text:
|Publication number
|Publication type
|Application number
|Publication date
|Mar 20, 1984
|Filing date
|Jan 11, 1982
|Priority date
|Jan 12, 1981
|Fee status
|Also published as
|Publication number
|Hans-Bernd Schmittmann, Alfons Thier
|Original Assignee
|Charles M. Wiersma, Jack G. Wiersma
|Export Citation
|BiBTeX, EndNote, RefMan
|Referenced by (39), Classifications (32), Legal Events (6)
|External Links: USPTO, USPTO Assignment, Espacenet
The invention relates a fire retardant and compounds based thereon such as to flameproof or fire retardant plastic, coatings and the like. Such plastics are usable for example as building materials, in seating, or the like. Coatings or stains could be useful in making an underlying substrate more fire resistant.
Building materials and building components of plastics are frequently utilized for the interior construction of renovated rooms. For example, wall protection panels, wall protection strips, handrails and like building elements of semi-hard or soft, flexible and elastic plastic foams are used for lining of walls, recesses, wall projections, swinging doors or the like, in particular in gymnasiums and sports halls or hospitals. Development in this field has led to building elements which are as a rule resistant to impact, scratching, abrasion and breakage and also nearly decay-proof, ageing-resistant against acids and alkalis, free from odor, and also developing no gases. They can be colored and cut or sawn, and are adhered to, e.g., concrete, masonry, wood or plaster with special adhesives. They are washable and easy-care.
Sound-absorbing elements can also be made of said building materials, so that the building materials have very versatile uses for the interior structure of spaces. Particularly outstanding building components in the above sense are, for example, described in Deutsche Gebrauchsmuster (DE-GM) 75 30 775. These are constructed of a foamed plastic core with relatively dense, thin surface layers of the same plastic material, the surface layers or edge zones being materially connected to the core. Such a building element preferably consists of a semi-hard or soft, elastic, flexible, foamed and solidified polyurethane, the surface layers having the same material, namely polyurethane. The polyurethane is foamed during the production of the building element in a mold in a conventional manner. For such building elements made of polyurethane it is to be emphasized that they have quite excellent heat-insulating properties.
The building materials described can, of course, also be used for cushioning, for protection or for decoration or the like for other elements such as, e.g., furniture or appliances or the like and thereby fulfill the same or other objectives. Similarly, the fire retardant of the present invention can be used in coatings and stains.
The usability of many materials such as building materials, seating cushions, and the like can be problematic in cases in which high flame retardancy is required or desired. For example, a flameproof material according to DIN 4102 Building Material Class B1, a West German designation, is very difficult to obtain in plastic. According to DIN 4102, and comparable codes in other countries, the burning behavior of building materials and building components is standardized, the building materials being divided into two main classes. Main Class A relates to incombustible materials. Main Class B contains, in contrast, the combustible building materials. The building materials with which the present invention is concerned fall into Building Material Class B. This class is further divided, according to the West German standard, into the following subclasses:
B1 Flameproof building materials
B2 Normally inflammable building materials
B3 Easily inflammable building materials.
The described, known building materials as a rule belong to the easily or normally inflammable building materials and are thus counted in Classes B2 and B3. Only a few plastics building materials are flameproof (Class B1) and even fewer are incombustible (Class A).
The object of the invention is to make easily inflammable and/or normally inflammable plastics materials flameproof, so that building components or other items produced from them satisfy the conditions of the West German DIN 4102 standard, and comparable standards in other countries, and can be classified in Class B1.
It is known that building materials of plastics, in particular, of polyurethane foam, can be made flameproof when asbestos is used as a filler. The processing of asbestos is however partially prohibited, due to the danger of asbestos, so that the use of building material parts utilizing asbestos is no longer permitted. In addition, the filler causes a hardening of the plastic foam, so that some desirable properties such as flexibility and elasticity of the building components can be lost. Research on the use of other fireproof fillers has up to now been abortive. None of the products satisfied the requirements of the DIN 4102 or any comparable standard.
It is further known to reduce the inflammability of plastics by the addition of chemicals. For example, phosphates or borates are used, mixed into the plastic mass. These measures in fact lead to more difficult flammability. However even this is not substantial enough to fulfill the requirements for the building materials, e.g., the conditions of the West German DIN 4102 standard. Possibly building materials of the kind described can be produced which are sufficient for Class B2. Inorganics such as antimony trioxide are also used, but are expensive.
The object of the invention is to provide fire retardant plastics, which can be produced easily and without danger, and which are sufficient for Class B1 of DIN 4102, and comparable tests in other countries, without the desired advantageous properties of the plastics being substantially impaired or lost.
This object is achieved by adding to a plastic or other composition, chemicals which undergo fractional endothermic reactions under the action of heat over a wide range of temperatures. The term fractional endothermic reaction refers broadly to fractional melting and/or fractional decomposition and/or fractional chemical reaction, which absorbs heat. The first endothermic reaction is advantageously to begin at about the melting point and/or ignition point of the plastic.
This is preferably achieved by adding to the plastic composition ammonium polyphosphate, monoammonium phosphate, an anhydrous inorganic compound capable of hydration, most preferably anhydrous borax, an inorganic compound which releases water when heated, most preferably borax decahydrate, and a urea polymer, most preferably melamine.
The term `fractional`, in the sense of the invention, refers to the reaction behavior of the material in temperature stages, e.g., melting, in which melt phases, for example, are formed at different temperatures from the solid of which, e.g., a building part or other plastic member or surface is composed. The melt phases, which occur in temperature stages or at different temperatures, are to arise, according to the invention, from endothermic reactions, so that heat energy is consumed. The same holds for decomposition reactions and the reactions for formation of new compounds or phases, these being endothermic processes according to the invention, consuming heat. The endothermic reactions are preferably to occur in succession, as for example a decomposition product being formed at 90� C. with consumption of a given amount of heat. When the decomposition product has been formed in a nearly complete amount, the temperature in the building material or in the decomposition zone rises. On reaching, for example, 100� C., a melt phase results, mainly in the decomposition zone, and again occurs endothermally and can form as long as the melting is available in the building material or in the decomposition zone. After this, the temperature in the reaction zone further rises until the next endothermic reaction provided occurs, which can be a phase change, e.g., a solid state reaction. The endothermic reactions can, of course, also all be melting processes or solid state or decomposition or other reactions; it depends here solely on the required temperatures for initiation of the processes being stepped in height and on sufficient heat energy being consumed, so that the plastic material is not heated so much below or behind or in the region of the reaction zone that the reaction zone, which acts as a protective zone, flows away or slips off or floats off. A building material, for example, made from polyurethane and containing the fire retardant of the present invention thus immediately fulfills the conditions of the West German DIN 4102 standard for the Class B1 and in practice also resists high temperatures for a given time.
