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US 3980594 A Abstract Quaternary ammonium salts or inorganic and organic oxygen acids having pK values (where pK is the negative log of the dissociation constant) for at least one of the dissociable hydrogen atoms equal to or greater than 2.0 in aqueous solution are employed as extremely efficient catalysts for trimerization of organic isocyanates, particularly aromatic isocyanates, to isocyanurates and for urethane formation.
Claims(8) 1. A method which comprises reacting organic isocyanates in contact with at least 0.01 part by weight of said isocyanates of a compound displaying catalytic activity for exothermic cyclic trimerization of organic isocyanates and for urethane formation, said compound corresponding to the structural formula (NR4)y A in which
A is an anion derived from an acid having a pK value, in aqueous solution at substantially room temperature, of 2.0 or greater and being free of substituents which can react with isocyanates under conditions of trimerization and being selected from the group consisting of inorganic oxygen acids, carboxylic acids and carbonic acid, each R is any organic group other than A and free of any substituents and functional groups which can react with isocyanates under conditions of trimerization, no more than one R per N containing an aromatic ring attached directly to N, and y is a whole number equal in value to the valence of A. 2. A method in accordance with claim 1 wherein each R is a hydrocarbon group containing no more than about 18 carbon atoms, the total number of the carbon atoms of the four R groups on any N being no more than about 25.
3. A method in accordance with claim 2 wherein each R is a hydrocarbon group containing no more than about 8 carbon atoms, the total number of the carbon atoms of the four R groups on any N being no more than about 12.
4. A method in accordance with claim 2 wherein the acid from which A is derived has a pK value in aqueous solution at essentially room temperature of from about 4 to about 10.
5. A method in accordance with claim 1 wherein said organic isocyanates are polyisocyanates and said reaction takes place in contact with from 20 to 60 parts by weight per 100 parts by weight of said isocyanates of hydroxylated ingredients selected from the group consisting of aliphatic polyethers, aliphatic polyesters and polyepoxides, said hydroxylated ingredients having a number average molecular weight from about 250 to 12,000.
6. A method in accordance with claim 1 wherein said reaction takes place in contact with alcohols and/or polyols containing secondary and/or tertiary alcohol groups, the ratio of the total secondary and tertiary hydroxyl groups introduced into the system to the total isocyanate groups introduced into the system being from about 0.01 to 0.25 -OH group per -NCO group where the compound is a monoalcohol and from about 0.01 to 0.50 -OH group per -NCO group where the compound is a polyol having 2 or more -OH groups.
7. A method in accordance with claim 5 wherein said reaction takes place in contact with from 0.5 to 5 parts by weight of water per 100 parts of organic isocyanates.
8. A method in accordance with claim 5 wherein said reaction takes place in contact with from 2 to 4 parts by weight of a carbodiimide-forming catalyst per 100 parts by weight of organic isocyanates, the amounts of said carbodiimide-forming catalyst and said trimerization catalyst being such that the weight of said carbodiimide-forming catalyst is from 1 to 3 times the weight of said trimerization catalyst.
Description Isocyanurates are prepared by cyclic trimerization of isocyanates. These products have excellent thermal stability and superior flame resistance and are, therefore, desirable structural units for thermally resistant plastic materials. One of the advantages of the isocyanurates is that they retain their strengths to temperatures of 160�C. or more and are resistant to most organic solvents, acids, alkali, ultraviolet light and humidity. The isocyanurates can be employed as solvent-free systems, and the curing conditions can be varied over a wide range of times and temperature from rapid cure at room temperature to curing at elevated temperatures up to about 160�C. while maintaining satisfactory pot life. The isocyanurates can be modified with other polymers such as polyether polyols, epoxy resins, acrylic resins and alkyd resins or they can be extended with fillers, pigments and the like. Heretofore, a variety of catalysts has been used to promote trimerization, including quaternary hydroxides of nitrogen, phosphorus, arsenic and antimony (British Patent No. 837,120); tertiary amines, alkali or alkaline earth metal salts of 1-3 carbon carboxylic acids, alkali metal alkoxides and organic tertiary phosphines (U.S. Pat. No. 3,211,703); special tertiary amines such as N,N',N"-tris(dimethylaminopropyl) hexahydrotriazine (U.S. Pat. No. 2,993,870), and 2,4,6-tris(dimethylaminomethyl) phenol (U.S. Pat. No. 3,222,303); certain epoxide-tertiary amine mixtures (U.S. Pat. No. 2,979,485); and heavy metal compounds, such as iron acetylacetonate, which are soluble in organic solvents (U.S. Pat. No. 3,135,111). SOME OF THESE CATALYSTS ARE RELATIVELY INACTIVE AT ROOM TEMPERATURE, AND HEAT AND/OR EXCESSIVELY HIGH LEVELS OF CATALYST ARE REQUIRED. Others are such strong bases that their presence in the final product has a detrimental effect upon the aging properties of said product, especially in the presence of chemical groups that are sensitive to nucleophilic attack. Therefore, there is still a need for new catalysts for cyclic trimerization of isocyanates which do not have these inherent disadvantages. This invention comprises the use of quaternary ammonium salts of weak acids having pK values of at least 2.0 in aqueous solution at room temperature as catalysts for the formation of isocyanurates from aromatic isocyanates, preferably unhindered isocyanates, as well as for the urethane reaction, and the unique products produced thereby. More specifically, this invention comprises principally the use of compounds of the formula (NR4)y A as isocyanurate-forming and urethane-forming catalysts wherein each R can be any organic group other than A free of any substituents (including functional groups) which react with isocyanates under conditions of trimerization, no more than one R per N containing an aromatic ring attached directly to N; A can be any anion derived from an acid, primarily an inorganic oxygen acid or a carboxylic acid free of active hydrogen atoms or other substituents which can react with isocyanates under conditions of trimerization, said acid having a pK value in aqueous solution at essentially room temperature of at least 2, preferably at least about 4 and no greater than about 10, and y is a whole number (at least 1) equal in value to the valence of A. Examples of suitable acids from which A can be derived appear in the lists on pages D-77 and D-78 of the The Handbook of Chemistry and Physics. 45th Edition (1964-1965), The Chemical Rubber Co., Cleveland, Ohio. Each R is preferably a hydrocarbon group such as, for example, an alkyl, cycloalkyl, alkenyl, cycloalkenyl, aryl, aralkyl or alkaryl group, preferably containing no more than about 18 carbon atoms, more preferably no more than about 8 carbon atoms. However, possible additional substituents in the R groups include halogen atoms, ether oxygen atoms, ester groups, tertiary amine groups, amide groups, urethane groups, urea groups and the like. The R groups on any N can be the same or different, and the total number of carbon atoms in the R groups on any N atom is preferably no greater than about 25, more preferably no greater than about 12. The above-defined compounds can be used as catalysts in the formation of urethanes and/or the formation of isocyanurates in amounts of from 0.01 to 2 percent or more by weight based on the weight of the isocyanates employed. Because the efficiency of a catalyst is directly influenced by its compatability in a particular reaction system, the (NR4)y A compounds should be chosen as to give optimum compatibility in the particular reaction system. The catalysts employed in this invention provide optimum process control at low catalyst concentrations and do not impair aging characteristics while making possible strongly exothermic, fast reactions at ambient temperatures. These accomplishments are two of the principal general objects of this invention. The characteristics of the subject catalysts are such that the isocyanurate-forming and urethaneforming or urea-forming reactions can be readily modified to yield a wide variety of products. For example, trimerization of diphenyl-methane-4,4'-diisocyanate, generally identified as MDI and MDI-based polymeric isocyanates in the presence of small amounts of water and/or an auxiliary blowing agent give rigid cellular products. Brittle resins in cellular or noncellular form, such as those obtained by trimerization of polymeric MDI, can be made less brittle without significantly decreasing temperature stability by incorporating