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21. 发明专利

GB481099A Process for rendering cellulosic material water-repellent 未知
公开(公告)号：GB481099A
公开(公告)日：1938-02-28
申请号：GB2345236
申请日：1936-08-26
申请人： REGINALD JOHN WILLIAM REYNOLDS , ERIC EVERARD WALKER , ICI LTD
IPC分类号： D06M15/423
摘要： Cellulosic materials such as cotton, jute or linen fabrics, paper, regenerated cellulose, cellulose esters and ethers, e.g. viscose and cellulose acetate are rendered water repellent by treatment with an aldehyde and an amide of a higher fatty acid having at least 10 carbon atoms, or with a pre-formed reaction product of such an amide compound with an aldehyde, and subjecting the treated material, preferably in the presence of an acid substance as catalyst, to the action of dry heat. The treatment may be carried out in the presence of a wax. Example 3 described treating mercerized cotton fabric with an aqueous dispersion made by milling in a ball mill stearohydroxy-ethylamide water and a naphthalene formaldehyde sulphuric acid condensation product prepared as described in Specification 224,077, [Class 1 (i)], and adding sodium dihydrogen phosphate, drying at 30-40 DEG C. and then heating at 120 DEG C. Reference has been directed by the Comptroller to Specification 463,300.ALSO:Cellulosic materials such as cotton, jute, or linen fabrics, paper, regenerated cellulose, cellulose esters and ethers, e.g. viscose and cellulose acetate are rendered water repellent by treatment with an aldehyde and an amide of a higher fatty acid having at least 10 carbon atoms, or with a pre-formed reaction product of such an amido compound with an aldehyde, and subjecting the treated material, preferably in the presence of an acid substance as catalyst, to the action of dry heat. The treatment may be carried out in the presence of a wax. Suitable acid amides are oleyl amide, stearamide, lauramide, lauryl benzamide, stearomethylamide and stearanilide. The reaction product may be stearohydroxymethylamide prepared as described in Specification 475,170. The reagents may be applied simultaneously or successively as solutions in organic solvents such as acetone or as aqueous dispersions. The aldehyde, e.g. formaldehyde or paraformaldehyde may be applied in aqueous solution or as vapour. Suitable acid catalysts are sodium dihydrogen tartrate, tartaric acid and lactic acid; they may be applied before, together with, or after the treatment reagents. Examples describe (1) treating cotton fabric in an acetone solution of stearamide, drying and immersing in aqueous formaldehyde containing sodium dihydrogen phosphate, drying at 30 DEG C. and heating at 130 DEG C.; (2) wetting cotton fabric with an aqueous solution of sodium dihydrogen phosphate, drying, treating with an ethanol or acetone solution of stearohydroxymethylamide or oleyl hydroxymethylamide at 40 DEG C., drying at 30-40 DEG C. and heating at 120 DEG C. Alternatively, the catalyst may be phosphoric acid added to the solution of the amide; (3) treating mercerized cotton fabric with an aqueous dispersion made by milling in a ball mill stearohydroxyethylamide, water and a naphthalene formaldehyde sulphuric acid condensation product prepared as described in Specification 224,077, [Class 2 (iii)], and adding sodium dihydrogen phosphate, drying at 30-40 DEG C. and then heating at 120 DEG C.; (4) impregnating cotton fabric in a warm solution containing paraffin wax dissolved in benzene and methylol stearamide and phosphoric acid dissolved in methylated spirits, drying at 35 DEG C. and then heating at 130 DEG C. French Specification 797,049 also is referred to. Reference has been directed by the Comptroller to Specification 463,300.