The invention preferably provides for the use of inorganic salts, most preferably those discussed above, which ensure fractional reactions, e.g., by melt formation at predetermined temperatures and by the consumption of a relatively large amount of heat energy. The salts can also, however, enter into compounds with the plastics (in appropriate circumstances, like an alloy), the compound formation occurring with large consumption of heat and/or the compound itself melting with high heat comsumption. To this extent, the addition of a salt can be sufficient to effect the fractional, endothermic reactions to a sufficient extend (compound formation and melting or decomposition or the like).
FIG. 1 is a cross section of an article made in according with one aspect of this invention.
According to a preferred embodiment of the invention, ammonium phosphate, ammonium polyphosphate, an inorganic compound which yields water when heated, most preferably borax, anhydrous borax and a urea polymer, most effectively melamine, are particularly effective as a fire retardant additive for plastics. Urea can also be added, but the most important ingredients seem to be the foregoing.
The borax used is the decahydrate. Other inorganic compounds which yield water when heated are operable in the broadest sense of the invention. Hence, borax pentahydrate is operable. Boric acid is operable, since it loses water in stages as it is heated. However, borax decahydrate or a hydrate showing a comparable endothermic reaction upon releasing water is the most preferable component.
Indeed, the combination of borax decahydrate and anhydrous borax yields surprisingly effective results. Hence, this specific combination is especially preferred.
As indicated above, the most preferable urea polymer employed is melamine. However, other urea polymers can be substituted. Cyanurdiamide (ammeline) and cyanuramide (ammelide) and decyandiamide are examples.
The five main ingredients should have a relatively uniform particle size so that they can be thoroughly mixed together. To a point, a smaller particle size is preferred. However, one should not mill material such as the borax decahydrate too fine or one will drive out the water of hydration during the milling process.
The anhydrous borax typically has to be milled in a hammer mill until it will pass through a #325 screen. This is approximately the particle size at which the borax decahydrate is commercially available. Preferably, all of the particles of the five main ingredients should pass through #325 mesh screen, or in other words, be less than 10 microns in particle size.
Uniformity of particle size is important in insuring uniform cell size in blown plastic materials. The smaller particle sizes, i.e., less than 10 microns, are desirable for several reasons, not the least of which is that they have much less tendency to sink to the bottom of any plastic resin mixture. Also, the finer particle sizes tend to be more efficient, thereby enabling one to use less retardant material and still obtain the same fire retardant ratings. Finally, the smaller particles will have less tendency to clog automated processing and molding equipment.
None of the above ingredients are presently considered to be hazardous substances or carcinogenic. This is in sharp contrast to retardants such as antimony trioxide which is now considered highly suspect from a human factors standpoint.
In using the present invention in connection with plastic foams, it does appear important to avoid the use of water blown systems. The water causes the fire retardants to settle to the bottom of the foam during blowing, thereby leaving the upper portion of the foam component unprotected. Hence, freon blown systems or alternative nonwater blowing systems should be employed where the fire retardant of the present invention is used in a foamed plastic.
The presence of water does not appear detrimental to the performance of the fire retardant per se. Thus, the fire retardant of the present invention has been found very effective in water borne coatings, as for example aqueous coatings prepared in a vinylidene chloride latex binder.
The fire retardant must be thoroughly mixed with the plastic resin or other material whose fire retardancy it is to enhance. When mixing the fire retardant with a polyol in a polyurethane system, a 3000-4000 rpm mixer seems to be most effective in insuring a regular mixture and avoiding air bubbles. In any mixture, care must be taken to promptly use the composition and effect curing in order to prevent the fire retardant component from settling to the bottom of the material.
In foamed plastic systems, one must also take care to cure the system rapidly in order to prevent the foam from collapsing due to the increased weight added by the presence of the fire retardant. Hence, a so-called "hot cure" is preferred in order to maximize the speed of curing of the foam. A "hot cure" is typically effected by utilizing an external heat source such as an oven. The speed of curing can also be increased to some extent by increasing the amount of catalyst used in the system. This is applicable in either molded or free rise foam applications.
The present fire retardant can be used in conjunction with some other fire retardants. For example, it has been used in latex coatings in conjunction with intumescent additives. In such systems the fire retardant of the present invention may be desired as a thickener, as well as a fire retardant, in place of combustible organic thickeners.
However, care must be taken when mixing this retardant with other retardants. Some retardants currently used is urethane foams, for example, appear to inhibit the effectiveness of the present invention.
The invention can be implemented in an outstanding manner in building materials and seating of semi-hard to soft polyurethane foam. The use of such foams as a building material for building parts for the interior construction of spaces is known (DE-GM 75 30 775).
A particularly suitable recipe for a polyurethane building material (without the fire retardant of this invention) has the following components:
48 through 58, preferably 50 through 55, wt.% polyol
17 through 22, preferably 18 through 20, wt.% isocyanate (hardener)
0 through 1, preferably 0.2 through 0.6, wt.% accelerator, e.g., DBTL
15 through 50, preferably 20 through 30, wt.% blowing agent (Arkton).
On mixing these materials together there is known to arise a so-called semi-hard foam structure with a relatively dense outer skin. If the foaming is carried out in a mold supported on all sides, components are obtained with a foam core and relatively dense surface layers (DE-GM 75 30 775).
The fire retardant of the present invention is then mixed with the polyol in amounts sufficient to yield a final product in which the fire retardant is from about 20 to about 64% by weight of the overall composition. In polyurethane foam, 20% of the fire retardant by weight will cause the foamed product to have a Class II rating by accepted United States standards. 29% fire retardant in polyurethane foam will yield a Class I rating by the same standards. Further increases do not substantially improve fire retardancy, but may be desirable for other reasons, as for example to provide increased filler, increased thickening, increase stiffness and the like. In epoxy coatings, our fire retardant serves as a thickener and may eliminate in some applications the need for any additional thickeners.