into a formulation from 20 to 60 parts by weight of aliphatic polyethers, aliphatic polyesters or polyepoxides (number average molecular weight of 250 to 12,000, preferably 500 to 6000) per 100 parts of isocyanate. The catalyst compounds described herein are also excellent urethane-forming catalysts and in this respect are at least comparable to stannous octoate. If any of the R or A groups carriers a function such as a tertiary amine, new catalysts for flexible urethane foams are produced. The efficiency of the subject catalysts can be altered by the addition, for example, of aromatic primary polyamines such as phenylene diamine or diamino toluene. These additives delay the activity of the catalyst giving a corresponding increase in "cream time" for rigid isocyanurate foams. It has also been found that alcohols and polyols containing principally secondary and tertiary hydroxyl groups inhibit trimerization apparently until the hydroxyl groups have been substantially eliminated by the formation of urethanes even though the isocyanate-hydroxyl reaction normally proceeds at a considerably slower rate than trimerization. This apparent catalytic selectivity makes it possible to increase the pot life or cream time of the isocyanate reaction mixture without affecting the cure time, total set-up time being extended only by the increase in cream and rise times. The total concentration of secondary and/or tertiary alcohol groups should be in the range of from about 0.01 to 0.25 OH group per NCO group if the OH containing compound is a monoalcohol or from about 0.01 to 0.50 OH group per isocyanate group if the OH compound has 2 or more hydroxyl groups. Thus, any secondary and tertiary hydroxyl groups in the other components in the total system must be taken into account, such as any secondary (or tertiary) hydroxyl group in the aliphatic polyethers, polyesters or epoxides previously referred to. The preferred sources of secondary and tertiary hydroxyl groups are secondary alcohols of 3 to 10, preferably 3 to 5, carbon atoms, tertiary alcohols of 4 to 5 carbon atoms and polymeric polyols, preferably polyether polyols, of the types described herein and having molecular weights no higher than about 12,000, preferably no higher than about 6000. Simple alcohols are preferred because they are easier to handle and because they do not produce network links. Suitable alcohols include isopropanol, sec-butanol, tert-butanol, 2-methyl-2-butanol, 2-pentanol, 3-pentanol, 2,3-dimethyl-3-pentanol, 3-ethyl-3-pentanol, 2-hexanol, 3-hexanol, 2-methyl-2-hexanol, 5-methyl-2-hexanol, 3-methyl-3-hexanol, 2-heptanol, 3-heptanol, 4-heptanol, 2-octanol, 2-methyl-2-octanol and tricyclo[5.2.1.02,6 ]-dec-3-en-8(9)-ol and mixtures thereof. The quaternary ammonium salts of this invention are generally prepared by standard techniques well known in the art. One method involves alkylation of tertiary amines, conversion to the hydroxide or alkoxide and reaction of the hydroxide or alkoxide with a selected acid to form the desired salt, usually in alcohol solution. Examples of typical compounds include tetramethyl ammonium octoate; tetramethyl ammonium 2-ethyl hexoate; tetramethyl ammonium carbonate; tetramethyl ammonium chloroacetate, and bis (trimethyl benzyl ammonium) maleate. Of special interest are quaternary ammonium carbonates such as tetramethyl ammonium carbonate. This highly active trimerization catalyst additionally reacts with acids inherent in the separate ingredients, such as in the polyisocyanate, and with other acids having pK values less than 6 purposely added to the formulation to produce a source of carbon dioxide for additional blowing in a foam while neutralizing the system. When the acids are weak acids, i.e., acids having ionization pK's or 2 or more, the resulting salt formed therefrom is at least equally effective as a catalyst as is the carbonate. Thus, addition of small amounts of weak acids to formulations employing a quaternary carbonate as the catalyst does not significantly affect the reactivity of the system while giving foams of lower density. The isocyanates and polyisocyanates suitable for use with these novel compounds to form isocyanurate products are preferably unhindered aromatic isocyanates having more than one active isocyanate group per molecule. Examples of these include 1,5-naphthalenediisocyanate, 4,4'-diisocyanatodiphenylether, benzidinediisocyanate, 9,10-anthracenediisocyanate, 4,4'-diisocyanatodibenzyl, 4,4'-diisocyanatostilbene, and 1,8-naphthalenediisocyanate. It is to be understood that mixtures of two or more of these polyisocyanates may be employed. preferred among the polyisocyanates is 4,4'-diisocyanatodiphenylmethane, popularly known as "MDI," and the polyisocyanates obtained by phosgenation of crude condensation products of aniline with formaldehyde. The catalyst of this invention may be mixed with the aforedescribed polyisocyanates at levels of from 0.01 to 2 parts by weight per 100 parts by weight of the isocyanates. Where these catalysts are chosen to be miscible or soluble in the isocyanate, the polymerization reaction proceeds significantly faster than if the catalyst is not homogeneous with the isocyanate. The homogeneity of the catalyst and the isocyanate is controlled greatly by the R substituents on the nitrogen N as well as the structure of the anion. Additives may be employed to produce products with different properties using the same catalysts of this invention. For instance, polyisocyanates alone or in admixture with polyether polyols, polyester polyols or epoxy resins and/or with small amounts of water can be reacted in the presence of the catalysts of this invention to produce a wide variety of products. Employing polyols reduces brittleness of trimerized polyisocyanates. Adding small amounts of water causes formation of foams. Of the polyols suitable for use herein, polyether diols, triols, and tetrols are preferred. Preferred polyethers are the polyalkylene ether polyols prepared by adding propylene oxide to various diol, triol, tetrol and other polyol starters to produce adducts of various molecular weights. Polyethers which deserve special mention are the 1,2,6-hexanetriol and glycerol adducts of propylene oxide having molecular weights of from about 250 to 6000. Generally, the polyethers preferred for employment in this invention can be conveniently characterized as liquid polyethers having viscosities in the range of from 50 centipoises to about 50,000 centipoises at room temperature (i.e., 25�C.) and having molecular weights in the range of from 1000 to about 6000. When water is used to form a cellular product, the water should be used in levels of 0.5 to 5 parts by weight per 100 parts by weight of polyisocyanate. Other gas-producing materials can be utilized either alone or in conjunction with water such as volatile halogenated (preferably fluorinated) hydrocarbons. Where no water or other pneumatogen is employed and the isocyanate is modified by addition of a polyether polyol such as a polyether triol, the catalysts of this invention produce isocyanurate coatings and adhesives that display exceptional bond strength to such diverse adherends as fiber-reinforced polyester sheets, metal surfaces and rubber surfaces. These adhesives retain their strength to temperatures of 160� C. or more. In addition, they can be applied as solvent-less systems, and the cure rate of the isocyanurate can be adjusted over a wide range of temperatures and times from rapid set-up at room temperature to slow cure at elevated temperatures. They can also be readily applied as a two-component system with spray guns such as for use in spraying rigid urethane foam insulation. These coatings and adhesives are preferably prepared from the aforementioned polyisocyanates, the catalysts of this invention and polyether polyols. Generally, such polyols are employed in amounts ranging from 20 to 60, preferably around 40, parts by weight per 100 parts by weight of the polyisocyanate, and the catalyst is employed at levels ranging from 0.25 to 1.25 parts by weight on the same basis. Modifications can be attained by the inclusion of fillers, pigments and other extender materials. When the catalysts of this invention are combined with aromatic primary polyamines such as diamino-benzene and diaminotoluene in isocyanurate foam systems, two significant effects are produced. The first is a marked increase in time for the start of fast exotherm at a given catalyst concentration as compared to a similar formulation not containing the polyamine. See, e.g., Example VI below. This delay in time may vary from one to twelve times the normal time for start of the exotherm. For example, where a time of 1.4 minutes is experienced when 1.5 parts of tetramethyl ammonium octoate are blended with 100 parts of polymeric isocyanate, the addition of an equal molar amount of toluene diamine increases the lapse time to about 11.8 minutes. For production control it is very desirable to be able to control this time to compatibilize the formulation with various equipment and process requirements. The second effect