. Pub. No. 2011/0061666 to Dube et al.; US Pat. Pub. No. 2011/0139164 to Mua et al.; US Pat. Pub. No. 2011/0247640 to Beeson et al.; Us Pat. Pub. No. 2011/0315154 to Mua et al.; US Pat. Pub. No. 2012/0031414 and US Pat. Pub. No. 2012/0031416 to Atchley et al.; US Pat. Pub. No. 2012/0055493 to Novak et al.; 2012/0055494 to Hunt et al.; US Pat. Pub. No. 2012/0118310 to Cantrell et al.; PCT Pub. No. WO 04/095959 to Arnarp et al.; and PCT Pub. No. WO 10/132444 to Atchley; each of which is incorporated herein by reference.
Representative smokeless tobacco products that have been marketed include those referred to as CAMEL Snus, CAMEL Orbs, CAMEL Strips and CAMEL Sticks by R. J. Reynolds Tobacco Company; GRIZZLY moist tobacco, KODIAK moist tobacco, LEVI GARRETT loose tobacco and TAYLOR'S PRIDE loose tobacco by American Snuff Company, LLC; KAYAK moist snuff and CHATTANOOGA CHEW chewing tobacco by Swisher International, Inc.; REDMAN chewing tobacco by Pinkerton Tobacco Co. LP; COPENHAGEN moist tobacco, COPENHAGEN Pouches, SKOAL Bandits, SKOAL Pouches, RED SEAL long cut and REVEL Mint Tobacco Packs by U.S. Smokeless Tobacco Company; and MARLBORO Snus and Taboka by Philip Morris USA.
It would be desirable to provide an improved means for delivering compact or compressed amounts of smokeless tobacco wherein the means of delivery provides various advantageous features, such as ease of dispensing, use, and an overall enjoyable form.


A pull-up latch mechanism includes a stator (2) with an inner open channel (20), a cap (10) attached to a cylinder (1) lodged into the open channel (20) of the stator (2), a shaft (8) provided with a latching pawl, and a control system connecting the shaft (8) to the cylinder. The control system is adapted for generating a first movement of rotation of the cylinder, a movement of the shaft (8) away from the cylinder in the direction of the longitudinal axis, for generating a second movement of rotation of the cylinder, and a movement of the shaft towards the cylinder in the direction of a central axis.

Pull-up latch mechanism have already been used in the prior art. Such known pull-up latch mechanism comprises:
a stator with a substantially cylindrical inner open channel having a longitudinal axis and extending from a front opening up to a back opening with a cross section smaller than the section of the front opening,
a cap attached to a cylinder (1), whereby the cylinder is adapted to be lodged into the open channel of the stator, when the cap is lodged at least partly into the front portion, whereby the cap and cylinder are adapted to rotate within the inner channel on the action of a control means,
a shaft (8) provided with a latching pawl and provided with a hole for receiving a rod, and
a control system comprising an outer sleeve and an inner sleeve provided each with a groove, said inner sleeve being inserted within the outer sleeve which is inserted within the inner channel of the stator through the front opening thereof.
a rod connects the shaft 8 with the said inner and outer sleeves, the end portions of the rod extending within the grooves of the said sleeves.
a system for connecting the outer sleeve with the cylinder.
Such systems are disclosed for example in GB2158866 and U.S. Pat. No. 7,441,427.
Drawbacks of such disclosed system is that inner and outer sleeves have to rotate with the channel of the stator, whereby increasing potential problem of gripping, as well as pivoting movements between the sleeves and/or with the shaft.
In such disclosed system there is no means for retaining the sleeves with the cylinder, as well as there is no means for maintaining the sleeve within the channel of the stator and/or for preventing some longitudinal movement of the sleeve in case the mechanism being in unlocked position.
In case of longitudinal movement of one or more sleeves, the shaft in unlocked position can also move longitudinal, whereby the latch can extend in a position preventing its rotation within a locked position.
EP1411198 disclose a latch mechanism comprising a drive input means arranged in a fixed housing, an output shaft connected to the drive input means. The output shaft is provided (a) with a L-shaped guide cam surface cooperating with a cam follower attached to the housing, and (b) an inclined cam surface cooperating with another cam follower pushed into a hole of an end of the drive input means, through a hole of the housing. In said mechanism, the drive input means is inserted into a sleeve of the output shaft, before inserting the drive input means and the output shaft within the axial passage of the housing through the back opening. Thereafter a guide pin has to be inserted through a lateral hole of the housing into the L shaped guide cam surface of the sleeve of the output shaft, so as to maintain the said sleeve into the housing. For the insertion of said cam follower, the sleeve and possibly the drive input means have to be correctly placed within the axial passage of the housing.
In such a mechanism, the cam follower acts as means for maintaining the sleeve into the passage of the housing, meaning that in case of excessive rotation of the sleeve, for example by a thieve, the cam follower can be broken off, whereby the sleeve can be pushed backwards, and whereby the mechanism is no more suitable to maintain locked a door, etc.
The mechanism of the invention aims to solve one or more of the problems listed hereabove.