The premix of the other reactants is then added and the mixture is processed in the usual way. A combination of additives consisting of ammonium polyphosphate, monoammonium phosphate, borax, anhydrous borax, and melamine is here preferred. The amounts added are regulated respectively according to the desired endothermic heats of reaction. The amounts of ammonium polyphosphate and anhydrous borax are selected such that these materials act as nucleating agents for the reaction products from monammonium phosphate and borax, and favor the desired reactions or hinder undesired reactions. The action of these materials even in small amounts, possibly as nucleating agents and/or catalysts or the like is surprising. Their addition leads to particularly good results in combination with the other stated materials.
In some applications, it has been found that as little as 15 to 20% fire retardant is extremely effective. Epoxy coating are an example of such an application.
It is particularly advantageous to add the additives in the following proportions to one another, i.e., based on the total amount of the additives:
2-10, preferably 5-8, wt.% ammonium polyphosphate
10-50, preferably 30-40, wt.% monoammonium phosphate
4-12, preferably 7-10, wt.% anhydrous borax
12-40, preferably 20-30, wt.% borax
12-40, preferably 20-30, wt.% melamine
0-20, preferably 5-10, wt.% urea.
Dispersion of the additives takes place, according to a further embodiment of the invention, with the addition of pyrogenic, hydrophobic, and in particular siliconated, silicic acid. It is also advantageous to mix in a silane or silicone or to add a stearate or another hydrophobizing medium. The silicic acid is preferably added in amounts of 0.1-2.5 wt.%, based on the amount of additives. Because of a considerable improvement in dispersibility, hydrophobizing also acts to improve the flowability of the additives when they are mixed in and to improve the stability properties during storage. In addition hydrophobizing is effected and counters entry of water during foam formation, which is problematical in particular in the production of a polyurethane foam.
A further process variant according to the invention proposes the addition of diluents which are preferably neutral to the reaction, for example alcohols, preferably n-butanol or methylene chloride, up to about 50 wt.% of the premix, so that the processability of the mixture is improved by liquefaction. The structure and properties, e.g., the elasticity, can also be influenced. Methylene chloride also acts here in an advantageous manner as a blowing agent.
The new flameproof polyurethane foam is in particular suitable for the production of plate-form cushioning components, handrails, sound absorbent panels according to DE-GM 75 30 775, and wall protection strips. The properties of the new building material are substantially unchanged, apart from inflammability, in comparison with the conventional building materials; the additives have produced no substantial negative effects. The structure of the new building material of the building components is characterized by the presence of the additives in the solid webs and the surface layers. The additives are analyzable and hence sufficiently individualized. The choice of material conditions in a surprising manner the particular applicability of the building components as flameproof building elements.
A building component according to the invention is explained in more detail with reference to the drawing. The illustration shows a part of a cushioning panel, which in particular also has notable sound insulating properties.
The panel has a highly elastic core 1 of foamed polyurethane, consisting of predominantly closed spherical cells 2 and the solid webs 3. The surface layers 4 and 5 are relatively densely structured, likewise consist of polyurethane, and are materially integrally connected to the core 1. Holes 6 can be stamped or bored or the like through the surface layer 4 into the core 1, and serve to absorb sound. It is important that the solid webs 3 contain the additives, which are schematically shown as points 7. It is also important that if closed cell plastic foams, rather than open cell are used, holes should be provided which open at the surface of the foam structure in order to facilitate degassing, i.e., the escape of gases, when the structure is heated.
The invention is clarified below by means of examples.
A basic mixture, consisting of
53.0 wt.% polyol
20.0 wt.% isocyanate
0.4 wt.% accelerator
17.6 wt.% Freon blowing agent,
from which the foam building components can be produced which do not correspond to the conditions of Class B1 of DIN 4102, had approximately equal amounts of the following additive formulation mixed into it, the additives being added to the polyol:
7 wt.% ammonium polyphosphate
35 wt.% monoammonium phosphate
25 wt.% borax
8 wt.% anhydrous borax
25 wt.% melamine.
Foaming occurred in a mold supported on all sides, so that cushioning panels with the dimensions 100 cm�19 cm�2 cm resulted. Four panels were subjected to the test conditions according to West German standard DIN 4102, Part 1, point 6.1.2, with the result that the residual length in the middle was 17 cm and only a maximum gas temperature of 139� C. occurred, so that the conditions for a building material B1 according to DIN 4102 were fully fulfilled.
The formulations for polyrurethane foam and fire retardant as set forth in Example 1 above were substantially the same for Example 2. However, the first retardant comprised only 29% of the composition by weight rather than 50% by weight as in Example 1. The resulting foam yielded a Class I rating in accordance with accepted United States fire retardant standards. This rating is determined in accordance with an ASTM test known as the "Butler Chimney Test." The test sample is suspended in a cylinder and is exposed to a Bunsen burner flame at 700� F. Once the test sample is ignited, the material is pulled away and the following are measured:
(1) The height of the flame in the chimney after the burner is pulled away;
(2) The amount of smoke generated after the burner is pulled away; and
(3) The amount of weight loss in the sample after burning has ceased.
The materials of Examples 1 and 2 were utilized, but only 20% by weight of fire retardant was employed in the overall resulting foam. The material achieved a Class II rating in accordance with accepted United States fire retardant standards, as determined by the "Butler Chimney Test" described in Example 2.
Approximately 20% by weight of fire retardant was introduced into an epoxy coating composition. A small patch was painted onto a substrate and allowed to cure. The coated substrate was placed at one end of a four foot tunnel and then subjected to an exposed blow torch flame and wind in order to determine how far flame from the epoxy would spread down the tunnel. No flame spread occured. There was also a drastic reduction in smoke and no off-gasses were given off as is the case when brominated chemicals are used as fire retardants.
The procedure of Example 4 was repeated with a polyester coating containing approximately 20% of the fire retardant of Example 1. The polyester material included glass fibers since it is a typical fiberglass patch formulation. Again, no flame spread resulted during the test period.
A flexible urethane foam containing 29% by weight of fire retardant in accordance with the present invention was subjected to Underwriters Laboratory Test #94 for flame retardancy. In this test, a 1"�6"�1/8" strip is suspended over a Bunsen burner for 10 seconds and is then removed from the flame and timed to determine how long it will continue burning until it self-extinguishes. Our sample did not even ignite when exposed to the flame. No burning occured at all.