observed when aromatic polyamines are added to the formulation is a very marked increase in initial viscosity of the formulation. The increase in viscosity at the onset of foaming produces a greatly improved and more highly stabilized cellular structure and results in improved reverse impact strengths in the final product without loss of other properties such as surface hardness of molded integral skin rigid foam parts. A further embodiment is the use of the catalysts of this invention for trimerization of polyisocyanates in combination with a catalyst for the promotion of carbodiimide formation. The product resulting from the reactions is a rigid foam having excellent dimensional stability at elevated temperatures and low friability. By controlling the relative amounts of the two catalysts, the physical density and chemical crosslink density of the foam can be altered. Any of the known catalysts for carbodiimide formation can be used in this embodiment such as, for example, the phosphorus catalysts described in U.S. Pat. Nos. 2,853,473 and 2,853,518. A catalyst that has been found to be exceptionally compatible with the trimerization catalysts of this invention is 1-phenyl-3-methyl-3-phospholene-1-oxide. Typical levels of carbodiimide-forming catalyst used in this embodiment are 2 to 4 parts by weight per 100 parts by weight of isocyanate and 1 to 3 times the weight of the trimerization catalysts of this invention. The quaternary ammonium salts of weak acids of this invention are extremely effective catalysts for urethane formation comparable to, and in some cases, surpassing the efficiency of stannous octoate. When employing the catalysts of this invention in the preparation of flexible foams, products with improved resilience are obtained. By these means a wide range of catalysts with varying balances between activity in catalyzing the hydroxyl and water reactions should be possible. For example, in particular, a bridgehead nitrogen should increase its effectiveness in catalyzing the reactions which take place in preparing flexible polyether water-blown foams or other urethane foams. As a further embodiment, these catalyts are also of value in producing highly resilient cold-molding polyurethane foams, i.e., foams that are cured at room temperature. These foams are generally formed from a conventional urethane reaction between the aforedescribed polyisocyanates and predominantly primary hydroxyl terminated polyether polyols having molecular weights of from about 1000 to 6000. A particular advantage of isocyanurate foam formulations using the catalysts of this invention to the substantial exclusion of the tertiary amines and tin catalysts normally used in the preparation of rigid polyurethane foams is that such isocyanurate formulations, being nearly neutral and free of metal cations, can be formed in silicone rubber molds without attacking the silicone rubber as occurs with tertiary amine and/or tin catalysts. Since the silicone rubber molds are very expensive because of the high cost of silicone rubber and the large amount of hand labor required in their manufacture, a marked increase in mold life represents a considerable savings in the cost of producing articles such as furniture from such rigid foams. An additional advantage of quaternary salt catalyzed isocyanurate rigid foam over conventional urethane foam is that demolding time of the isocyanurate foam can be a third or less of that required for urethane foams. The shorter contact of foam and mold not only reduces processing time with consequent savings but again increases mold life. A further advantage of the isocyanurate foam system is the very low viscosity of the components, which should give better detail in the moldings. Better dimensional stability at higher temperatures, excellent flame resistance and excellent hydrolytic and environmental aging resistance are also possible with our systems. The following examples further illustrate the subject invention and are not intended to limit the invention, the scope of which is properly delineated in the claims. All quantitative measurements are by weight unless otherwise stated. To 100 ml. of a 0.675 molar solution of phenyl isocyanate in dioxane (equivalent to 8.04 grams of phenyl isocyanate) there was added 0.00312 gr.-mole (0.07 gram) of tetramethylammonium-2-ethyl hexoate. The solution was permitted to react at 20�C., and the rate of disappearance of free isocyanate was determined by titration of 10 ml. samples of the solution with dibutyl-amine-hydrochloric acid. After 88 minutes, 94% of the isocyanate had reacted. The reaction was repeated using bis-tetramethylammonium carbonate in equal molar substitution for the tetramethylammonium-2-ethyl hexoate. After 70 minutes, 88.5% of the isocyanate had reacted. For comparison the reaction was again repeated using N,N',N"-tris(dimethylaminopropyl)sym-hexahydrotiazine (a conventional trimerization catalyst) in equal molar substitution for the bis-tetramethylammonium carbonate. After 240 minutes at 21�C., 92% of the isocyanate had reacted. The reaction product in each case was isolated, and each product had a melting point of 275�-280�C. Some of each product was dissolved in chloroform for reviewing infrared spectra. Each showed a strong absorption peak at 5.82μ which is characteristic of the isocyanurate carbonyl. Absorption peaks of free isocyanate (4.4μ) and of dimer carbonyl (5.63μ) were either missing or barely detectable in the samples. To separate portions of 11.9 grams (0.1 gm.-mole) of phenyl isocyanate dissolved in sufficient chlorobenzene to provide a total of 25 ml. of solution at room temperature was added 0.0002 mol of each of the following catalysts (dissolved in ethanol to simplify handling) of this invention: bis-tetramethylammonium maleate tetramethylammonium chloroacetate tetramethylammonium dibutylphosphate After 24 hours at room temperature some of each reaction product was dissolved in chloroform for reviewing the respective infrared spectra. All samples showed strong absorption at 5.82μ whereas absorption at 4.4μ and 5.63μ was either absent or barely detectable. Similar reaction mixtures were made using compounds that do not agree with the formula (NR4)y A as defined hereinbefore in lieu of the compounds of this invention. These compounds, viz., tetramethyl ammonium-p-toluene-sulfonate, polyoxyethylene-oleyl-methyl ammonium chloride, tetramethylammonium-N,N-di-methyl-dithiocarbamate, and potassium-2-ethylhexoate, did not cause trimerization of the phenylisocyanate even after 24 hours. A rigid polyisocyanurate foam was prepared by adding one gram of 33.3% solution of tetramethylammonium octoate in methanol (diluted with 5 grams of diglyme) to a vigorously stirred mixture of 0.15 gram of a silicone surfactant and 50 grams of diphenylmethane-4,4'-diisocyanate (MDI). A rapid reaction took place at room temperature with the development of a dense rigid foam. The foam was powdered and the residual free isocyanate thereof determined; a value of 0.202 milliequivalent of NCO per gram was found which corresponded to 98% conversion of the isocyanate to trimer. The experiment was repeated using polymeric MDI in lieu of MDI and a vlue of 0.70 milliequivalent of NCO per gram was found which corresponded to 92% conversion of the isocyanate. Isocyanate determination on the same foam sample after 2 hours post cure at 175�C. gave 0.1 milliequivalent of NCO per gram corresponding to about 99% conversion of all isocyanate present to trimer. Samples of rigid isocyanurate foams were prepared from the formulations shown below by intimately mixing the ingredients in the parts shown and pouring them into a tray at room temperature. Visual observation of the cream time, rise time and tack-free time were made and are also listed as well as is the density of each sample. ______________________________________ SAMPLESINGREDIENTS A B C D______________________________________diphenylmethane 4,4'-diisocyanate 50 50 50 50ethylene oxide capped, polyoxy- 20 20 20 20propylene triol 4500 MWsilicone surfactant 0.5 0.5 0.5 0.5tetramethyl ammonium carbonate 0.17 0.17 0.17 0.17(added as 33% solution inmethanol)2-ethyl-hexanoic acid -- 0.52 -- --glacial acetic acid -- -- 0.52 0.12PROPERTIEScream time (seconds) 24 18 30 27rise time (seconds) 42 48 49 60tack-free time (seconds) 49 60 180 90density (kg./cu. m.) 530 270 160 400______________________________________ Addition of the acid to the formulation tends to reduce the foam density by providing additional blowing from the carbon dioxide generated in the salt-forming reaction. Two polyisocyanurate adhesive formulations as shown below were prepared using the recited compounds in the parts shown. The triol and the epoxy resin were added to improve ductility. ______________________________________ SAMPLESINGREDIENTS E F______________________________________diphenyl methane 4,4'-diisocyanate, 50 50(PAPI 143L)tetramethyl ammonium 2-ethylhexoate, 3.0 3.08.5% in polypropylene ether glycol(2000 MW)ethylene oxide capped polyoxypropylene- 18 --ether triol (4500 MW) (Dow CP 4701)diglycidyl ether of polypropylene ether -- 20glycol (epoxy equivalent wt. 175 to 205)(Dow DER 733)______________________________________ These adhesives were used to adhere 2.54 cm. � 5.08 cm. � .16 cm. test pieces of shot blasted steel and cleaned fiberglass-reinforced cured polyester strip to each other and together; the assemblies were cured at 150�C. for 5 minutes. The adhesive strengths of the resulting assemblies (in pounds per square inch) were as follows: ______________________________________ FORMULATIONSASSEMBLIES E F______________________________________FRP* to FRP 160 168FRP to Steel 125 105Steel to Steel not tested 265______________________________________ *glass fiber reinforced thermoset polyester styrene resin Five samples of 11.9 grams of phenylisocyanates, each diluted in 13.6 grams of chlorobenzene, were treated with different amounts of tetramethyl ammonium-2-ethyl hexoate (TMAO) and orthotoluene diamine (TDA) as shown below. The times to onset of exotherm and the rates of temperature increase during exotherm were observed in each case and are recorded below. ______________________________________ RATE OF MOLE TIME OF EXOTHER- WT. WT. RATIO ONSET OF MIC TEMP.SAM- TMAO TDA TDA/ EXOTHERM INCREASEPLE (gms) (gms) TMAO (min.) (�C./min.)