Cosmetic methods for obtaining a slimming effect are disclosed. The methods include providing a composition containing a carob (Ceratonia siliqua L.) seed extract and caffeine or a derivative of caffeine as a slimming active agent and a physiologically acceptable medium, and topically applying the composition on at least a portion of the body or face. The topical application of the composition includes the application of an effective amount of the composition that increases the expression of aquaglyceroporins, increase lipolysis, promotes the elimination of lipids, reduces localized excess body fat, and/or attenuates the “orange peel” appearance of the skin.

The subcutaneous adipose tissue is located at the hypodermis. It is a type of connective tissue where adipocytes are predominant, organized in lobes around 5 mm in diameter, separated by fine connective bridges. Each adipocyte contains a voluminous lipid vacuole containing essentially triglycerides and having a diameter that may range from 40 to 120 μm.
Adipose tissue may be considered to be a dynamic reservoir, constantly being renewed, balancing the dietary intake with the energy requirements of the body. Thus, adipocytes ensure the synthesis, accumulation and release of lipids. This process is dependent upon hormones such as insulin or leptin.
Lipid synthesis, or lipogenesis, originates with triglycerides of dietary origin and glucose. Conversely, the triglycerides stored in the adipocytes may be hydrolyzed, during lipolysis, to release fatty acids, glycerol and glycerol mono- and diesters.
The non-esterified fatty acids thus released may circulate in the blood and then be available for the energy requirements of other cells of the body, or be quickly reused by the adipocyte so as to generate, again, triglycerides by lipogenesis.
If a sustained imbalance occurs in the body promoting lipogenesis, the quantity of lipids stored in the adipocytes increases, leading to hyperplasia of the mass of body fat and more specifically to the appearance of localized excess body fat. In fact, in human adults, under the effect of sex hormones, the adipose tissue is distributed differently according to sex and forms the silhouette. Adipose tissue accumulates in the chest, on the hips, the buttocks and the thighs in women, and on the nape and shoulders in men. In addition, localized excess body fat is often associated with modifications in the skin, which develops a dimpled or "orange-peel" appearance. This localized excess body fat is currently considered to be unattractive, and people affected may want to improve the appearance of their skin and silhouette using cosmetic methods.
Numerous active agents having an action on lipolysis or lipogenesis, intended for slimming effect, have thus been identified. Among them, the following may be cited:                Xanthine bases (xanthine derivatives), such as theophylline, caffeine, theobromine (described in patents FR 2 609 395, FR 2 671 487), used for their action promoting the lipolytic activity of fat cells.        Synthetic peptides, such as the peptide of sequence Arg-Gly-Ser-NH2 (described in patent FR 2 858 769), or the peptide of sequence Pro-Leu-Asp-Thr-Ala-Lys-Val-Arg-Leu-Gln (described in patent FR 2 879 924) used for their action in the decoupling between coenzyme reoxidation and phosphorylation of ADP into ATP in the mitochondria.        Plant extracts, such as marine algae extract of the Palmaria or Rhodymenia genus (described in patent FR 2 887 447), gingko biloba extracts (see patent FR 2 669 537), or soy flavones or isoflavones (described in patent WO 01/64177).
However, these products generally have moderate or limited efficacy over time. It is therefore important to provide new active cosmetic agents having remarkable efficacy as slimming active agents.
The solution to the technical problem addressed lies in the cosmetic use of the association of a carob germ extract and caffeine or a derivative thereof. The inventors have indeed demonstrated that a carob germ extract acts on aquaglyceroporins, thereby promoting the transport of glycerol released during lipolysis, from the adipocyte. The association of this extract with caffeine, or derivatives thereof, the latter already being known to increase lipolysis, makes it possible to obtain a slimming active agent having remarkable properties.
Aquaporins are a class of transmembrane proteins carrying water and small molecules in solution, between the cells and the internal medium. Aquaporins may be classified into two distinct sub-groups: aquaporins enabling only the transport of water, and aquaglyceroporins which enable, in addition to the transport of water, the transport of glycerol.
In this second sub-group, aquaglyceroporin 7 was identified in the membrane of human adipocytes and plays an important role in the metabolism of reserve fats (Mariko Hara-Chikuma et al. Progressive adipocyte hypertrophicity in aquaporin-7 deficient mice, J. Biol. Chem., vol. 280, no. 16, Apr. 22, 2005).
The particular properties of aquaglyceroporins therefore makes them beneficial biological targets for promoting the elimination of lipids contained in the adipocytes.
"Elimination of lipids" refers to the phenomenon of lipolysis leading to the export of glycerol from the adipocyte cell.
The invention and the resulting advantages will be better understood upon reading the description.