The procedure of Example 6 was repeated only on a sample of rigid urethane foam containing approximately 29% by weight of the fire retardant in accordance with the present invention. This sample did ignite when exposed to flame, but no burning continued after the sample was removed from the Bunsen burner flame.
In this test, the so-called "O.I." test, a 1"�1/2"�6" piece of flexible urethane foam containing 29% by weight of fire retardant in accordance with the present invention was placed in a cylinder which is purged with nitrogen. An open flame is then held over the product and oxygen is introduced into the system until ignition is achieved. A plastic material, such as a flexible foam, is considered acceptable, if a measure of 17 on the "O.I." test scale is achieved. The flexible foam sample made in accordance with the present invention did not ignite. The scale does not exceed 50 and hence the test was discontinued at this point with the sample still in tact.
The "O.I." test of Example 8 was repeated with a rigid polyurethane sample containing approximately 29% by weight of the fire retardant of the present invention. Ignition did not occur until the oxygen level reached approximately 36 on the "O.I." test scale.
A flexible urethane foam containing approximately 29% by weight of fire retardant was subjected to a radiant panel test. In this test, a panel is heated to 1000� F. and a 3"�3"�1" sample of foam is placed in front of the panel for 10 minutes. The sample is then subjected to three small propane flames at 1700� F. each. The time which it takes for the burning of the samples to stabilize, as determined by rate of smoke emission, and the amount of unburned sample then remaining are then determined. In the optimum prior result of which we are aware, the material stabilized at 10 minutes and was 100% consumed by the conflagaration. Our test sample stabilized at 15 minutes, at which time there was still in excess of 50% of undamaged foam left in the sample.
An epoxy coating was prepared containing 20% by weight fire retardant made in accordance with this invention. A substrate was coated and the coating cured at unusually high temperatures, i.e., 450� F. The epoxy did not ignite or degrade in any way during this curing.
After curing, the sample was heated in a 550� F. oven for twenty minutes. No ignition or degradation occurred.
It is surprising that the addition of salts and the other stated materials leads to reactions under the action of high temperatures, consuming obviously larger amounts of heat than the additives require for melting or decomposition or the like, and that flameproofness can thus be achieved. An explanation has not yet been found for this unexpected property of the new plastics, because, e.g., the melting points or decomposition points of some of the stated additives lie much higher than the temperature stages of the corresponding fractional reactions according to the invention. The material made with the present fire retardant seems to develop an insulating carbon char which helps the material resist further degradation and thereby further exposure to flame. A plastic foam for example, which contains this fire retardant resists melting when exposed to heat. So-called "fall out" of burning or hot material is thereby minimized.
There is a major reduction in gaseous by-products, i.e., "off-gases," and smoke when the present fire retardant is used, as compared to other retardants. The brominated retardants give off considerable gaseous by-products for example. Further, the smoke resulting from using the present invention is white, not thick and black. In part the reduction in smoke and off-gases is a result of the nature of the fire retardant per se, and in part because of the significant reduction in combustion of the component which has been fireproofed.
Besides the action, as described above, of the said mixtures of additives on plastics, the same action also occurs on synthetic resins such as, for example, epoxy resins, vinyls and latex products such as, e.g., latex paints, other paints and also in strains applied to wood building materials. Indeed, the fire retardant per se of the present invention can be incorporated directly into the body of so-called pressed wood, also known as chipboard. The fire resistance of the resulting board is significantly increased.
Naturally in utilizing the fire retardant of the present invention in various different compositions, other processing adjustment may have to be made to accommodate the changes in the nature of the material being processed. For example, when the fire retardant of the present invention is used in a polyurethane material, the material tends to be more viscous. This may require one to alter the pump, for pumping the material to a nozzle, from a rotary pump to a rotary screw pump. Larger ports and larger hoses may have to be provided to accommodate the polyol with the fire retardant in it. These facts will, of course, be apparent to those skilled in the art.
It will also be appreciated by those skilled in the art that changes and modifications of the preferred embodiments can be made without departing from the spirit and broader aspects of the invention as set forth in the appended claims.
|Citing Patent
|Filing date
|Publication date
|May 3, 1984
|Nov 5, 1985
|Mobay Chemical Corporation
|Polyether polyurethane prepolymers containing finely divided inorganic particles and cast elastomers made therefrom
|Jul 11, 1986
|Mar 8, 1988
|Bayer Aktiengesellschaft
|Flame-retarding sealing compounds
|May 21, 1987
|Jul 12, 1988
|Reeves Brothers, Inc.
|Flame retardant melamine containing polyurethane foam
|May 21, 1987
|Jul 12, 1988
|Reeves Brothers, Inc.
|Melamine cured polyurethane foam with improved properties
|May 21, 1987
|Apr 4, 1989
|Reeves Brothers, Inc.
|Rapid cure of polyurethane foam with ammonium containing materials
|Jul 14, 1987
|May 16, 1989
|Bayer Aktiengesellschaft
|Preparation of intumescent materials for coatings and building elements
|Oct 20, 1988
|Oct 3, 1989
|Firestop Chemical Corporation
|Fire protected foamed polymeric materials
|Jun 17, 1988
|Nov 7, 1989
|Macmillan Bloedel Limited
|Chemically treated wood particle board
|Oct 31, 1988
|Feb 12, 1991
|Tag Investments, Inc.
|Polymer fire retardant
|Jul 17, 1989
|Mar 12, 1991
|Blount David H
|Process for the production of flame-retardant polyurethane products
|Dec 15, 1994
|Apr 9, 1996
|Hickory Springs Manufacturing Company
|Polyurethane foams
|Jul 1, 1994
|Jul 2, 1996
|Societe National Des Poudres Et Explosifs
|Inorganic resins, process for their preparation and materials for heat protection
|Dec 15, 1994
|Jul 16, 1996
|Hickory Springs Manufacturing Company
|Polyurethane foams
|Jun 5, 1995
|Oct 29, 1996
|Hickory Springs Manufacturing Company
|Fire-retardant polyurethane foams and method of producing
|Dec 4, 1997
|Feb 29, 2000
|Masonite Corporation
|Method of making cellulosic composite articles
|Dec 1, 1997
|Mar 28, 2000
|Fireguard Scandinavia As
|Fire retarding composition and a method for impregnation of a combustible material
|Mar 26, 1999
|Jan 2, 2001
|Kenneth R. Hallo
|Method for dissipating heat
|Jan 17, 2001
|Jun 10, 2003
|Ernest Jeffrey Sosebee
|Method and composition for treating volatile waste
|Jul 19, 2005
|Jun 30, 2009
|Sierra Pine Ltd
|Fire retardant composite panel product and a method and system for fabricating same
|Jun 11, 2007
|Jan 26, 2010
|Sierra Pine Ltd.