______________________________________G .045 -- 0:1 1.4 6.3H .045 .025 1:1 8.8 5.6J .045 .025* 1:1 11.8 5.3K .045 .122 5:1 8.0 4.4L .090 .122 5:2 3.4 15.4______________________________________ *meta toluene diamine Comparing samples G and L it can readily be seen that addition of the aromatic primary polyamine to the novel compounds of this invention inhibits the onset of exotherm or, in other words, retards the beginning of the trimerization reaction without significant effect upon the trimerization reaction (rate of exothermic temperature increase) once it begins. Samples of polyisocyanurate, polycarbodiimide, and polyisocyanurate-polycarbodiimide foams were prepared using catalysts of this invention alone and in combination with carbodiimide catalysts as shown below. The ingredients in the parts shown were intimately blended in a beaker and poured into a cardboard dairy container to react and rise into a foam at room temperature. Each foam sample was oven cured at 160�C. for 10 minutes. ______________________________________ SAMPLESINGREDIENTS M N P Q______________________________________diphenylmethane-4,4'- 25 25 25 25diisocyanateethylene oxide capped 10 10 10 10polyoxypropylene triol(MW 4500)silicone surfactant 0.5 0.5 0.5 0.5tetramethyl ammonium -- -- 0.25 0.25octoate 33% in methanol(trimerization catalyst)1-phenyl-3-methyl-3-phos- 0.5 1.0 1.0 --pholine-1-oxide (carbodi-imide catalyst)PROPERTIESdensity (kg./cu. m.) 96 32 96 580type flex- flex- rigid rigid ible iblefriability low low low highdimensional stability good good excel- excel-after 6 hrs. at 190�C. lent lent______________________________________ To a stirred mixture of 7.4 grams (0.1 mol) of secondary butanol, 5.7 grams of monochlorobenzene and 0.1 ml. of a catalyst solution of 4.4 grams of tetramethylammonium-2-ethylhexoate in 10 ml. of methanol were added 11.9 grams (0.1 mol) of phenyl isocyanate, and the resulting mixture was allowed to react 30 minutes at room temperature (about 20�C). An infrared spectrum taken on a 3 weight percent solution of the resulting reaction mixture in chloroform showed it to be free of both isocyanate groups and isocyanurate linkages. The spectrum was in agreement with the spectrum for N-phenyl-sec-butyl-urethane. This test was repeated using half as much sec-butanol and 2.3 grams more chlorobenzene. The infrared spectrum of the resulting reaction mixture indicated about equal parts of N-phenyl-sec-butyl-urethane and triphenylisocyanurate. To a stirred solution of 11.9 grams (0.1 mol) in 13.1 grams of chlorobenzene was added 0.1 ml. of a catalyst solution of 4.4 grams of tetramethyl-ammonium-2-ethylhexoate in 10 ml. of ethanol, and the resulting reaction was allowed to proceed with stirring until the maximum exotherm was reached as determined by the use of an iron-constantan thermocouple and commercial electronic recorder. This test was repeated three times substituting for 3.7 grams of the chlorobenzene 3.7 grams (0.05 mol) of n-butanol, sec-butanol and tert-butanol. The respective maximum temperatures and times were as follows: ______________________________________Additive Max. temp. (�C.) Time (min.)______________________________________control 120 1.5n-butanol 127 2sec-butanol 109 6-7tert-butanol 97 14.5______________________________________ Two foam samples were prepared by intimately blending the following ingredients in the parts shown and allowing the foams to form. ______________________________________INGREDIENTS R S______________________________________commercial polymeric MDI 100 100ethylene oxide capped poly- 40 40oxypropylene triol (MW 4500)silicone surfactant 2.0 2.0tetramethyl-ammonium octoate 2.5 2.533% in methanoltert-butanol -- 6.0PROPERTIEScream time (sec.) 23 42rise time (sec.) 31 53tack free time (sec.) 35 57density (kg./cu. m.) 270 115______________________________________ By adjusting the concentrations of secondary or tertiary hydroxyl and catalyst level, a foaming profile, i.e., the relationship between cream time, rise time and cure time, can be adjusted within wide limits. This processing control is very desirable in making isocyanurate solids and foams. Patent Citations
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A 27-year-old Molalla man was hospitalized Thursday after he lost control of his motorcycle on a sharp 90-degree curve on Mulino Road, about two miles from Mulino.
Faron Michael Bennett was reported in good condition Friday morning at Oregon Health & Science University hospital.
A motorist called 911 about 5:30 p.m. to report finding an injured man lying by the roadside. The Clackamas County Sheriffs Office said Bennett's green 1999 Kawasaki Ninja motorcycle landed about 50 feet away in the stubble of a farmers grain field. It did not appear that any other vehicles were involved in the crash.
Three units from the Canby Fire District responded and transported the injured man to the hospital.


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Hey guys, I'm fermenting my first batch right now, and an having so much fun with this. I love beer and I also love spicy things, on my next batch I'd like to combine the two. I had an awesome jalapeno beer in Weed, California, and would like to emulate that, but maybe with habaneros. Is this a totally stupid idea, and if not, when would I add them? Thanks in advance for the advice, and I have thick skin so don't hold back if I sound like a moron.
Not a moron. People have done it before. Search the forum for pepper beer and ou will get some info.
Will do, thanks!
you can use the search funciton on the forum. Or just google type in hombrewtalk.com (press spacebar) extract pepper beer. This is just the first link I found, didn't even look at it but this can be done although it is real easy to over do it.http://www.homebrewtalk.com/f12/chil...er-beer-80869/
I hate Walder Frey...
No, certainly not an odd request. There are plenty of beers with peppers and spices in them. I'd probably say to add them to secondary, start small and taste it in a few days. I like both spicy and beer, but I'm not a fan of them together so I haven't made it before. I'd do them in an IPA, myself.. Or a Stout. Take half of one, and maybe add it in the last couple of minutes of the boil. And/or rack one to a bit of it in secondary. Remember you can add more, but can't take it out!
---------- Bubba's Backyard Brewery
I made a hot pepper beer really, really early in my brewing career. Recipe - I took a can-and-kilo Pale Ale kit, fermented according to the instructions (including using the packet of yeast that came with the can...my, how I've changed!), a racked the beer onto crushed jalapenos for a two weeks secondary. Racked off the peppers at bottling time. Awesome with grilled anything. Even better if said anything was grilled on a campfire. The point of this otherwise pointless anecdote: Not a stupid idea, and not difficult. No matter what stage of brewing you're at, this style is in your reach. I agree with msujack - do a search, there's better recipes than the one I used...but definitely go for it if you want to!
Boreal Brewer -"Son, you can't sing or dance, I don't like your writing, and you can't draw a picture to save your life. But you make a fine beer!" An 80 year old friend
A lot of folks do it, and do it different ways. Some roast the peppers, some don't. Some soak them in vodka to make an extract, then just add the liquid and not the pepper. Some only add the flesh, some include the ribs and seeds. I'm planning to do a 5-way split batch Smoked Porter with varying degrees of heat (jalapeno, serrano, habanero, ghost, and then all four) some time in the next few months, and I'm still trying to get a good idea on how much to use (I plan on slicing, soaking in vodka, then adding the whole thing, seeds/ribs and all). Seems since people's preference for heat is very subjective, so there's not much agreement.