This patent is subject to a terminal disclaimer.

Cosmetic use of the combination of a carob germ extract and caffeine as a slimming active agent


Method and apparatus for data transmission based on sliding detection are disclosed. The method includes: when it is detected that a TimeLine scrolls on a screen of a user device, recording, by a message client, application a Message Cell visible on the screen; and determining, by the message client application, whether the Message Cell is still visible on the screen after a predefined time interval; if the Message Cell is still visible, downloading, by the message client, data corresponding to the Message Cell from a message server. An apparatus for data transmission based on slide detection includes a detecting module, a recording module, a determining module and a downloading module. Thus, downloading is avoided for the data corresponding to Message Cells that enters into then slides out of the screen quickly. Network data traffic of users is reduced and user's experience is improved.

With development of network techniques, Internet has deeply rooted in network users' mind. Among most Internet applications, information propagation and sharing via message client applications have become an indispensable part of people's daily life. During a communication procedure based on a message client application, there are usually a lot of messages (such as text information, image information and audio/video information, etc.) need to be transmitted.
Microblog is an information transmission system adopting the above message client application. Microblog is an instant information sharing, propagation and obtaining platform based on relationships of users. Users may log on microblog client applications via devices such as cell phone, computer, etc., so as to realize information sharing.
Considering instantaneity of the microblog, cell phone becomes one of the most carriers of the microblog. When browsing microblog messages using a cell phone, a user usually performs some sliding operations. Thus, one message not displayed on the screen will slide into the screen.
In the microblog system, a message is usually carried by a message unit (Message Cell). Usually, each Message Cell may include message content, a name and an avatar of a message author, etc. Multiple Message Cells form a list or a table (TimeLine) according to their times and are displayed on the screen of the cell phone.
When the user performs the sliding operation, a Message Cell not displayed on the screen will slide into the screen. As to each Message Cell which slides into the screen during the sliding operation, the microblog client application needs to download the message content, the name and the avatar of the message author corresponding to the Message Cell.
When the user performs the sliding operation quickly and continuously, there will be a lot of Message Cells sliding into the screen and then sliding out of the screen again. Thus, the microblog client application has to download the message content, the name and the avatar of the message author corresponding to each Message Cell once slid into the screen. However, at this time, what the user cares about is not the Message Cells once slid into the screen during the quick and continuous sliding operation, but those Message Cells which are displayed on the screen when the sliding operation ends. Thus, large amounts of network resources are wasted in downloading the message content and/or avatar of the message author corresponding to the Message Cells sliding into the screen during the sliding operation, especially when the message content corresponding to the Message Cells contains large files such as image or audio/video data.
As to cell phone users who accessing the network based on data traffic charge, the above download procedure wastes a lot of traffic and brings bad user experience.
Similarly, as to computer users who access network via wireless manners such as 3G, the same problem also exists.