|Fire retardant composite panel product and a method and system for fabricating same
|May 17, 2011
|Scott Powers
|Railway tie of non-homogeneous cross section useful in environments deleterious to timber
|Dec 17, 2008
|Nov 13, 2012
|U.S. Borax Inc.
|Fire resistant cellulosic materials and method of making the same
|Jan 8, 2013
|Ashtech Industries, Llc
|Utility materials incorporating a microparticle matrix
|Apr 6, 2011
|Apr 30, 2013
|Jonathan Jaffe
|Railroad tie of non-homogeneous cross section useful in environments deleterious to timber
|May 14, 2013
|Ashtech Industries, Llc
|Shear panel building material
|May 21, 2013
|Ashtech Industries, Llc
|Sound attenuation building material and system
|Nov 4, 2009
|Nov 26, 2013
|Ashtech Industries, Llc
|Utility materials incorporating a microparticle matrix formed with a setting agent
|Jan 7, 2013
|Apr 7, 2015
|Ashtech Industries, Llc
|Utility materials incorporating a microparticle matrix
|May 20, 2013
|Jul 7, 2015
|Ashtech Industries, Llc
|Sound attenuation building material and system
|Jul 19, 2005
|Nov 10, 2005
|Graham Hume
|Fire retardant composite panel product and a method and system for fabricating same
|Apr 25, 2007
|Oct 30, 2008
|Scott Powers
|Railway tie of non-homogeneous cross section useful in environments deleterious to timber
|Mar 21, 2008
|Jan 1, 2009
|Kipp Michael D
|Utility materials incorporating a microparticle matrix
|Sep 25, 2008
|Apr 30, 2009
|Kipp Michael D
|Sound Attenuation Building Material and System
|Dec 17, 2008
|Jun 18, 2009
|Schubert David M
|Fire resistant cellulosic materials and method of making the same
|Feb 19, 2009
|Sep 3, 2009
|Lanxess Deutschland Gmbh
|Sound-deadening insulating materials with high fire-resistance time
|Jul 21, 2011
|Lanxess Deutschland Gmbh
|Sound-deadening insulating materials with high fire-resistance time
|Jan 7, 2013
|Aug 15, 2013
|AshTech Industries LLC
|Utility Materials Incorporating a Microparticle Matrix
|Nov 16, 2009
|May 25, 2011
|H2V Bvba
|Fire retardant for polyurethane foams
|Nov 16, 2010
|Mar 8, 2012
|H2V Bvba
|Fire retardant for polyurethane foams
|U.S. Classification
|252/609, 428/921, 521/907, 106/18.13, 521/906, 252/601, 106/18.14, 521/106, 521/103
|International Classification
|Cooperative Classification
|European Classification
|Sep 1, 1982
Owner name: WIERSMA, CHARLES M. PRO-AM CORPORATION, 66 OTTAWA
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNORS:SCHMITTMANN, HANS-BERND BER;THIER, ALFONS;REEL/FRAME:004030/0005
Effective date: 19820402
Owner name: WIERSMA, JACK G. PRO -AM CORPORATION, 66 OTTAWA N.
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNORS:SCHMITTMANN, HANS-BERND BER;THIER, ALFONS;REEL/FRAME:004030/0005
Effective date: 19820402
|Aug 14, 1984
|Certificate of correction
|Aug 27, 1987
|Fee payment
Year of fee payment: 4
|Oct 22, 1991
|Maintenance fee reminder mailed
|Mar 22, 1992
|Lapse for failure to pay maintenance fees
|May 26, 1992
|Expired due to failure to pay maintenance fee
Effective date: 19920322


text:
Irish dancers mix with circus clowns
Dancers from the Ryan Irish Dance Academy and the Inishfree School of Irish Dance taught clowns from Ringling Bros. and Barnum and Bailey Circus a few moves. The event, in the spirit of St. Patrick's Day, was held at Nassau Coliseum. Videojournalist: Jim Staubitser (March 15, 2013)
If Hillary Clinton is elected, what should we call Bill? Nassau Junior Firefighters 2nd annual camp LI shop owner says election 'cup count' has never been wrong Newsday reporter talks Obama, Biden, Bloomberg DNC speeches Long Island delegates react to Barack Obama's DNC speech New York delegates react to Michael Bloomberg's DNC speech Puppy of the day: Mike Giuliani: Probable cause for Clinton indictment Bloomberg endorses Clinton at DNC Kaine: Barack gave us hope, and now Hillary is ready Obama: 'Nobody more qualified than Hillary' Joe Biden on Trump: 'Malarkey'

subset: commoncrawl


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Chance Rollins, who ranks second in the jockey standings at Golden Gate Fields' fall meeting, injured his left shoulder in a spill in the first race Sunday and will be sidelined for two to three weeks.
Rollins came off his mount, Jamestown Flash, when the 4-year-old gelding broke his right front ankle at the top of the stretch. The rider was clipped by a second horse, Yak Attack.
"He has a tiny undisplaced fracture in the middle of his left shoulder blade, which is where he was kicked," reported Dr. David Seftel, track physician at Golden Gate Fields. "He also has some bruising of his left knee."
Rollins has 30 wins at the fall meeting. Perennial champ Russell Baze tops the jockey standings with 39 victories.
Jamestown Flash was euthanized.
Rider Rollins Sidelined After Golden Gate Fall
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Ticket Policies
Rice Student Information
Will Call Policy
All ticket orders placed 7 or more business days before the event will be shipped unless the person purchasing the tickets request for them to be held in Will Call. Tickets purchased less then 7 business days in advance will automatically be held in Will Call.
Any persons picking up tickets at Will Call will be required to show a photo ID. Will Call opens an hour and a half before game time.
3rd Party Will Call
The Rice University Ticket Office is pleased to accept your outside will call for your convenience.