Up Next: Oud Bruin, Flemish Pale Ale, Kriek Primary: Galaxy Rye APA, Scottish 60/-, Bluebird Bitter Clone v5 Souring: Lamebic, Flanders Red, Brett. C. Old Ale, Sour Stout, Brett C. Wild Bitter, Wild Cider Polypins: Bluebird Bitter Clone v4 Bottled: English Cider, Belgian IPA, Spiced Winter Warmer, Malt Liquor, Dark Mild, Robust Porter, Kitchen Sink Brown Porter In the "cellar": Brett B. Tripel, Quadrupel, Tripel, Brett C. Oaked English Barleywine, Lamebic
The only stupid question is, a question not asked...At least that's what I've always been told. Try it, you never know what your going to come up with, that's the fun part of home brewing....experimentation.
I might think about using a different variety of pepper... you get so much spice for so little pepper with habaneros, it'll be hard to get any pepper flavor at all without making it overwhelmingly spicy. Unless a clean-flavored beer with a ton of capsaicin heat is what you're going for, in which case, carry on...
You guys were awesome. Thanks for all the quick feedback!


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Kristin Cavallari admits prior cocaine use but denies current drug use
By Christopher Rocchio, 05/05/2010
Kristin Cavallari revealed that she has previously used cocaine but said recent claims and speculation that she currently uses the drug are much ado about nothing.
"I tried it in high school. I admitted it! I don't like being around it. I think it's kind of a shady disgusting drug,"
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"Don't you think that if that was really true, it would have come out right after Coachella? Someone would have been talking about it. It would have been on Perez [Hilton] right after Coachella if that was true!"
Rumors that Cavallari was allegedly using cocaine first surfaced earlier this year and were addressed during
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"Up until that, no one had ever expressed any concern about me. It's not even like I go out that much! It just came out of left field and then died down because there is no story, but now with the show premiering again, it came back up!"
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text: We came across Diane and Bill's wonderful B and B by chance on our hunt for burrowing owls. What a find - in a beautiful location overlooking the bay and facing west to take advantage of the spectacular sunsets. We occupied a large comfortable room with views over the bay and the adjacent Osprey nest! With Pelicans fishing and manatees... More


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Feds curtail paper applications for health care law
FORT LAUDERDALE, Fla. — Federal health officials, who encouraged alternate sign-up methods amid the fumbled rollout of their online insurance website, began quietly urging counselors around the country this week to stop using paper applications to enroll people in health insurance because of concerns those applications would not be processed in time.
Interviews with enrollment counselors, insurance brokers and a government official who works with navigators in Illinois reveal the latest change in direction by the Obama administration, which had been encouraging paper applications and other means because of the problems with the website. Consumers must sign up under the federal health overhaul by Dec. 23 in order for coverage to start in January.
"We received guidance from the feds recommending that folks apply online as opposed to paper," said Mike Claffey, spokesman for the Illinois Department of Insurance.
After a conference call earlier this week with federal health officials, Illinois health officials sent a memo on Thursday to their roughly 1,600 navigators saying there is no way to complete marketplace enrollment through a paper application. The memo, which Claffey said was based on guidance from federal officials, said paper applications should be used only if other means aren't available.
Federal health officials discussed the issue during a conference call on Wednesday with navigators and certified counselors in several states.
"They've said, do not use paper applications because they won't be able to process them anywhere near in time," said John Foley, attorney and certified counselor for Legal Aid Society of Palm Beach County, who was on the call.
That contradicts what federal health officials told reporters during a national media call this week, during which they said there were no problems with paper applications.
"There is still time to do paper applications," Julie Bataille, communications director for the Centers for Medicare and Medicaid Services, said on the call Wednesday.
A CMS spokesman declined to comment directly on the issue Friday. "With the recent fixes to the website, we are encouraging consumers to use HealthCare.gov, since it's the quickest way to get coverage, but paper applications remain an option for consumers and navigators if they choose," said spokesman Aaron Albright.
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2014's fast food atrocities
Burger King's black cheeseburger: Made with squid ink and bamboo charcoal, arguably a symbol of meat's destructive effect on the planet. Only available in Japan.
Topics: Entertainment News
If we want computers to be easier to use — and who doesn't? — a good place to start would be with that all-important command, "Undo." Although many of today's computer systems have some sort of undo capability, few of them work consistently throughout the system, or even in one application. As a result, users can't depend upon it, and lots of people lose a lot of work.
The need for a better undo is one of the important ideas in designer Jef Raskin's first book, "The Humane Interface," published earlier this year by Addison-Wesley. Although Raskin is perhaps best known as the creator of the Apple Macintosh project, his book is not a rant arguing why the Mac has a better user interface than Windows. Of course the Mac is better, says Raskin, but both computer systems have fundamental problems that make using them an unpleasant experience for both novices and experts alike.
Raskin bases his arguments not on opinion but on nearly 30 years of research by people around the world who have studied how the human brain interoperates with engineered systems from aircraft to computers. Raskin suggests that we should apply this research to the design, or redesign, of today's operating systems.
One of Raskin's early observations is that people quickly become habituated to routine processes and procedures. This works to both the advantage and the detriment of the interface designer. Habituation lets an experienced person use a well-designed interface more quickly. But that same habituation can also lead to errors — sometimes catastrophic ones. And that's when it would be great if we had a truly workable undo.
Consider the Yes/No or OK/Cancel questions that many computer systems ask. "Do you really want to empty your trash? (Y/N)" "Are you sure you want to permanently delete the selected items?" People become so accustomed to these questions and pop-up boxes, Raskin writes, that after seeing them a few times they habitually click "OK," even when they should click "Cancel." Hence, they click right through something like: "WARNING: All data on non-removable Disk Drive C: will be lost. Proceed with format? (Y/N)"
Far better than giving the user a Yes/No or OK/Cancel choice would be to create a general undo facility that worked consistently throughout the entire computer system. When, weary from slaving for hours on that paper you're writing, you mistakenly tell your word processor to shut down without saving the final version, you don't want it to ask, "Are you sure?" You want it, when you realize your mistake, to promptly undelete any work you've foolishly trashed.
Raskin's words became especially poignant to me last month, when a minor user-interface tick and an OK/Cancel alert caused me to lose the minutes of a board meeting that I had been taking on my Palm Pilot. It was an hour into the meeting, and one of the organization's board members asked me to beam my minutes into her Palm VII. Trying to be helpful, I clicked the button to display my computer's pull-down menu, selected "Beam Memo" and was prompted with a pop-up box asking: "Beam current memo? OK/Cancel." I clicked "OK" and suddenly the memo vanished.
Of course, I hadn't clicked "Beam Memo" on the Pilot's menu, but "Delete Memo." As Raskin notes, I had been so focused on the idea of beaming my memo to the board member that I had misread the confirmation box — a box that was designed to prevent me from doing precisely what I had then proceeded to do.
Instead of a confirmation box, a far better design would be to have the computer always delete the menu, but then to allow the ability to undo the last action. The ubiquitous OK/Cancel box is a terrible user-interface design, writes Raskin, because it slows you down the majority of the times you are actually trying to do something, and the few times that you really, really need the confirmation box — when you are habituated to a user interface and about to make a mistake that will cause you to irrevocably lose data — you don't stop to read it. You don't stop because you have become habituated.
Of course, the Palm operating system does have an undo feature. Unfortunately, it doesn't work all the time. Undo works for undoing modification to text in the memo pad application, for example, but it can't undo the deletion of a memo. There's an undo option on the Palm's appointment book program, but it can't undo changes you might make to an appointment's date or time. These limitations aren't the result of the Palm's low-powered microprocessor or small memory; they're the result of poor design — poor design of both the memo pad application and the underlying operating system. And they are design problems shared by many systems.
Speaking as a programmer and as a designer, creating a generalized undo feature is hard work. To do it, you must remember every change that affects the user's data so that you can undo those changes if the user asks. Few application frameworks provide an undo facility, so each programming team has to create its own. Although this shouldn't be hard to do in principle, in practice it enforces a discipline that few of today's programmers are up to. One of the reasons, I think, is that they lack good examples: Since no program currently on the market today does undo properly, there is little incentive for other programmers to do better.