22. 发明专利

GB669195A Medical and surgical dressings 未知
公开(公告)号：GB669195A
公开(公告)日：1952-03-26
申请号：GB835149
申请日：1949-03-28
申请人： JOSEPH EDWIN DAVISON , REGINALD JOHN WILLIAM REYNOLDS , FRANCIS LESLIE ROSE , ICI LTD
IPC分类号： A61L15/26 , A61L15/46
摘要： A material for use in medical and surgical dressings comprises a thin film of an N-alkoxymethylpolyamide containing at least 0.04 per cent by weight of the polymer of an arylmercuric salt or salts, wherein the aryl group is unsubstituted, e.g. phenylmercuric acetate and phenylmercuric nitrate. The mercuric salt(s) may be incorporated with the polyamide by incorporating in the solution from which the film is to be cast, e.g. phenylmercuric acetate is added to a solution of N-methoxymethyl polyhexamethylene adipamide in aqueous n-propanol. Specification 648,733, [Group VI], is referred to. According to the Provisional Specification a small proportion of an arylmercuric salt(s) is used, a further example being tolylmercuric acetate.

23. 发明专利

GB619576A Manufacture of new polyamides 未知
公开(公告)号：GB619576A
公开(公告)日：1949-03-11
申请号：GB3680646
申请日：1946-12-13
申请人： ERIC ELLERY , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： C08G69/26
摘要： Equimolecular proportions of 1 : 6-diamino-6-methyl-heptane and an aliphatic dicarboxylic acid are heated together to give a polyamide. Amide forming derivatives or low molecular weight polymers or the preformed salt may be used. The reactants are heated until filaments formed from a melt of the polyamide can be cold-drawn into fibres. The acids include oxalic; glutaric; adipic; pimelic; suberic; azelaic; sebacic; brassylic; tetradecanedioic; octadecanedioic; p-phenylenediacetic; hexahydroterephthalic and 1 : 3-cyclopentane dicarboxylic acids. The heating, which is usually at from 200 DEG to 300 DEG C. in the presence or absence of solvent or catalyst and preferably in the absence of air or oxygen, is performed under conditions allowing the removal of water, e.g. under reduced pressure, at least during later stages. A mono-functional amide-forming reactant may be used to stop the reaction at any stage as described in Specification 495,790. The products are soluble in methanol and ethanol and may be made into films forming strongly adhesive bonds to glass, metals and similar surfaces. Solutions in water-miscible organic solvents on mixing with water provide stable aqueous dispersions. In an example, a solution of 1 : 6-diamino-6-methylheptane in ethanol is added to an ethanol solution of adipic acid, the white crystalline salt separating out on standing. The salt is heated for 3 hours at 220 DEG C. in a closed vessel, which after cooling is opened and heated at 255 DEG C. for 1 hour at atmospheric pressure and then for 12 hours at 0.3 mms. pressure. The product, which has an intrinsic viscosity of 0.74, softens at 100 DEG C. and can be spun at 165 DEG C. to filaments which may be cold-drawn.ALSO:1 : 6-Di-amino-6-methyl heptane is converted into an aliphatic dicarboxylic acid salt by interacting equimolecular proportions of the amine and adipic acid in ethanolic solutions, the salt crystallizing out on standing. Reference is made to the formation of salts of the amine with other aliphatic dicarboxylic acids, e.g. oxalic, glutaric, pimelic, suberic, azelaic, sebacic, brassylic, tetradecanedioic, octadecanedioic, p-phenylene diacetic, hexahydro-terephthalic and 1 : 3-cyclo-pentane dicarboxylic acids. The salts are starting materials for the production of polymeric amides (see Group IV (a).

24. 发明专利

GB610138A Process for stabilising highly polymeric linear esters 未知
公开(公告)号：GB610138A
公开(公告)日：1948-10-12
申请号：GB964146
申请日：1946-03-28
申请人： JOHN RICHARD LEWIS , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： C08G63/20
摘要： Highly polymeric linear esters of the kind obtainable by heating glycols of the series HO(CH2)nOH, where n is an integer greater than one but not exceeding 10, with terephthalic acid or with an ester-forming derivative of the acid, are stabilized by incorporating with the reactants, or with the low molecular weight product formed, a monofunctional compound which is a relatively non-volatile acid such as benzoic, phenoxyacetic or stearic acids, or ester-forming derivatives of these acids, a relatively non-volatile alcohol such as benzyl alcohol or an aliphatic alcohol containing more than 9 carbon atoms or their carboxylic acid esters, conveniently the terephthalic acid esters. In the examples, dimethyl terephthalate and ethylene glycol are reacted in the presence of (1) ethylene glycol; (2) ethyl benzoate; (3) ethylene glycol dibenzoate; (4) ethylene glycol stearate; (5) cetyl terephthalate; (6) cetyl alcohol, and in example (7) terephthalic acid, ethylene glycol and benzoic acid are heated. Other monofunctional compounds are specified in the Provisional Specification.