Upon determining that a message cell of a time line is still visible on a screen after a predefined time interval, dowloading an avatar of an author of the message cell

Tencent Technology (Shenzhen) Company Limited


The present disclosure provides a method, system, and device for securely updating a software release across a network. To illustrate, a server may compile a transaction log that includes information corresponding to one or more nodes in the network to which the software release has been transmitted. The server may analyze one or more files based on vulnerability information to identify at least one file of the one or more files that poses a risk. The server may also identify at least one node of the network at which the at least one file is deployed. Based on identifying the at least one node, the server may transmit a corrective action with respect to the at least one node.

Computer systems and software have become an integral part of modern society and affect a variety of aspects of daily life. Software can be developed as a monolith, such as one piece of software, or as a service-oriented architecture where each piece of software provides a specific service and multiple pieces of software operate together. Software can be updated to add or remove functionality, to correct bugs (e.g., critical/functional issues), and/or to address security issues.
After a software release is deployed and in use by one or more devices, an issue or problem may be identified. For example, an operating bug, a data breach issue, a safety issue, a worm, or other malware may be identified in existing software. However, identifying that a problem exists does not indicate the scope/extent of the problem or a resolution of the problem. In order to determine how the problem affects deployed software, a large amount of computational resources and personnel resources may be needed. For example, it may be difficult to determine which version of a software release is being executed at various devices, and which versions of software releases include the problem. In addition, how to respond to or compensate for the identified problem is not always readily apparent. Thus, dealing with an identified problem can be a time and resource-consuming process.


A method for determining an intervention response category for provisioning workflows. The method determines provisioning features of a provisioning step. The method performs outlier detection to identify and remove outliers from non-intervention data to produce a non-intervention normal data set. The method performs iterative grouping on the non-intervention normal data set to determine significant variables in the provisioning features. The method performs response mapping of provisions using results of the iterative grouping including a significance of errors and a presence of errors in the non-intervention normal data and partial intervention data to categorize the provisions into a response category.

Provisioning a virtual machine or baremetal server in the cloud involves a number of provisioning steps during which unstructured, timestamped logs are generated as the workflow progresses through the provisioning steps and reflect the provisioning status. Of approximately tens of thousands of virtual server infrastructure (VSI) provisions that happen per day, a few hundred provisions can end up in a stuck state during a given provisioning step. Proactive detection and remediation of overdue provisions generally involves having to manually identify the error causing the provision to be in the stuck state, which can be a significant performance bottleneck. Additionally, not all overdue transactions require manual attention because of their ability to self-resolve. Current methods of anomaly detection do not provide guidance on when to intervene.

Method for proactive trouble-shooting of provisioning workflows for efficient cloud operations

International Business Machines Corporation


A power semiconductor device for an igniter comprises: a first semiconductor switching device; and an integrated circuit, wherein the integrated circuit includes: a second semiconductor switching device connected in parallel with the first semiconductor switching device and having a smaller current capacity than a current capacity of the first semiconductor switching device; a delay circuit delaying a control input signal so that the second semiconductor switching device is energized prior to the first semiconductor switching device; a third semiconductor switching device including a thyristor structure connected to a high voltage side main terminal of the second semiconductor switching device and being made conductive by a part of a main current flowing through the energized second semiconductor switching device; and a first excess voltage detection circuit stopping the first semiconductor switching device when voltage on the high voltage side main terminal is equal to or more than a predetermined voltage.