Consider the undo feature in Microsoft Word. Overall it's pretty good, but it frequently behaves in an unpredictable manner. For example: Type a paragraph of text. Select the paragraph with your mouse and choose the "Copy" command. Now select the last sentence of the paragraph and choose the "Cut" command. Now click undo, click the mouse at the end of the paragraph and choose the command "Paste." What happens? You should get the entire paragraph, but, instead, you get just the last sentence. That's because Microsoft's undo doesn't really undo your last command; instead, it reverts to the last change to your document. In this example, the last command also affected the clipboard, which Word's undo command doesn't restore.
Many applications don't even have an undo facility. Last year, for instance, I received an e-mail from a reader who was furious at Intuit. The reader had lost a significant amount of time because Intuit's Quicken lacks an undo feature and he had inadvertently made a change to a transaction in his checking register. Of course, he didn't know what the change was — it was, after all, inadvertent — and he spent several hours trying to figure out why a reconciled transaction had disappeared but his register still balanced. The man eventually discovered that he had changed the year of a credit card charge from 1999 to 1909. An undo feature that would undo a change to the last transaction would have saved him much work and frustration.
The computer industry has technical standards that describe everything from the voltage transmitted on an Ethernet cable to procedures that companies must follow for ensuring the "quality" of their products. But few standards ensure that these products will be usable or, to use Raskin's word of choice, humane. Building an undo feature that always works would be a good place to start.
"Simson Garfinkel is a frequent contributor to Salon, the Chief Technology Officer of Sandstorm Enterprises, and the Chief Scientist of Broadband2Wireless, Inc."
Burger King's black cheeseburger: Made with squid ink and bamboo charcoal, arguably a symbol of meat's destructive effect on the planet. Only available in Japan.
McDonald's Black Burger: Because the laws of competition say that once Burger King introduces a black cheeseburger, it's only a matter of time before McDonald's follows suit. You still don't have to eat it.
Domino's Specialty Chicken: It's like regular pizza, except instead of a crust, there's fried chicken. The company's marketing officer calls it "one of the most creative, innovative menu items we have ever had" -- brain power put to good use.
Arby's Meat Mountain: The viral off-menu product containing eight different types of meat that, on second read, was probably engineered by Arby's all along. Horrific, regardless.
KFC'S ZINGER DOUBLE DOWN KING: A sandwich made by adding a burger patty to the infamous chicken-instead-of-buns creation can only be described using all caps. NO BUN ALL MEAT. Only available in South Korea.
Taco Bell's Waffle Taco: It took two years for Taco Bell to develop this waffle folded in the shape of a taco, the stand-out star of its new breakfast menu.
Krispy Kreme Triple Cheeseburger: Only attendees at the San Diego County Fair were given the opportunity to taste the official version of this donut-hamburger-heart attack combo. The rest of America has reasonable odds of not dropping dead tomorrow.
Taco Bell's Quesarito: A burrito wrapped in a quesadilla inside an enigma. Quarantined to one store in Oklahoma City.
Boston Pizza's Pizza Cake: The people's choice winner of a Canadian pizza chain's contest whose real aim, we'd imagine, is to prove that there's no such thing as "too far." Currently in development.
7-Eleven's Doritos Loaded: "For something decadent and artificial by design," wrote one impassioned reviewer, "it only tasted of the latter."


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| UpdatedDoctors at a British hospital were startled when an upset patient told them that the clock in his ward had announced his time was up, the British Medical Journal (BMJ) reports.
Topics: offbeat, human-interest, doctors-and-medical-professionals, health, england, united-kingdom
A bulldozer driver from the Kalgoorlie superpit is among the group which has won the ABC's Exhumed battle of the bands competition.
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| UpdatedAs if being an anti-apartheid hero wasn't enough, Nelson Mandela also had an enviable sense of humour.
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| UpdatedNelson Mandela announces his retirement with a twist: he wants to be left alone
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| UpdatedNelson Mandela's advisor growled at him when he said he would retire
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| UpdatedNot one for formalities, Nelson Mandela put in a call to the Queen directly
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| UpdatedIn the pantheon of truly terrible garden smells, fertiliser springs to mind more readily than the scent of a flower.
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| UpdatedA communal latrine of fossilised faeces has been found to date back 240 million years, 20 million years earlier than the previous record-holder.
| UpdatedFrom Cardboard Kev to the carbon tax hokey pokey, view a collection of memorable moments from Federal Parliament.
Topics: federal-parliament, offbeat, race-relations, australia
| UpdatedA war of words has broken out between staff and students at the University of Sydney over the handling of a law exam that was interrupted by a fire alarm.
Topics: university-and-further-education, education, community-and-society, offbeat, human-interest, the-university-of-sydney-2006
| UpdatedA grazier in central-west Queensland says she is a little bemused at a friendship that has developed between a baby goat and an 800-kilogram Brahman bullock.
The unlikely friendship is blossoming on the Newstead cattle station near Ilfracombe, east of Longreach.
Owner Tracey Walker says the one-month old kid Moe has taken up with a bullock called Lickity Split since birth.
Topics: animals, offbeat, ilfracombe-4727, longreach-4730, mount-isa-4825, qld
| UpdatedShe's 98, he's 102 and their 81st wedding anniversary is fast approaching. Find out their secret to a happy marriage.
Topics: marriage, community-and-society, offbeat, united-states
She's 98, he's 102 and they've been married for 80 years. Find out their secret to a happy marriage.
Topics: marriage, offbeat, united-states
| UpdatedThe assassination of John Fitzgerald Kennedy, the 35th president of the United States, on November 22, 1963, remains one of the defining events of the 20th century.
In the minds of many, much about what happened that day remains shrouded in mystery. Fact Check reveals 10 unusual facts about the death of JFK.
Topics: world-politics, offbeat, united-states
Take a look at some of Australia big assets.
Topics: human-interest, offbeat
Topics: television, offbeat
| UpdatedThe Oxford dictionary says this photo - posted on ABC Online in 2002 - is the world's first known 'selfie'.
Topics: internet-culture, photography, offbeat, armidale-2350
| UpdatedIn a massive city-wide effort, San Francisco has transformed itself into Gotham City for 'Batkid', a five-year-old boy battling cancer.
Topics: human-interest, offbeat, united-states
| UpdatedA famous hotel rebuilt every winter in northern Sweden using only ice will this year install fire alarms.
Topics: human-interest, offbeat, travel-and-tourism, travel-health-and-safety, sweden
| UpdatedThe Christmas tree was sitting in position in the ABC Adelaide newsroom, but not yet decorated when News Breakfast crossed to a live interview guest. It prompted this exchange later between Michael Rowland and Beverley O'Connor, hoping the festive spirit would build.
Topics: offbeat, sa, adelaide-5000
| UpdatedGlasgow has dropped plans to stop jokers putting traffic cones on a celebrated statue's head, after more than 10,000 people signed a petition in protest.
Topics: offbeat, human-interest, scotland, united-kingdom
| UpdatedMarvin, a golden retriever, sits in the sidecar of a 1955 BMW R50 motorbike.


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Jon Stewart defends satire on Egyptian TV
CAIRO — Amid growing tension at the approach of the June 30 anniversary of Mohamed Morsy's assumption of Egypt's presidency, Jon Stewart, the host of Comedy Central's "The Daily Show," appeared on Egyptian TV on Friday night, drawing laughs in a funny yet very serious tribute to the importance of satire in a free state.
Stewart was the guest of Bassem Youssef on "Al Barhnameg," or "The Program," one of Egypt's most popular shows. In March, Morsy's government charged Youssef with insulting the president and Islam. Youssef was released on $2,200 bond, and Stewart has stood by him.
On Friday, Youssef introduced Stewart by saying that he had brought in one of the many feared spies of the regime. Stewart, wearing a black mask and led by two men in suits, walked in. As he lifted the mask, the crowd cheered.
Stewart deployed some Arabic: "Ani regal basset. Membaasaa al riftya," or "I am a simple man. I don't want to be carried."
He also got serious.
"If your regime is not strong enough to handle jokes, then you have no regime. Yes, maybe (a joke) is an insult, but it is not an injury," Stewart said.
Youssef, he said, "is showing satire can still be relevant. It is just the opportunity to be heard."