25. 发明专利

GB596688A Production of coloured masses and articles from organic filament-forming materials 未知
公开(公告)号：GB596688A
公开(公告)日：1948-01-08
申请号：GB1638845
申请日：1945-06-27
申请人： JOHN LEWIS MOILLIET , REGINALD JOHN WILLIAM REYNOLDS , WILLIAM TODD , ICI LTD
IPC分类号： C08J3/22 , C08L67/02
摘要： Coloured masses of filament-forming linear polyesters are obtained by incorporating therein while molten a dispersion of a pigment in a different linear polyester or in a linear polyester-amide. In an example, Turkey Red Oxide 2G and the low-molecular linear polyester-amide described in example (1) of Specification 569,170 are mixed to a smooth paste which is added to molten polyethylene terephthalate.

26. 发明专利

GB593163A Improvements in or relating to the manufacture of gelatine blasting explosives 未知
公开(公告)号：GB593163A
公开(公告)日：1947-10-09
申请号：GB1400045
申请日：1945-06-04
申请人： REGINALD JOHN WILLIAM REYNOLDS , STANLEY FORDHAM , ICI LTD
IPC分类号： C06B23/00 , C06B25/30
摘要： 593,163. Gelatine blasting explosives. REYNOLDS, R. J. W., FORDHAM, S., and IMPERIAL CHEMICAL INDUSTRIES, Ltd. June 4, 1945, No. 14000. [Class 9 (ii)] A gelatine blasting explosive has included therein a nitrocellulose cross-linking agent defined as dimethylol urea or a dialkyl ether thereof ; a methylol-melamine or an ether thereof; an organic diisocyanate; an N- methylol- or N-alkoxymethyl-polyamide; an N : N -di-methylol derivative of a dicarboxylic acid ; or an N : N -bis-(alkoxy-methyl) derivative of a diamide of a carboxylic acid. Examples of suitable nitrocellulose cross-linking agents include the hexamethyl ether of hexamethylol-melamine; the dibutyl ether of dimethylol urea ; hexa-methylene diisocyanate, and di-methylol adipamide. The amount of the cross-linking agent employed may be from 0.05 to 0.5 per cent. Examples describe mixtures of (1) nitrated 80 : 20 mixture of glycerine and ethylene glycol, nitrocellulose, dibutylether of dimethylol urea and chalk, and (2) nitroglycerine, nitrocellulose, hexa-methyl ether of hexa-methylol melamine and beta-naphthyl methyl ether. Specification 567,940 is referred to.