1. Field of the Invention
The present invention relates to a power semiconductor device for an igniter having an overheat protection function to protect a semiconductor switching device at an abnormally high temperature in an ignition system for an internal combustion engine.
2. Background Art
An ignition system for an internal combustion engine such as an automobile engine has, as components for generating a high voltage to be applied to an ignition plug, and a power semiconductor device incorporating an ignition coil (inductive load), a semiconductor switching device for driving the ignition coil and a circuit device (semiconductor integrated circuit) for controlling the semiconductor switching device. These components constitute a so-called igniter. The ignition system also has an engine control unit (ECU) including a computer. In such a power semiconductor device for an igniter, the resistance to a load dump surge, i.e., a transient excess voltage surge generated in the power supply voltage, is ordinarily assured as one of items of reliability of the power semiconductor device. In ordinary cases, therefore, a method is used in which the power supply voltage is directly observed and the operation of a semiconductor switching device or an integrated circuit controlling the semiconductor switching device installed in the power semiconductor device is stopped when the power supply voltage is excessively high to protect the integrated circuit.
Electric power for the above-described power semiconductor device for an igniter is ordinarily supplied from a motor vehicle battery. However, fluctuations and surge voltages in the voltage of such a power supply are large. In most cases, therefore, the power supply voltage is clamped with a Zener diode, then regulated in a constant-voltage circuit and supplied into the integrated circuit. Direct observation of the battery voltage requires adding a special signal taking-in terminal and providing a protective device of a large power capacity at the terminal. This means an inevitable increase in manufacturing cost. Further, since the Zener diode is provided on the terminal through which the battery voltage is input for power supply to the integrated circuit, the voltage is fixed substantially at the Zener clamp voltage and the desired sensitivity cannot be obtained with respect to an excess voltage. Thus, the above-described voltage observation method is not suitable for high-accuracy voltage detection.
As a solution to the above-described problem, a technique to protect the above-described switching device by monitoring the current between main terminals of the semiconductor switching device and limiting the control terminal voltage on the semiconductor switching device when the current flowing becomes equal to or larger than a predetermined value has been devised (see, for example, Japanese Patent Laid-Open Nos. 5-259853 and 7-86587).
A technique including forming a thyristor on the substrate on which the switching device is formed to extract a high-potential-side main terminal voltage on the semiconductor switching device when the switching device is off and indirectly monitoring the power supply voltage from the output from the thyristor is also disclosed (see, for example, Japanese Patent Laid-Open No. 2000-183341).


Liquid resin compositions that can be used in the manufacture of composite materials are described. A method of making a fiber-reinforced polymeric composite material comprises wetting a fibrous material with a liquid prepolymer composition comprising at least one (meth)acrylic monomer, at least one base, and at least one peroxy ester; and polymerizing the liquid prepolymer composition to form a fiber-reinforced polymeric composite material.

Mechanical or structured parts that have to absorb high stresses during their use are widely manufactured from composite materials. A composite material is a macroscopic combination of two or more materials. Typically, a composite material comprises a matrix material that forms a continuous phase for the cohesion of the structure, and a reinforcing material with various architectures for the mechanical properties.
Composite materials are widely used in several industrial sectors; for example, building, automotive, aerospace, transport, leisure, electronics, and sports. Composite materials are often considered to provide better mechanical performance (e.g., higher tensile strength, higher tensile modulus, higher fracture toughness, etc.) in comparison to homogenous materials with lower density.
On the commercial industrial scale, the most important class of composites by volume are composites with organic matrices, wherein the matrix material is a polymer. The principal matrix or continuous phase of a polymeric composite material is typically either a thermoplastic polymer or a thermosetting polymer. In order to prepare a polymeric composite material, the prepolymer is typically mixed with the other component, such as glass beads or fibers, which become wetted or impregnated with the prepolymer, and the composition is subsequently cured.
A major disadvantage of a thermoset polymer matrix is its rigidity. Once the polymer has been cured, the form is fixed, such that the matrix cannot be easily shaped into other forms. This also makes it difficult to recycle thermoset composite materials. In contrast, thermoplastic polymers can soften or become less viscous when heated, and can take on new shapes by the application of heat and/or pressure. However, a drawback in using thermoplastic polymers for the fabrication of composite materials is that they have a high viscosity in the molten state, which makes it difficult to homogenously wet or impregnate a substrate, such as a fibrous substrate. The wetting or impregnation of fibers by the thermoplastic polymer can only be achieved if the thermoplastic resin is sufficiently fluid. In order to have a low viscosity or sufficient fluidity of the thermoplastic polymer, the chain length or molecular mass is often reduced. However, a molecular weight that is too low can have a negative impact on the performance of the composite material and on resulting structured parts, especially on mechanical properties such as deformation modulus.
Methods for making polymers, some of which can be used to make composite materials, have previously been described:
U.S. Pat. Nos. 3,362,942, 4,189,451 and 4,197,215 are directed to processes for polymerizing and curing methyl methacrylate monomer-polymer syrups in the presence of metal salts of hemi-peresters of maleic acid; and
U.S. Pat. No. 6,552,130 is directed to a resin composition that is suitable for use as a covering material for civil engineering and construction applications.
WO2013/056845 A2 is directed to a composite material via in-situ polymerization and its use and is incorporated herein in its entirety.
WO2014/013028 A1 is directed to impregnation process for a fibrous substrate and a liquid (meth)acrylic syrup for the impregnation process, and articles obtained from it and is incorporated herein in its entirety.
For at least the reasons described above, there remains a need for improved composite materials that can be fabricated using thermoplastic polymers, and efficient methods for manufacturing the composite materials.