We ask that you completely fill out the Rice Athletics will call envelope provided by the Ticket Office. Please indicate the name of the person picking up the tickets, the number of tickets and your name as the owner of the tickets. The individual picking up the tickets must have a photo ID to obtain the tickets.
Food and Drink Policy
No outside food or drinks are allowed in any of Rice University Athletic venues.
"R" Room Access
The "R" Room is located in the south end zone and is available to Rice Athletics Fund members at the Sammy Level ($500 & above) and active "R" Association members. This area allows fans to watch great Rice Owls football action from the comfort of being indoors with televisions to watch other games at the same time. There is a cash bar available, snacks and this area opens an hour and a half before game time.
Stadium Club Access
The stadium club is located in the press box on the west side of the stadium. This area is available to Rice Athletics Fund members at the President Level ($5,000 and above). This area allows fans to watch great Rice Owls football action from the comfort of being indoors with televisions to watch other games at the same time. There is complimentary food and drinks in this area.
Football Away Game Ticket Orders
Rice University receives a limited number of tickets for regular season away games. All tickets will be assigned based on the allocation policy set forth for postseason play. Requests must be received two weeks in advance of the game. Tickets will be mailed approximately two weeks prior to each game. For information on ordering tickets, Rice Athletic Fund members or season ticket holders may call the Rice Ticket Office at (713) 522-6957. Only current season ticket holders or donors can order for away games.
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07/21/2016 - W. Track - Rice University women's track & field/cross country head coach Jim Bevan announced on Tuesday the creation of the Emily Massad Rabbitt Award.
Rice Remembers Hally Beth Poindexter
07/20/2016 - General Release - Dr. Hally Beth Walker Poindexter (Rice, 1947), who worked tirelessly to establish women's intercollegiate athletics at Rice University, will ...
Lyons Tabbed by C-USA Coaches
07/20/2016 - Football - Rice senior linebacker Alex Lyons, who has led the Owls in tackles in each of the last two seasons, has been named to the 2016 preseason Coaches...
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Langley Announces 2016-17 Non-Conference Schedule
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Which Emoji Describes Crushing Student Debt?
Only 15 more months until the election.By Dayna Evans
Only 15 more months until the election.By Dayna Evans
But it sounds like she's already deleted all of her emails.By Margaret Hartmann
Wisdom from the BasedGod.By Sean Fitz-Gerald
And Kanye.By Margaret Hartmann
Guardian columnist says yes.By Jonathan Chait
It's not a criminal inquiry, and Clinton herself is not being targeted, so far.By Margaret Hartmann
New polls show Hillary's favorability plummeting among white women.By Annie Lowrey
The socialite and First Lady–beloved designer has died at 85.By Véronique Hyland
She may be part of a political dynasty, but unlike some other candidates, her parents weren't.By Margaret Hartmann
According to the Times, his associates have been calling potential supporters and donors.By Chas Danner
The State Department releases another batch of Hillary Clinton's emails.By Jaime Fuller
They blasted the paper for "egregious" errors in a report about a criminal inquiry into Clinton's emails.By Margaret Hartmann
A government review finds that she may have sent classified information on her personal email account.By Margaret Hartmann and Jaime Fuller
In Cedar Rapids, Iowa.By Caroline Bankoff
Clinton would also beat Michelle Obama and Jon Stewart.By Jaime Fuller
Isn't it ironic?By Adam K. Raymond
The presidential hopeful is no stranger to the "aesthetic tax" on women.By Jessica Roy
It's the biggest mystery of her platform, and she isn't saying.By Jonathan Chait
"I'm leaning into the idea that they're from Arkansas, and there's some trashy nugget of her that lies behind Hillary's exterior."By Nate Jones
Her sit-down with CNN doesn't count.By Frank Rich


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DNC Starts With Bernie Sanders, Cory Booker, Michelle Obama, Elizabeth Warren
Group Livid Over Gay Couple On 'Loud House' Voiced By Wayne Brady, Michael McDonald
Darren Criss, Chita Rivera Stage Concert To Benefit Orlando LGBT Community
Raul Castillo Hopes 'Looking' Character Will Lead To Greater Hollywood Diversity
Hillary Clinton: Donald Trump '100% Wrong' On LGBT Rights
Prince Harry, Elton John: Young People Needed To Combat HIV Epidemic
Social conservatives in Connecticut say
they oppose a bill that would ban transgender discrimination because
the measure would leave women and children vulnerable to attacks from
sexual predators.
The proposed bill would outlaw
discrimination on the basis of gender identity in the areas of
employment, housing, public accommodations and credit.
At a House Judiciary Committee hearing
on the bill that lasted more than 11 hours, Peter Wolfgang, president
of the socially conservative Family Institute of Connecticut,
referred to the measure as the "bathroom bill."
"I am here today to oppose bill 6599,
An Act Concerning Discrimination, or as it is known to us the
'bathroom bill,'" Wolfgang
told lawmakers.
"This bill is a radical assault on
the right to privacy and safety of all women and children on behalf
of one of the smallest special interest groups. Nothing would
prevent a sexual predator from pretending that he is confused about
his sex to gain access to vulnerable women and children in what
should be safe spaces for their accommodation and health."
The committee's chairman, Democratic
Representative Gary Holder-Winfield, grilled Wolfgang on his
"You said if this bill passes,
nothing would prevent the sexual predators from taking the actions
that you suggest might happen," he said. "What prevents them
from doing that now?"
"Well they'd certainly have more of a
reason to do it," Wolfgang answered.
"But my question to you is, what
prevents them from doing it now?" he repeated.
"Well, I mean, you know, there are
laws that prevent crimes, obviously, from taking place in bathrooms
in general. But, I mean, why give sexual predators a pretext? Why
give them an excuse to say, 'Look, I'm transgendered and that's why I
went into the women's bathroom.' Obviously it's – you know, there
are laws for registered sex offenders."
At Holder-Winfield's pressing Wolfgang
eventually agreed that laws against such crimes would continue to be
enforced even if the bill became law.
Governor Dan Malloy, a Democrat, has
said he'll sign the bill if approved by lawmakers.
similar measure in Maryland dropped its public accommodations
language in an effort to boost support.
On Top Magazine


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Snowman with Lamppost Christmas Ornament
Personalized Christmas Ornament
Dimensions: 3 1/4" x 4 1/4"
Material: Resin
This lantern lights the way for the Christmas carolers on a cold and blustery day in winter.