27. 发明专利

GB582520A Modification of the properties of filaments, films and other shaped articles derived from nylon 未知
公开(公告)号：GB582520A
公开(公告)日：1946-11-19
申请号：GB1552544
申请日：1944-08-15
申请人： JOHN RICHARD LEWIS , DAVID MCCREATH , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
摘要： Undrawn filaments, bristles, yarns, fabrics, films and like articles derived from a nylon are given an improved reversible extension by heating in the presence of an alcohol, formaldehyde in the vapour form, and an acidic catalyst. The alcohol also may be used in the form of a vapour, and conveniently the nylon articles are first impregnated with the acidic catalyst and then heated to 80-150 DEG C. whilst exposed to formaldehyde and a volatile monohydric alcohol both in the form of vapour. Suitable alcohols for the process are methyl, ethyl, propyl, iso-propyl, n-propyl, iso-butyl, n-butyl, octyl, dodecyl, and methallyl alcohols, castor oil fatty acids, cyclo-hexanol, ethylene glycol, diethylene glycol, b b 1-dihydroxyethyl sulphide, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, and benzyl alcohol. Mixtures of alcohols may also be used. Catalysts specified are phosphoric acid, ammonium dihydrogen phosphate, oxalic acid, maleic acid, glycollic acid, lactic acid and citric acid. Additional ingredients may be added such as wetting, dispersing or swelling agents, e.g. cetyl pyridinium bromide and sodium cetyl sulphate. The products of the invention may be finished or treated in any way, for example, they may be cold drawn. The following examples are given. (1) Polyhexamethylene adipamide yarn is steeped in an aqueous solution of an acidic catalyst at 50 DEG C., removed, squeezed, dried, and heated in a vapour containing formaldehyde and methyl alcohol. The catalysts used are (a) 20 per cent ammonium dihydrogen phosphate, (b) 10 per cent maleic acid and 30 per cent glycollic acid. (2) Polyhexamethylene adipamide yarn is steeped in a solution of oxalic acid, dried, and heated to 100 DEG C. in a vapour containing formaldehyde and methyl alcohol in the ratio 18 : 82. (3) Polyhexamethylene adipamide yarn is steeped in a solution containing oxalic acid and dodecyl alcohol, dried, and heated to 100 DEG C. in the presence of a vapour containing formaldehyde and methyl alcohol in the ratio 25 : 27. (4) The process of (3) is repeated but using a vapour containing formaldehyde and iso-butanol in the ratio 11 : 89. (5) Polyhexamethylene adipamide yarn is steeped in a solution of oxalic acid, dried, and heated to 100 DEG C. in a vapour containing formaldehyde and methyl alcohol in the ratio 18 : 82, and then stretched by about 100 per cent and maintained in its stretched condition for 24 hours. (6) Monofil from the interpolyamide obtained from hexamethylene diammonium adipate, hexamethylene diammonium sebacate and epsilon-aminocaprolactam is steeped in a solution of glycollic acid, dried, and heated to 120 DEG C. in the vapour of formaldehyde and methyl alcohol in the ratio 1 : 1. (7) Fabric woven from a warp of viscose rayon and a weft of polyhexamethylene adipamide yarn is steeped in a solution of glycollic acid, dried, and heated to 115 DEG C. in a vapour containing formaldehyde and methyl alcohol in the ratio 40 : 60. (8) Fabric woven from polyhexamethylene adipamide yarn is steeped in a solution of oxalic acid, dried, and heated to 110 DEG C. in a vapour containing formaldehyde and methyl alcohol in the ratio 25 : 75. The mixed vapours of formaldehyde and methyl alcohol may be prepared by distilling a mixture of equal parts of paraformaldehyde and methyl alcohol until the vapours are present in the required proportion. Specifications 461,236, 461,237, 474,999, 495,790, 534,698 and 582,517 are referred to.

