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    • 2. 发明专利
    • Manufacture of new derivatives of aliphatic alcohols
    • GB475119A
    • 1937-11-15
    • GB1360136
    • 1936-05-13
    • ALFRED WILLIAM BALDWINHENRY ALFRED PIGGOTTICI LTD
    • Quaternary ammonium salts are obtained by the interaction of an aliphatic alcohol, sulphur dioxide, formaldehyde or a polymer such as paraformaldehyde, and pyridine or an alkylpyridine. The products are of the type ROCH2N­X, where R is an aliphatic hydrocarbon radicle, N­ is a molecule of pyridine or an alkylpyridine, and X is an anion of sulphurous or pyrosulphurous acid. Specified aliphatic alcohols are methyl, propyl, butyl, oleyl, dodecyl, hexadecyl and octadecyl alcohols, and these may be single compounds or mixtures such as are obtainable by saponifying spermaceti or by reducing the acids of fats and fatty oils such as coconut oil and palm oil. As alkylpyridines, mention is made of picolines and lutidines, or use may be made of technical "pyridine bases." The reaction may be effected by passing sulphur dioxide into a mixture of the other reagents at 70--100 DEG C. in the presence or absence of a diluent, e.g. benzene, toluene or chloroform. The products derived from the higher aliphatic alcohols form foaming aqueous solutions and are useful as textile assistants. Examples are given of the manufacture of products from paraformaldehyde, sulphur dioxide, pyridine and (1) hexadecyl alcohol, (2) methyl alcohol, (3) butyl alcohol, and (4) dodecyl alcohol. The Provisional Specification refers generally to the reaction of an aliphatic alcohol with sulphur dioxide, an aldehyde and a tertiary amine.
    • 3. 发明专利
    • Improvements in the treatment of cellulosic material
    • GB469476A
    • 1937-07-26
    • GB3577935
    • 1935-12-24
    • ALFRED WILLIAM BALDWINREGINALD JOHN WILLIAM REYNOLDSERIC EVERARD WALKERCLARENCE SYDNEY WOOLVINICI LTD
    • D06M13/322
    • Cellulosic materials are treated with a halogeno-methyl ether of the general formula R--O--CH2--Hal, in which R is a normal or branched chain aliphatic hydrocarbon radical, saturated or unsaturated, of not less than 8 carbon atoms, and Hal is a halogen atom, the treatment being carried out at a raised temperature in an inert organic diluent or solvent for the reagents, and preferably in the presence of an acid-binding agent. As an alternative, there may be used a quaternary ammonium salt formed from the halogeno methyl ether and a tertiary organic amine. The cellulosic material may consist wholly or in part of natural or regenerated cellulose or cellulose esters, e.g. cotton, viscose or other artificial silk including cellulose acetate material, linen, jute or mixtures of these fibres. Paper or films, threads, yarns, woven or knitted fabrics may be treated. The materials may be dyed. The chlormethyl ethers used are obtained by treating the respective alcohol with formaldehyde and hydrogen halide. Chloro methyl dodecyl, sec-dodecyl, cetyl, or octodecyl ether, or a chloromethyl ether of the mixture of alcohols from sperm oil may be used. The treatment renders the material waterproof and gives it a soft handle and these effects are resistant to laundering and dry cleaning. Toluene, benzene, acetone, carbon tetrachloride, trichlorethylene, and other hydrocarbons or chlorinated hydrocarbons may be used as organic diluent or solvent. Pyridine, aniline, N-alkylaniline or dialkyl aniline, di- or triethylamine, piperidine, alkyl piperidines, sodium or potassium carbonate, potassium acetate, or calcium hydroxide may be used as acid binding agent. The treatment is carried out at raised temperature, preferably at or near the boiling point of the diluent. In an example, a -chloromethyl octadecyl ether is dissolved in dry toluene and pyridine is added. Undyed boiled out cotton limbric is immersed in this solution which is heated at 90 DEG C. The fabric is removed, pressed, washed with alcohol, and dried. In other examples, cotton-wool union fabric, gaberdine and limbric are treated. Cotton fabric is impregnated with a solution of octadecoxymethyl pyridinium chloride in trichloroethylene, squeezed, and dried in a current of warm air. It is then baked at 105 DEG C. Limbric is padded with chloromethyl octadecyl ether, diethylaniline, and benzene mixture. It is dried in warm air and then heated at 120 DEG C. on a drying cylinder. Knitted cellulose acetate fabric is immersed in a solution of toluene containing a chloromethyl ether of sperm-oil alcohols, and pyridine. The solution is heated for 30 minutes and the fabric is then rinsed in alcohol and dried. Specifications 340,555, 390,553, 396,992, and 426,482 are referred to.