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Durham, NCUSA 27701
January 20, 2014
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Video | Homepage - Dorset Echo
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Royal Manor Prom 2012
10.34am Tuesday 3rd July 2012
STUDENTS got glammed up for the 2012 Royal Manor Prom at Southwell Business Park on Portland.
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Australian Al-Jazeera reporter Greste deported, Fahmy and Mohamed still...
Steven Tyler, Charli XCX headline Rolling Stone party on Super Bowl eve
Justin Timberlake has confirmed his wife Jessica Biel is expecting a baby...
Cartoonist Steve Nease goes all the way back to 1912 to find a suitable and...
CLARINGTON -- Clarington is changing and so is its local library....
NEW YORK, N.Y. - Boston Bruins forward Shawn Thornton said Sunday he won't contest a fine of more than $2,800 for squirting water from the bench at Montreal Canadiens defenceman P.K. Subban in the final minute of Game 5 of the Eastern Conference semifinals.
"I obviously got caught up in the moment," Thornton said on an offday at the TD Garden. "I'm sorry that this silly incident kind of overshadowed how my teammates played and the great win and how good this series has been.
"There's definitely more important things that we can focus on."
The Bruins were leading the Canadiens 4-2 in the final minutes Saturday night when Subban skated past the Boston bench with the puck. Thornton squirted water at the Montreal defenceman, hitting him in the face shield.
Angered, Subban approached the bench and exchanged words with Thornton. He then went to complain to the referee.
"Somebody sprayed water on my visor at the end of the game. I couldn't see out of half of it," Subban said after the game, acknowledging the incident, while annoying, did not affect the outcome. "I don't want it to be bulletin board material."
Boston held on to win the game 4-2 and take a 3-2 lead in the best-of-seven series. The Bruins need a victory Monday night in Montreal to eliminate the Canadiens and avoid a decisive seventh game in Boston on Wednesday.
The fine of $2,820.52 is the maximum allowed under the league's collective bargaining agreement with the union. The money goes to the players' emergency assistance fund.
Bruins coach Claude Julien said he didn't approve of Thornton's behaviour and let him know.
"As a coach, you always want to support your players but there's certain things you can't support," Julien said Sunday. "I don't think I can support Shawn on those actions.
"To me, I don't think we like seeing our players do that. Now whether he got caught up in the game or whatever, to me he's got to own up to it."
At the Canadiens training centre in Brossard, Que., coach Michel Therrien seemed satisfied with the fine.
"What are you going to do?" he said with a shrug. "That's not something we appreciate, that's for sure."
By The Associated Press
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Life is a breeze on Lefkada, a cheery Greek isle that inspires delusions of grandeur
The sea swilling about the Ionian Islands in Greece is normally as quiet as a millpond.
But not today, which is a pity, because we are in a 30 horsepower boat in the thick of a storm. The hull slams up and down into the waves; we're pelted with rain and there's even a call for life jackets.
No wonder all the other boats made a quick dash for the shore, while we had one final swim off pretty Scorpios (the Onassis family's private island).
Aristotle's playground: The private island of Scorpios near Lefkada, owned by the Onassis family, is something of an inspiration, shimmering invitingly on the horizon
By the time we arrive back on Lefkada, the storm has passed and Dennis, the boat owner, ensures us that these weather hiccups are over in minutes.
Maybe. Though there's nothing like raising the tempo on what is otherwise a supremely lazy beach holiday – without a drop of rain thereafter.
Lefkada is joined to mainland Greece by a lagoon-lined causeway and is only 40 minutes by car from Preveza airport.
If you are hiring a car, invest in the extra insurance. The roads are riddled with pot holes, exuberant drivers, hair pin bends and sign-free junctions.
Our group of five friends are staying in a newly-built stone house sitting well above the din of the town. It could be walking distance if it wasn't for the very steep hill, which demands first gear growling all the way to the top, where it overlooks Madhouri (owned by the family of poet Nanos Valaoritis), Sparti, Skorpios and Meganisi.
Shipshape: Jenny, left, and her fellow crew members prepare to head out to the private island of Skorpios for a spot of sea swimming
The view is reason enough to stay put and do nothing but lounge and stare. But pool lolling is not a patch on sea swimming - and Lefkada does beaches brilliantly.
Culture isn't the island's strong point - according to our villa representative. Phew. Avert your eyes from those monastery signs (the hike to uninhabited Faneromeni is off the agenda). Sound the culture claxon.
There's sand on the west side, pebbles on the east, both blissfully warm, instantly deep, with a sprightly sea and few people anywhere.
The nearest, nicest beach from our villa is at Poros, a 15-minute drive away to a curvy bay of white chalky pebbles - impossible to walk on with grace. We also like Mikros Gialos, five minutes further on in the car.
Porto Katziki, on the west coast of Lefkada, is just one of the many family-friendly beaches on the island
At Poros you can swim to an empty private beach around the severely sliced rocks and there's a leafy taverna serving garlicky Greek lunches and iced coffees.
It's term time, so there are no children, only couples and retired locals, including a biker with resplendent Poseidon-like moustache and Hooters t-shirt.
These beaches are, though, supremely family friendly, they shelve gently and are full of shady umbrellas.
The west coast feels more off-piste. It takes over an hour to toil to the beaches here as you climb the interior, which is more than a kilometre above sea level.
High up, it's almost tropical. Rain threatens; roads narrow; toothless women grin by their honey and olive oil stalls. Gialou beach, the first of three on this strip, is almost deserted.
Cafe chairs rust overlooking the sea, which is a shame because a cold beer would have been just the ticket on this shade-free stretch of sand - though when it comes to building a makeshift teepee, the abandoned cafe is a goldmine. The east side of the island is a sailor's playground.
Poros at sunset, where leafy tavernas serve garlicky Greek food and iced coffees
Nearly all the passengers from our flight are bussed off to craft moored around Nidri, a touristy strip with shops offering everything from homemade gelato (we try mojito, the zingy signature flavour) to rubber chickens, wigs, full English breakfasts, Slovenian evenings and nights out to the beat of Dj Feta. There are also bakeries laden with baklava, pastries, breads of every kind.
The beat back at our villa is forever mellow - but villa holidays can be dangerous.
By day three we are all plotting to buy our own place in the sun. Scorpios is something of an inspiration - shimmering invitingly on the horizon.
Aristotle's private island has a deep harbour and helipad, naturally. Reports over the years that Madonna, Armani and even Bill Gates had bought it are untrue.
Totting up our savings on Villa Galatia's lofty balcony, a big night out at Dj Feta's seems rather more likely.
Travel Facts
Villa Galatia or the sister house Villa Galini is available from CV Travel (0207 401 1026, www.cvtravel.co.uk) from £2,015 per week including maid service, food hamper and car hire based on a maximum occupancy of six. Prices for smaller parties and flights are available on request.
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text:
Received my Novice license in 1958 and I have been active ever since. In the early 90's I upgraded to Extra Class. I operate CW and PSK31. My station consists of an Elecraft K3/100 coupled with a P3 scope for CW operations and a second K3/100 for digital work. I use a computer to handle logging needs and to integrate the various radio units. The computer also handles contest logging for me and updates new firmware for the Elecraft equipment. This is the main operating postion. For CW keying I use an iambic paddle Model P-2 by K8RA (sk) and a BY-1 by Bencher. For longer ragchewing I use a keyboard. Over the years I have built and reworked several straight keys that I used often. Now, due to health issues caused by aging I can't use a straight key anymore so I rely on either a paddle or my keyboard for CW. I am an active member of ARRL, NAQCC #3894, SKCC #1540, FISTS #4687 and ARCI #9616. Pictured are a several straight keys that I either fabricated or rebuilt and used for a number of years. Antennas consist of a CF Zepp up 30 feet and a separate 40 meter dipole up 20 feet. Both antenna systems have home made masts that are self supporting. 1656229 Last modified: 2015-01-31 22:07:02, 2102 bytes You must be logged in to file a report on this page
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Written on: 05/04/2013
Managed to get 2 tickets for my Daughters the day after they sold out.
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Go Navy! – We have four stores for you to Shop Navy…. The Gift Shop and Museum Stores are open to the public. We also have a Navy Online Store for your online shopping convenience. The Midshipmen Store is available to authorized patrons. All offer tax free shopping with proceeds supporting the Brigade of Midshipmen.