28. 发明专利

GB574739A Treatment of linear polymers with formaldehyde or formaldehyde-liberating substance 未知
公开(公告)号：GB574739A
公开(公告)日：1946-01-18
申请号：GB607442
申请日：1942-05-06
申请人： DAVID AUGUSTINE HARPER , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： C08G18/84
摘要： Linear polymers containing, as integral members of the main chain of atoms therein, groups of the structure but not containing, as integral members of the main chain of atoms therein, groups of the structure where X represents an oxygen or sulphur atom and Q represents an oxygen or sulphur atom or an NH or N-alkyl group, are heated in the presence of formaldehyde or a formaldehyde-liberating substance, whereby their softening points are markedly increased, their solubilities in organic liquids are very much reduced, and their flexibility is increased. Plasticizers, pigments and fillers may be admixed with the products. The linear polymers mentioned above include polymers, polythioureas, and N-alkyl derivatives thereof, as well as polycarbonates and polythiocarbamates. It is preferred to effect the heating in the presence of an acid, an acid anhydride, or an acid-reacting salt, or in the presence of a material which is substantially neutral and remains so during any milling or other mixing operation prior to the heating, but which develops acidity during the heating, e.g. to 100-150 DEG C. Specified formaldehyde-liberating substances are paraformaldehyde, trioxane, dimethylolurea, trimethylolmelamine, hexamethylolmelamine, diphenylol-propane tetra-alcohol, methylolchloracetamide, methylol stearamide, N-methylol-p-toluenesulphonamide, dimethylolurea dimethyl ether, dimethylolurea dibutyl ether, N : N1-dimethyloluron dimethyl ether, 1 : 2-glycol methylene ether, di-(b -hydroxyethyl) formal, and hexamethylene - tetramine - zinc chloride complexes. Specified additions, in the presence of which heating may be carried out, are formic, glycollic, oxalic, succinic, maleic, stearic, adipic, tartaric, salicyclic, anthranilic, phthalic, citric, tannic, boric and phosphoric acids, phthalic and maleic anhydrides, phthalimide, potassium or sodium dihydrogen phosphate, butadiene sulphone, butadiene tetrabromide, 2 : 3-dimethylbutadiene sulphone, styrene dibromide, acetylene tetrabromide, tribromohydroquinone, 1-bromo-2-naphthol, 1 : 6-dibromo-2-naphthol, 1 : 4 : 6-tribromo-2-naphthol, 2 : 4-dibromo - 1 - naphthol, methyl a : b -dibromo-propionate, p-chloroethyl a : b - dibromoisobutyrate, ethyl a - bromopropionate, phenyl trichloroacetate, a : a : b -trichloro-propionitrile, trichloroacetamide, trichloroacetyldiethylamide, N-trichloroacetylanilide, N : N1-di-(trichloroacetyl) methylenediamine, N : N1-di-(trichloroacetyl) ethylenediamine, interpolymers of asymmetrical dichloroethylene and vinyl chloride, and chloranil. Examples are given in which: (1) a polycarbamate obtained from hexamethylene glycol and hexamethylene diisocyanate is heated with paraformaldehyde in the presence of maleic anhydride; (2) a polyurea obtained from decamethylene diamine and hexamethylene diisocyanate is heated with para formaldehyde in the presence of maleic anhydride. Specifications 461,237, 524,795, 528,437, 530,267, 534,699, 535,139 and 32979/38 (as open to inspection under Sect. 91) are referred to.

29. 发明专利

GB514861A Textile treatment agents 未知
公开(公告)号：GB514861A
公开(公告)日：1939-11-20
申请号：GB1475638
申请日：1938-05-17
申请人： REGINALD JOHN WILLIAM REYNOLDS , JOHN DONALD ROSE , ERIC EVERARD WALKER , ICI LTD
IPC分类号： D06M13/46 , D06P1/66 , D06P5/22
摘要： 514,861. Textile assistants ; dyeing. REYNOLDS, R. J. W., ROSE, J. D., WALKER, E. E., and IMPERIAL CHEMICAL INDUSTRIES, Ltd. May 17, 1938, No. 14756. [Classes 2 (iii) and 15 (ii)] Diquaternary ammonium compounds of the general formula where Z and Z1 each represent a tertiary amine, X and Y are chlorine or bromine atoms, and A is a divalent aliphatic hydrocarbon radicle, are made by reacting ethers of the general formula with two molecular proportions of a tertiary amine or amines. As ethers of the general formula, 2-chlorethyl chlormethylether, 2- bromoethyl chloromethyl ether, and 3-chloropropyl chlormethyl ether are specified. As tertiary amines may be used trimethylamine, triethylamine, dimethylaniline, 'alkylpiperidines, N-benzylpiperidine, pyridine, picoline and quinoline. Mixtures of amines may be used, and the reaction may be carried out in two stages, a different amine being used in each stage. The products may be used for increasing the fastness of dyeings of direct dyestuffs on cellulosic materials, or for conferring upon such materials an affinity for acid dyes. In examples, (1) 2-chloroethyl chloromethyl ether is reacted with pyridine (2 mols.) ; (2) 3-chloropropyl chloromethyl ether is reacted with pyridine (2 mols.), (3) 2- chloroethyl chloropropyl ether is reacted with triethylamine (1 mol.) and the product is reacted with pyridine (1 mol.); (4) 3-chloropropyl chlormethyl ether is reacted with alpha-picoline (2 mols.), (5) 2-chloroethyl chlormethyl ether is reacted with N-benzylpyridine (1 mol.) and pyridine (1 mol.), (6) 2-bromoethyl chloromethyl ether is reacted with pyridine (2 mols.), (7) bleached cotton limbric dyed with Chlorazol Fast Red K is impregnated with an aqueous solution containing the product of example 1, squeezed, dried and heated to 150‹ C. ; the fastness of the dyeing to washing is improved, and (8) spun viscose material is padded with an aqueous solution of the product of example 1, squeezed, dried and heated to 140‹ ; the material can then be dyed with acid dyestuffs in the manner normally used for dyeing wool. Specification 394,196 is referred to. 3-Chloropropyl chloromethyl ether is made 'by treating trimethylene chlorohydrin with paraformaldehyde and hydrochloric acid in an aqueous medium. 2-Bromoethyl chloromethyl ether is made by reacting 2-bromoethanol with formaldehyde and hydrochloric acid.