    • 4. 发明专利
    • Improvements in the production of detergent solutions
    • GB378454A
    • 1932-08-11
    • GB1393131
    • 1931-05-11
    • ICI LTDANTHONY JAMES HAILWOODALFRED WILLIAM BALDWIN
    • Emulsifying and detergent agents are obtained by sulphonating alkylbenzylethers in which the alkyl groups are saturated and contain not less than six carbon atoms. The benzene ring of the benzyl residue may contain substituents such as methyl or chlorine. The detergent action of the products is improved by the presence of soaps or inorganic salts having the same kations as the detergents themselves. Dry solid compositions may be prepared by the addition of such inorganic salts to the soluble salts of the sulphonated alkylbenzylethers. In examples: (1) sulphuric acid monohydrate is used to sulphonate dodecylbenzylether, cetylbenzylether and octadecylbenzylether: (2) sodium chloride is mixed with the sodium salt of cetylsulphobenzylether to form a detergent: (3) another detergent comprises sodium sulphate, the sodium salt of cetylsulphobenzylether and the sodium salt of dodecylsulphobenzylether.ALSO:Wetting, emulsifying and detergent agents which may be used for example for washing raw wool, are obtained by sulphonating alkylbenzethers in which the alkyl groups are saturated and contain not less than six carbon atoms. The benzene ring of the benzyl residue may contain substituents such as methyl or chlorine. The detergent action of the products is improved by the presence of soaps or inorganic salts having the same kations as the detergents themselves. Dry solid compositions may be prepared by the addition of such inorganic salts to the soluble salts of the sulphonated alkylbenzylethers. In examples: (1) sulphuric acid monohydrate is used to sulphonate dodecylbenzylether, cetylbenzylether and octadecylbenzylether; (2) sodium chloride is mixed with the sodium salt of cetylsulphobenzylether to form a detergent; (3) another detergent comprises sodium sulphate, the sodium salt of cetylsulphobenzylether and the sodium salt of dodecylsulphobenzylether. Alkylbenzylethers are prepared from the aliphatic alcohols by known methods, e.g. dodecyl or cetyl alcohol is boiled with sodamide in xylene until ammonia ceases to be evolved, and the resulting sodium compounds condensed with benzylchloride.
    • 6. 发明专利
    • Making woollen materials non-felting and soft
    • GB540613A
    • 1941-10-23
    • GB710740
    • 1940-04-19
    • ALFRED WILLIAM BALDWINLESLIE GORDON LAWRIEICI LTD
    • D06M13/395
    • 540,613. Treating textiles with liquids. BALDWIN, A. W., LAWRIE, L. G., and IMPERIAL CHEMICAL INDUSTRIES, Ltd. April 19, 1940, No. 7107. [Class 15 (ii)] Wool is rendered non-felting and of a soft handle by treating it with an isocyanate of the formula :-R-X-NCO, wherein R is an alkyl radical of at least 8 carbon atoms and X is the divalent radical -CO-O-CH 2 -CH 2 - or is absent, and also treating it, before, during, or after the isocyanate treatment, with a reactive sulphur compound which is acid or is capable of liberating sulphuric or hydrochloric acid on hydrolysis with water, this treatment being so adjusted that the wool is not appreciably weakened. The isocyanate is preferably applied in the form of a solution or dispersion in an inert or relatively inert liquid, e.g. water, benzene, carbon tetrachloride, or white spirit. If it is applied as an aqueous emulsion before the treatment with the reactive sulphur compound, the wool must be dried between the two treatments. In an example, woollen yarn is immersed in a solution of octadecyl isocyanate and sulphuryl chloride in carbon tetrachloride. It is squeezed, rinsed in water, immersed in dilute ammonia, washed with water, and dried. Pentatriacontanyl isocyanate, stearyloxyethyl isocyanate, or tricosyl isocyanate may be used instead of octadecyl isocyanate. In another example, woollen yarn is immersed in a solution of sulphuryl chloride in carbon tetrachloride. It is squeezed and then immersed in a solution of octadecyl isocyanate in carbon tetrachloride. It is squeezed, washed, and dried. Specifications 464,503, 480,775, and 483,707 are referred to.