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text:
Lyrics Depot is your source of lyrics to Stormy Weather by Diana Ross. Please check back for more Diana Ross lyrics.
Stormy Weather Lyrics
Artist: Diana Ross
Album: An Evening With Diana Ross
(Ted Koehler/Harold Arlen)
I don't know why
There's no sun up in the sky
Stormy weather
Since my man and I ain't together
It's raining all the time
When he went away
The blues came in and met me
If he stays away
That old rocking chair's gonna get me
All I do is pray
My lord will let me
Walk in the sun once more
I can't go on
Everything I have in life is gone
Stormy weather
Just can't get my gal and I ain't together
It's raining all the time
Keeps raining all the time
Diana Ross Lyrics
Diana Ross An Evening With Diana Ross Lyrics
More Diana Ross Music Lyrics:
Diana Ross - Corner Of The Sky Lyrics
Diana Ross - Didn't You Know (You'd Have To Cry Sometime) Lyrics
Diana Ross - I Never Loved A Man Before Lyrics
Diana Ross - I Won't Last A Day Without You Lyrics
Diana Ross - I Wouldn't Change The Man He Is Lyrics
Diana Ross - In Your Arms Lyrics
Diana Ross - Until We Meet Again Lyrics
Diana Ross - You Are Everything Lyrics


text:
Information Links
BBH deputy ECD Caroline Pay exits
Bartle Bogle Hegarty has parted company with its deputy executive creative director Caroline Pay and has promoted Ian Heartfield, creative...
Marketers' Toolkit: brand-building lessons from Airbnb, Coca-Cola, Carling, Barclaycard and more
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It's great that we're battling the stereotypes in ads, but we won't win the war until brands apply the same...
Group M appoints Montgomery to lead global brand safety drive
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The woeful tales of BHS and Sports Direct expose retail's ruthless side
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Ogilvy & Mather Vietnam returns two Lions of own accord
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IAB Digital Upfronts returns for third year
Some of the world's biggest media owners will feature at the Internet Advertising Bureau UK's Digital Upfronts, which returns for...
Apple, Microsoft, Samsung top FutureBrand ranking
Tech giants continue to top brand rankings across the board, with most performing better than classic brands Coke, Nike and...
Openreach must be 'distinct' company within BT, says watchdog
BT has avoided a full break-up with Openreach, its wholesale network, after an Ofcom review into the UK's broadband.
There's no such thing as a strong brand story without a strong team
Lionel Benbassat, head of marketing and brand at Eurostar, searches for diversity of experience and personalities to build his dream...
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1 Liverpool FC to stream next match in 360-degree video
Liverpool Football Club will screen a live football match tonight with a 360-degree view on YouTube, as top Premier League teams continue to build their online brands for a global audience.
1 Agencies' anger at failure of Stronger In campaign
"We failed the country, we could and should have done better." So says one senior advertising executive involved in the Britain Stronger In Europe campaign.
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Microsoft's SkyDrive cloud service renovated with new app and more storage
Microsoft has enhanced its SkyDrive cloud storage service in an attempt to drive off competition from the likes of Dropbox.
Customers can now get even more storage so long as they're prepared to pay for it, though 7GB free storage will be available for first-time users.
For US$10 a year, SkyDrive is offering +20GB of storage, while US$25 a year will give you +50GB. For heavy users there's a third option that brings a whopping +100GB for US$50 a year.
SkyDrive had previously offered 25GB of free storage but despite the hike in price Microsoft has promised to honour that agreement to any existing users who have already uploaded files - though you will need actively to opt in for the upgrade.
SkyDrive has also released a new app enabling users to store and retrieve files and folders remotely to any PC, through Windows Explorer (on Windows 8, Windows 7 and Windows Vista) or Mac, through Finder, via SkyDrive.com
The app is even available on Windows and iOS mobile devices, though not on Android.
Perhaps the omission of Android lies with the fact that Google is expected to announce its own cloud storage service, Google Drive, any day now.
Have you used Microsoft's SkyDrive? Let us know your thoughts.
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- Pokemon Go: How to play and other tips and tricks
- Pokemon Go top tips: Master the Pokemon mayhem


text:
Sep 7
Aug 30
Aug 19
Rap Contest
Sounds Like: Eric B. & Rakim, Kanyewest, Jay-Z
Label: unsigned
Bio: Dubbs is a Riverside California native. His father was a singer in a band & one of his favorite uncle's is a bass player and DJ. Dubbs has been writing songs since 12 years old and started to produce his own music about 5 years ago. The new CD, "Helicopter II" is a hip-hop project that blends man...See Full Bio


text:
Hammam took suitcase full of bribe $$ to Trinidad
(Trinidad Express) Wealthy Qatari Mohamed bin Hammam and his nine-member delegation quite literally walked straight through Immigration and Customs to the VIP lounge of Piarco International Airport before being whisked away in an executive ride to the Hyatt Regency (Trinidad) Hotel on the morning of May 9, 2011 with a suitcase full of bribe money.
A documents trail and eyewitness accounts reveal the former Qatar Football Association president was issued a visa exemption by then Minister in the Ministry of National Security Subhas Panday days after a request was made by bin Hammam's buddy and the man who made the suggestion to bring cash to the Hyatt meeting, Jack Warner.
Documents obtained by the Sunday Express show Warner, the then Minister of Works and Transport and the man who arranged the infamous Caribbean Football Union (CFU) conference to facilitate bin Hammam's 2011 presidential campaign to FIFA voting members, made the request for a visa waiver for bin Hammam and nine others on April 29, 2011, days before the Qatari's planned arrival on a private jet at Piarco International Airport.
Visa Exemptions for AFC Delegation
On May 5, 2011, four days before bin Hammam's arrival in Trinidad, former deputy permanent secretary in the Ministry of National Security Sandra Lynch wrote to Warner in his capacity as president of the CFU, to advice that visa exemptions had been granted for the visiting ten-member Asian Football Confederation (AFC) delegation.
Lynch signed the approval letter giving bin Hammam and his party a free pass through Immigration and Customs for the substantive permanent secretary at that time Jennifer Boucaud-Blake, who has since retired and did not immediately return messages left on her voicemail.