Peroxy ester cure of liquid prepolymer compositions


An electron beam lithography system includes a laser for generating a laser beam, and a beam splitter for splitting the laser beam into a plurality of light beams. The intensity of the light beams is individually modulated. The light beams are of sufficient energy such that, when they impinge on a photocathode, electrons are emitted. Modulation of the light beams controls modulation of the resulting electron beams. The electron beams are provided to an electron column for focusing and scanning control. Finally, the electron beams are used to write a scanning surface, for example, using an interlaced writing strategy.

1. Field of the Invention
The present invention relates to electron beam lithography systems and, in particular, to a multiple beam system with modulated laser illumination.
2. Description of the Related Art
Electron beam lithography systems generally include an electron source and electron optics for accelerating the electrons into an electron beam and focusing the electrons onto a target, thereby exposing a mask (reticle) or wafer. In a conventional electron beam lithography system, a single beam in a single column is used to expose the resist and create the desired pattern.
The throughput of a conventional lithography system is limited by the total beam current: as the total beam current is increased, electronxe2x80x94electron interactions in the beam cause excessive blur, resulting in a degradation of the resolution in the written pattern. Several approaches are known to reduce electronxe2x80x94electron interactions and the associated beam blur. If the total current is distributed evenly among several beams, a reduction of the beam blur in each column results in higher resolution, and if all beams are operated in parallel, the throughput is not compromised. In addition, the clock rate of each individual beamlet is reduced by a factor equal to the number of beamlets, thus reducing the blanking rate for each beamlet significantly. This is impractical for a conventional column due to its overall dimensions and large footprint.
However, in a single electron beam column, the total current can be divided into several beamlets, which also reduces the blur due to electronxe2x80x94electron interactions and therefore allows a higher total beam current. Single beam-beamlet lithography systems are the patterned photocathode approach described in U.S. Pat. No. 5,684,360, xe2x80x9cElectron source utilizing negative electron affinity cathodes with ultrasmall emission areasxe2x80x9d, the gated electron emitter photocathode approach, described in WO9950874A3, or the VCSEL array approach described in co-pending U.S. patent application Ser. No. M-7958).
These and other drawbacks in the prior art are overcome in large part by an electron beam lithography system in accordance with the present invention.
The electron beam lithography system includes a laser for generating a laser beam, and a beam splitter for splitting the laser beam into a plurality of light beams. The intensity of the light beams is individually modulated. The light beams are of sufficient energy such that, when they impinge on a photocathode, electrons are emitted. Modulation of the light beams controls modulation of the resulting electron beams. The electron beams pass through an electron column for focusing and scanning control. Finally, the electron beams are used to write while scanning across a surface, for example, using an interlaced writing strategy.
In one implementation, a high throughput lithography system includes an electron beam column with a photocathode illuminated by an array of individually blanked laser beams in which the intensity of the individual laser beams is modulated or varied by one or more acousto-optical modulators. In particular, an argon-ion laser with a beam splitter and array of acousto-optic modulators in combination with a photocathode and 50 keV electron beam column is employed.