30. 发明专利

GB508523A Manufacture of condensation products from substituted phenols 未知
公开(公告)号：GB508523A
公开(公告)日：1939-07-03
申请号：GB16538
申请日：1938-01-03
申请人： REGINALD JOHN WILLIAM REYNOLDS , ERIC EVERARD WALKER , ICI LTD
IPC分类号： C07D213/20
摘要： 508,523. Hydroxymethylphenol derivatives; dyeing processes; wetting-agents. REYNOLDS, R. J: W., WALKER. E. E., and IMPERIAL CHEMICAL INDUSTRIES, Ltd. Jan. 3, 1938, Nos. 165 and 166. [Classes 2 (iii) and 15 (ii)] Water-soluble compounds are obtained by heating together a phenol substituted by one or more hydroxymethyl groups in the o or p positions and a salt of or inorganic acid anhydride addition compound of a heterocyclic tertiary amine. The - products are believed to be quaternary ammonium salts; and may be used as assistants in dyeing cellulose fibres. The phenols used may also contain, as substituents in the nucleus or side chain, halogen atoms, acylamido, acylamidomethyl, alkyl, aralky or hydroxyaralkyl groups ; the hydroxyaralkyl groups may be substituted by further hydroxymethyl groups. The tertiary amine salt may be made in situ, e.g. by passing in hydrochloric acid gas. The reaction may be carried. out under reduced pressure, or-in the presence of solvents or diluents, e.g. toluene. Substituted phenols , specified include mono. or polyhydroxymethyl derivatives of phenol, cresols; p-tert.-butylphenol, dodecylphenol, octadecylphenol, stearamidomethylphenol, p - chlorophenol, diphenylolmethane, di - o - cresylolmethane, diphenylolpropane and di-o-cresytolpropane. These hydroxymethyl derivatives may be prepared by alkaline condensation of the phenols with formaldehyde or paraform aldehyde. The amines specified are pyridine, c-alkyl pyridines and quinoline in the form of halides, sulphites, nitrates, m-nitrobenzene sulphonates, or p-toluene sulphonates or addition compounds with sulphur dioxide or trioxide. In one example, the picrate of the condensation product is referred to, and in another example the product is stated to give an aqueous solution which foams on shaking. According to the second Provisional Specification, formaldehyde, an acid or acid anhydride, a. heterocyclic tertiary base and a substituted phenol may be brought into combination in various ways. The phenol may be treated with aqueous formaldehyde saturated with hydrogen chloride to form hydroxyphenyl-chloromethane, which is then reacted with the amine, or the phenol may be treated with formaldehyde, hydrogen halide and tertiary amine in succession. The use of halogenacylamidophenols, e.g. p - chloracetamidophenol, is referred to. The formaldehyde may be monomeric or polymeric, or may be furnished by substance such as hexamethylene tetramine or formaldehyde-bisulphite.

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