The letter to Warner stated in part: "I am to refer to your letter dated April 29, 2011 and wish to advise that the Honourable Minister in the Ministry of National Security acting in accordance with the provisions of Regulation 13 (13) of the Immigration Regulation has exempted the persons listed in the attached from the requirements of a visa, over the period May 9 to 11, 2011, to participate in a special meeting of the AFC. Kindly ensure that this approval is presented to the Immigration Authorities upon arrival at the Port of Entry."
Immigration Bypassed
Guy Benjamin, the then Chief Immigration Officer, has no recollection of the May 5, 2011 ministerial order. He said no such directive came to his attention. Benjamin told the Sunday Express such instructions are usually issued to the Chief Immigration Officer because the CIO has to facilitate the visa exemption order for the identified foreign nationals.
In the case of bin Hammam and his AFC football associates, no instruction of any kind was issued to the office of the CIO. The directive was issued instead to Jack Warner, the former government minister and ex-vice-president of FIFA, the world governing body for football. Oddly enough, a May 4, 2011 Warner request for visa exemptions for a three-member Haitian delegation, headed by Yves Jean Bart, the Haitian Football Federation, and granted the following day, May 5 for the same May 10-11 conference, was copied to the CIO.
Lynch, who approved a controversial fire truck payout several times the value of the crashed tender during Warner's tenure as Minister of National Security, also signed off on the visa exemption order for the Haitians which also went to CFU president Warner. The former deputy PS could not be reached for comment.
Panday: My Hands are Clean
Panday, however, said he "may have signed" the request for the visa waiver without knowledge of the subsequent bribery allegations. Panday said yesterday he had no recollection of the specific Warner request for visa exemptions and made clear he had no conversation with Warner on the matter.
"I don't recall this one at all," he told the Sunday Express, adding that if he did sign off on the visa waiver request, "then there must be a record of it in the Ministry of National Security".
The former minister, who said his "hands are clean" added that no queries came to him following the subsequent cash-for-votes bribery allegations. He said by the time the police commenced investigations he was already out of the ministry.
Reginald Dumas, a career diplomat and former head of the Public Service questioned why the visa exemption letter was issued to Warner, then a Cabinet Minister wearing his CFU hat, and not to the COI as required by law to facilitate any Section 13 (13) government request. There are questions too about whether the visa exemption requests went to the Cabinet and why the authorisation letter for the bin Hammam party was not copied to immigration.
Eyewitness Reports place
Warner with the Money
Warner did not immediately respond to requests for a comment but eyewitness accounts reveal that bin Hammam's party was met as soon as they came off the tarmac on the morning of May 9 by Joan Brammer, head of Airport VIP Protocol, and taken straight to the VIP Lounge with hand luggage in tow.
They were shuttled in executive rides to the Hyatt Hotel immediately after their luggage was collected from the baggage claims area. There was no security screening of the bin Hammam delegation's hand luggage, according to sources with knowledge of the situation. Brammer refused comment when contacted by the Sunday Express.
Bin Hammam attended a private Warner-hosted dinner at Joseph's Restaurant in Maraval later that evening and met again with his former FIFA ExCo (Executive Committee) friend and colleague early the next morning (May 10) at the US$1,799 a night presidential suite at the Hyatt. Eyewitness reports place an empty-handed Warner entering the lobby of the hotel and later a suitcase-carrying Warner on his way out of the hotel.
Suitcase of Cash in Warner's Office
Testimony given to the FIFA Ethics Committee investigator and former FBI director Louis Freeh by former CFU general secretary Angenie Kanhai place the bribe money in a locked piece of hand luggage with the key in the front pocket in Warner's Works and Transport Minister's office at the corner of Richmond and London Streets.
Kanhai, in a May 2011 statement to the FIFA Ethics Committee said: "On May 10, 2011, Mr Warner advised me that he had gifts, which were to be distributed to the delegates. Mr Warner did not tell me what the gifts were, but advised that they were to be distributed from the hotel that afternoon. After consulting with my staff, Jason Sylvester and Debbie Minguell, I suggested to Mr Warner that the gifts be distributed between 3 p.m. and 5 p.m. that day."
The two-page statement, signed by Kanhai said: "During the morning session on May 10, Mr Warner made an announcement to the attendees about picking up the above mentioned gift." She said she was instructed to go to Warner's official government office to collect a locked bag and subsequently discovered that the bag contained envelopes stuffed with cash.
More Bribery Allegations
Warner quit the world governing football body following accusations of bribery in June 2011. He and bin Hammam were accused of giving Caribbean officials US$40,000 in cash to win support for bin Hammam's presidential challenge against Sepp Blatter.
More recently, the Sunday Times reported evidence of more alleged bribe payments from bin Hammam to football officials, including Warner, in exchange for support of Qatar's bid to host the 2022 World Cup. The British newspaper asserted that substantial payments were funneled directly to Warner controlled bank accounts.
Warner, identified as a key benefactor to bin Hammam's largesse had denied the newspaper claims and countered that the money he received from bin Hammam was to help with losses he suffered during an earthquake in China.
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Shareholders plan sees Clico retaining six companies
(Trinidad Guardian) The United Shareholders Limited's plan to deal with Clico's residual debts to Government envisages that CL Financial retain control of six companies—including Angostura Holdings Limited, Colfire Ltd and Home Construction Ltd—and that there be a joint approach among shareholders and Government to steer Clico's future.
T&T Cabinet agrees to pay cane farmers final TT$58m payment
(Trinidad Guardian) Cabinet has decided to pay cane farmers the final settlement of TT$57,965,675 of the compensation package promised back in 2007.
T&T petrol dealers facing crisis – association head
(Trinidad Guardian) President of the Petroleum Dealers' Association of T&T, Robindranath Naraynsingh, on Thursday said the country's 170 gas stations were on the verge of collapse due to poor profitability margins from the sale of fuel.
U.S., Cuba hold 'substantive' second round talks on claims
WASHINGTON/HAVANA July 29 (Reuters) – The United States and Cuba have concluded a "substantive" second round of talks on multibillion-dollar claims against one another in Washington and agreed to hold more regular meetings on the matter, a State Department Official said yesterday.
T&T Equal Opportunity tribunal rules: Employee of African descent discriminated against in favour of East Indian
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T&T petrol dealers facing crisis – association head
(Trinidad Guardian) President of the Petroleum Dealers' Association of T&T, Robindranath Naraynsingh, yesterday said the country's 170 gas stations were on the verge of collapse due to poor profitability margins from the sale of fuel.