Multiple electron beam lithography system with multiple beam modulated laser illumination


A drug-filled synthetic resin ampule includes an ampule body and a drug 8 filled in the ampule body. The ampule body includes a tip-side sealing portion, a hollow portion, and an annular breakable portion provided between the tip-side sealing portion and the hollow portion. The tip-side sealing portion includes a flat plate portion for grasping formed at an upper portion thereof, and an internal ceiling portion exposed to the interior of the hollow portion. The breakable portion includes an annular smallest diameter portion, and the smallest diameter portion is located near an annular circumferential edge portion of the internal ceiling portion and is located above the annular circumferential edge portion of the internal ceiling portion.

In recent years, in place of glass containers, synthetic resin ampules have been used as containers for containing drugs from the viewpoint of safety against breakage of a container as a result of falling, injury when a container is opened, generation of fragments, etc., as well as from the viewpoint of ease of handling.
A synthetic resin ampule is disclosed in Japanese Patent Application Laid-Open (kokai) No. 2014-69856 (Patent Document 1). The synthetic resin ampule container of Patent Document 1 includes a body portion (1) formed, by biaxial stretch blow molding, into the shape of a tube with a bottom and containing an internal solution (N), a head portion (6) which has the shape of a tube with a top and which is continuously provided to extend vertically from the upper end of the body portion (1), and a weakened portion (10) which is formed at the boundary between the body portion (1) and the head portion (6) and which is broken as a result of relative displacement of the body portion (1) and the head portion (6). A large number of longitudinal ribs (9) are provided on an inner circumferential surface portion (7) to which the peripheral edge of the lower end liquid surface (n1) of a residual internal solution (n) located within the head portion (6) adheres. The longitudinal ribs (9) are juxtaposed along the circumferential direction so as to form an uneven surface portion (8). The uneven surface portion (8) is formed by mixedly forming the longitudinal ribs (9) whose upper ends differ in height position.
Another synthetic resin ampule is disclosed in, for example, Japanese Patent Application Laid-Open (kokai) No. 2013-095436 (Patent Document 2). The synthetic resin ampule of Patent Document 2 is a plastic ampule 1 which includes an ampule body 3 having a spout 8, a stopper portion 5 which is communicatably connected to the ampule body 3 through a neck portion 4 formed along the spout 8, and a head portion 7 which is connected to the stopper portion 5 through a thin plate-shape edge portion 6 projecting outward from the stopper portion 5, wherein the head portion 7 has an arm plate 15 which is flat in a direction intersecting the edge portion 6. A user pinches the arm plate 15 with his/her fingers and pulls the arm plate 15 upward so as to bend the ampule at a position between the ampule body 3 and the head portion 7, while using the neck portion 4 as a fulcrum, thereby cutting and breaking the neck portion 4 to open the ampule.
Also, the applicant of the present application has proposed another synthetic resin ampule disclosed in, for example, WO2017/159832 (Patent Document 3). The synthetic resin ampule of Patent Document 3 includes an ampule body 2m and a drug 6 filled in the ampule body 2m. The ampule body 2m has a tip portion 3, a hollow portion 21 having a drug containing portion 23, and an annular breakable portion 5 provided between a lower portion of the tip portion 3 and an upper portion of the hollow portion 21. The ampule body includes no inner surface protrusion on an inside portion thereof which is located on a side toward the tip portion with respect to the breakable portion. The tip portion is configured such that an inner top surface of the tip portion is located near a plane defined by the annular breakable portion and an inner surface of the tip portion is a low-drug-retention surface.
Also, the applicant of the present application has proposed another synthetic resin ampule disclosed in, for example, WO2017/115752 (Patent Document 4). The synthetic resin ampule of Patent Document 4 includes an ampule body 7 capable of standing by itself and a drug 8 filled in the ampule body 7. The ampule body 7 has a tip portion 3 located on the upper side when the ampule body stands by itself, a hollow portion 71 having a drug containing portion 78, and a breakable portion 5 provided between a lower portion of the tip portion 3 and an upper portion of the hollow portion 71. The tip portion 3 has pressing portions 31 and 32 for guiding a pressing force applied thereto in a predetermined direction when an operation of breaking the breakable portion 5 is performed. The hollow portion 71 has a bottom surface portion 9 for allowing the ampule body to stand by itself. The bottom surface portion 9 has extension portions 41 and 42 extending in the predetermined direction (X direction, Y direction) in which the pressing portions 31 and 32 are guided during the breaking operation.