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Member, The American Ceramic Society.
Reaction Mechanisms in Al2O3/CuO Infiltration by Liquid Al
Article first published online: 9 JUL 2012
DOI: 10.1111/j.1551-2916.2012.05334.x
© 2012 The American Ceramic Society
Additional Information
How to Cite
Guedes, M., Ferreira, J. M. F., Ferro, A. C. (2012), Reaction Mechanisms in Al2O3/CuO Infiltration by Liquid Al. Journal of the American Ceramic Society, 95: 3064–3070. doi: 10.1111/j.1551-2916.2012.05334.x
Publication History
- Issue published online: 2 OCT 2012
- Article first published online: 9 JUL 2012
- Manuscript Accepted: 26 MAY 2012
- Manuscript Received: 20 OCT 2011
Funded by
- Portuguese Foundation for Science and Technology. Grant Number: SFRH/BD/25711/2005
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Let it snow: Your pictures of today's flurries across Birmingham and the Black Country
Cameras and phones at the ready as freezing weather sweeps across West Midlands sparking wintry showers
TRAVEL/WEATHER: Here's how the snow's affecting traffic in Longbridge near Bournville College which will close today because of weather conditions.
More »TRAVEL: Snow on the M42 southbound is slowing traffic and causing a hazard between J3 and J3A M40.
More »TRAVEL: On the M5 southbound all lanes are now open after an obstruction has been removed and snow cleared between J3 and J4.
More »TRAVEL: In Lickey snow is making it tricky for drivers in Rose Hill.
More »TRAVEL: On the M6 northbound an exit slip road is partly blocked and traffic is queueing after an accident at J10.
More »WEATHER: Bournville College has said it will close this afternoon because of the "extreme weather conditions".
More »TRAVEL: Trafiic's queueing on the A38(M) Aston Expressway outbound between Aston Road/Newtown Middleway (Dartmouth Circus) and M6 J6 (Spaghetti Jnuction).
More »TRAVEL: Snowfall is causing significant problems across the West Midlands.
More »WEATHER: Black swans are being turned white by falling snow in Moseley.
More »NEWS: The general election will see more overnight counts scheduled, MPs have heard.
More »WEATHER: It's not quite time for the St Bernards and barrels of brandy but snow is falling in Brum.
More »


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Le BLANC Pages (100+)
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Le BLANC
News Death Notice
Le BLANC, Randall G. "Randy" 56, of Springfield, died unexpectedly Friday morning, October 12, 2012 in Springfield Regional Medical Center. He was born in Port Dalhousie, Ontario, Canada on July 23, 1956, the son of H.A. "Joe" Le Blanc and Joan Moorhouse. He was the vice president of the Trivial Pursuit Company (Horn Abbott) for 16 years. While working for Horn Abbott, he served as the business advisor to the Prime Minister of Barbados. Following the sale of Horn Abbott to Hasbro of England, Randy moved to Springfield with his wife, Sunny and became vice president of sales and marketing for the Hugo Bosca Leather Company. He was currently working for Sears. He was a member of the Vineyard Church, Northridge where he was one of three leaders of the Men's Group. He was the beloved husband of Deborah "Sunny" (Cave) Le Blanc; father of J. Tyler Le Blanc of Springfield; step father of Brent (Jessica) Le Blanc of Port St. Lucie, Florida, Brad (Sarah) Husk of Yellow Springs and Valerie (Tom) Rieker of Springfield; brother of J. Blake (Lori) Le Blanc of Panama City, Panama and Jody (Daniel) McKay of Calgary, Alberta, Canada. He was preceded in death by his parents. Randy's funeral service will be held at 11:00 a.m. Tuesday in the Vineyard Church. A gathering of family and friends will be held in the church one hour prior to the service. Burial will be in Kingscreek Cemetery, Urbana. You may express condolences to the family at
Published in Springfield News-Sun from Oct. 13 to Oct. 15, 2012
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LEAP Grant applications are live! Our Literacy and Education in Action Program […]
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January 27, 2014
**Commercial white papers, product videos, and other sponsored documents posted on this site are paid content from third-party companies; inclusion and posting on this site does not imply an endorsement nor recommendation of the content by Technology Publishing/PaintSquare. By signing in and viewing or downloading this paid content, you agree to make your name and full contact information available to the sponsor of the content.
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My Car Is Back!
Guess what? My car's back, good as new! Well, some people might dispute that, stating that body shops can never actually return a vehicle to pre-accident condition because they can't duplicate certain factory procedures. But…my Honda Civic looks great!
As you recall, I hit a deer on June 7 and caused quite a bit of damage to my car. I walked away without a scratch, but the Civic sustained $6,000 of damage per the estimate at Nagy's Collision Specialists in Doylestown, Ohio. I chose Nagy's because Ron Nagy is a friend of mine, and I knew he'd do right by me. Plus, they're Honda certified.
Now, about that estimate. It was very thorough, accounting for every nut, bolt and clip. Frame setup and measure. Alignment. The works. I showed it to other shop owners and they agreed practically nothing was left out. Plus, everything was written OE. For these reasons, I thought I would certainly face friction from my insurer, GEICO.
But I didn't. In fact, the manager at Nagy's told me he waited three days for GEICO to reply about coming out to see the car before emailing them once again. The response? "Just run it through." Wow! They didn't even come out to see the car! After all the horror stories I've heard from you guys about customers getting steered and lowballed, I was shocked. They never tried to steer me, and they didn't haggle about the estimate. I even got an OE radiator!
Someone suggested, "Well, GEICO probably knew who you were!" I don't know. But I was prepared for the worst, and ended up having a smooth experience.
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of 28,259 Video Games
< what's the formula?
Uniracers, released as Unirally in PAL territories, is a video game created by DMA Design and Nintendo of America for the SNES in North America in December 1994 and in the PAL territories on April 27, 1995. The game focuses on fast moving action, and was released to show that the SNES could handle games similar to SEGA's popular Sonic games.
... more on Wikipedia


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by Sven Knispel
Due to major changes by Google in Kitkat root access is required from 4.4 and upward (see here for more details: https:/ …
100,000+ downloads, Rating 4.54 (7577)
Новости Ярославля
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Самые свежие новости из жизни города и области в твоем устройстве. Просматривайте фоторепортажи и инфографики, делитесь …
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Taringa! Shouts
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Súmate a la Inteligencia Colectiva con la aplicación oficial de Taringa! para Android.
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Great for card and board games: Magic, Carcassonne, etc...
With BoardGame Scorer you can :
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Via WiFi or Bluetooth connect to your PC/NB, BL Windows App Remote can control your application is running on Windows.
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The DEMO version is a fully functional version of the application, which can be used for 24 hours.
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Four nerds, drawn into a fantasy world and mistaken for heroes, have to battle their way through a massive, crazy advent …
10,000+ downloads, Rating 4.74 (3959)
by Foose Games
Motorcycles! Cars! High Speed! Get your Super Sport Motorcycle and ride on this Challenging game!!! Can you survive this …
1,000,000+ downloads, Rating 3.66 (20465)
Mac Miller
by ReverbNation (12)
The brand new official Mac Miller Mobile App is now available! Stream our music, see pictures, check out our bio, and sh …
100+ downloads, Rating 3.67 (3)
ES File Explorer File Manager
by ES APP Group
ES, 300 millions global downloads, file manager trend leader on Android!
Rated as one of best resource management tool …
50,000,000+ downloads, Rating 4.52 (1284622)
Steampunk Future City LWP
by SamsStuff
Steampunk Future City Live Wallpaper: View from a steampunk style futuristic place.
Set in a steampunk future city setti …
50+ downloads, Rating 4.00 (2)
Сите Македонија
by Arkenstone
Your biggest collection of Macedonian radios is here !!
Macedonia all brings collection of your favorite radios and FM s …
100+ downloads, Rating 4.92 (12)
Root Call Blocker Pro
by Fahrbot
Root Call Blocker is a powerful call, SMS and MMS blocker for root users. Stop bill collectors and text message spammers …
10,000+ downloads, Rating 4.12 (1843)