Drug-filled synthetic resin ampule and synthetic resin ampule body used for same


Provided are a coil unit for electromagnetic forming capable of stably processing a plurality of portions in the longitudinal direction of a tubular member while preventing the contact between the tubular member and a conductor or the contact between the conductors even when the tubular member is long, and a method for producing a formed article using the coil unit. The coil unit for electromagnetic forming includes: a shaft core member made of a resin; a conductor having a wound portion, which is wound around the shaft core member, and a pair of conductor extension portions; an insulating support; and a resin coating layer formed on the outer peripheral surface of the wound portion. In the insulating support, a conductor holding portion for holding the conductor extension portions apart from each other is formed along the longitudinal direction.

Steel members are used as automotive structural parts in many cases from the viewpoint of cost and workability in welding, etc. In response to recent demands for improvement of fuel economy, replacing some of the automotive structural parts made of the steel members with lightweight members has been tried, and applying those lightweight members to not only panel members, but also frame members has been considered.
An aluminum alloy is preferably used as the lightweight member. When a bracket or the like is attached to the lightweight member, using fixation by crimping to join the lightweight member to a counterpart member, such as a bracket, has been considered from the viewpoint of avoiding thermal deformation during welding of the bracket. A method utilizing electromagnetic forming is proposed as the fixing method by crimping (Patent Literature (PTL) 1). A method of partly forming a comparatively long tubular member with application of the electromagnetic forming is also proposed (PTL 2).

Electromagnetic forming coil unit and formed-article producing method using same


Compositions containing a reaction product of gellan gum and polyethylene glycol are disclosed. Methods of making controlled-release gellan gum nanoparticles and methods of using controlled-release gellan gum nanoparticles are also disclosed.

Gellan gum is an exocellular, microbial polysaccharide produced by Pseudomonas elodea and has been employed as a food additive. According to the FDA (21 CFR §172.665) gellan gum "may be safely used as a direct food additive for human consumption." The structural formula for gellan gum has been studied extensively and reported to consist of repeating tetrasaccharide units with the following structure:
which can also be represented by:
-3-β-D-glcp-(1-4)-β-D-glcpA-1-4)-β-D-glcp-(1-4)-α-L-rhamp-(1-
wherein "glcp" designates glucose, "glcpA" designates glucuronic acid, and "rhamp" designates rhamnose.
Gellan gum is commercially available in a clarified form under the trade designation KELCOGEL® for foods and industrial products and under the trade designation GELRITE® from CP Kelco, A Huber Company, (J.M. Huber Corporation, Edison, N.J.) for microbiological media, plant tissue culture, and pharmaceutical applications. Gellan gum has the potential to form gels in situ in the presence of mono- or divalent cations.
Gellan gum microparticles may be useful in encapsulating both bacteria and drugs (see, for example, U.S. Pat. Nos. 4,822,534 and 5,516,543). However, these gellan gum formulations of the prior art result in low biodistribution of encapsulated material, a feature attributed to susceptibility of the gellan gum polymer to degradation, which could present potential toxicity problems for applications such as anti-cancer drug delivery.
The physiological environment of tumors necessitates drug delivery systems that are capable of maintaining a controlled-release profile in acidic conditions. Thus, better formulations of gellan gum with improved controlled-release characteristics are needed for active drug targeting in vivo.

Gellan-gum nanoparticles and methods of making and using the same