    • 7. 发明专利
    • Treatment of cellulosic textile materials, paper, films and the like
    • GB477991A
    • 1938-01-10
    • GB1604536
    • 1936-06-08
    • ALFRED WILLIAM BALDWINJOHN GWYNANT EVANSCHARLES EDWARD SALKELDICI LTD
    • D06M13/322D06M13/35D06M13/46D06M13/47
    • Water-repellent properties are imparted to cellulosic materials by impregnating them with a quaternary ammonium salt of the general formula NR R --CH2--N(tert)--X (where R and R stand for radicals at least one of which consists of or contains an aliphatic hydrocarbon radical of 10 or more carbon atoms, N(tert) stands for the nitrogen atom of an aliphatic or heterocyclic tertiary amine, and X stands for the radical of a salt-forming acid) applied from aqueous medium, and if desired, after drying subsequently heating the impregnated material to a temperature such that the said salt decomposes. The group NR R may have the form Alph--CO--NR -- or Alph--N(COOR )-- in which Alph is a higher aliphatic radical, i.e. of 10 or more carbon atoms. Methods of making such compounds are described in Specifications 471,130 and 475,170. When drying is effected after impregnation and before heating, this should be carried out in a rapid current of hot air, or alternatively the drying should be carried out at a temperature below 40 DEG C. so as to avoid decomposition of the quaternary salt. The optimum heating or baking temperature is 90--120 DEG C. In the examples given the following quaternary salts are used, stearamidomethyl pyridinium chloride, bromide or nitrate, stearomethylamidomethyl pyridinium chloride, stearamidomethyl pyridinium hydrogen sulphate, N-carbomethoxyheptadecylaminomethyl pyridinium chloride (obtained from methyl heptadecylcarbamate, formaldehyde, hydrogen chloride, and pyridine), palmitoamidomethyl pyridinium chloride, stearamidomethyl pyridinium sulphite (prepared from stearamide, pyridine, paraformaldehyde and sulphur dioxide), stearamidomethyl pyridinium - m - dinitrobenzene - sulphonate, N - carbomethoxyundecylaminomethyl pyridinium chloride, oleylamidomethyl pyridinium chloride, lauramidomethyl pyridinium chloride, and lauramidomethyl pyridinium sulphate. In place of the above fatty acids, the acids of palm oil, cotton seed oil, tallow or hydrogenated fats may be used. Other amines are those obtained from fatty alcohols or the alcohols of spermaceti or sperm oil. Instead of pyridine, trimethylamine or triethanolamine may be used. The process may be applied to dyed or undyed material, and where dyeing has been effected with direct cotton colours, the dyestuff becomes fixed.
    • 8. 发明专利
    • Process for dyeing cellulosic material
    • GB450981A
    • 1936-07-27
    • GB268635
    • 1935-01-26
    • ICI LTDALFRED WILLIAM BALDWINHAROLD BLACKSHAW
    • D06P1/651D06P3/68
    • Azo dyes, forming on the material; regenerated celluloses, dyeing.--The fastness to rubbing of dyeings obtained upon cellulosic fibres, e.g. of cotton, linen or viscose artificial silk, by the azoic process is improved by conducting the dyeing in presence of a condensation product from a fatty or cycloaliphatic carboxylic acid containing 8 or more carbon atoms, (a) with an excess over an equimolecular proportion of glycerol or with a polymer thereof, e.g. di- or tri-glycerol, the product being an ester of a polyglycerol, or (b) with an excess of a polyvalent alcohol containing more than 3 hydroxyl groups, e.g. sorbitol, erythritol, a lower sugar or with a polymer of such an alcohol. In an example, cotton cops are impregnated for 20--30 minutes with an aqueous solution at 20--25 DEG C. of the 5-chloro-o-toluidide of 2 : 3-oxynaphthoic acid containing turkey red oil, caustic soda, formaldehyde and sodium chloride, the dyeing is developed by treatment for 20--30 minutes in an aqueous solution of Brentamine p fast red TR salt containing sodium chloride and an oleylester of polyglycerol obtained by heating oleic acid (120 parts) with glycerol (400 parts) in presence of potassium hydroxide (0,5 parts) for 12 hours at 280--290 DEG C., and the dyed material is rinsed, soaped at the boil and again rinsed.
    • 9. 发明专利
    • The manufacture of new compounds for the treatment of textiles
    • GB437285A
    • 1935-10-28
    • GB1263034
    • 1934-04-26
    • ICI LTDALFRED WILLIAM BALDWIN
    • Products stated to have emulsifying properties and to be useful as softening and cleansing agents in the textile industry are prepared by reacting a lower alkyl ester of an inorganic acid with a mercaptobenzthiazole which has an alkyl group containing at least eight carbon atoms in the 2-position and may carry substituents such as methyl, methoxy or ethoxy in the benzene nucleus. The lower alkyl ester may contain up to four carbon atoms. In examples: (1) 2-octadecylmercaptobenzthiazole, obtained by reacting octadecylbromide in butyl alcohol with the sodium mercaptobenzthiazole, is treated with dimethyl sulphate; the product may be used for softening cotton limbric; (2) 2-dodecylmercaptobenzthiazole, obtained by the interaction of dodecyl bromide and sodium mercaptobenzthiazole is treated with dimethylsulphate. The 2-alkylmercaptobenzthiazoles may also be prepared from the 2-mercaptobenzthiazoles by treating them with the sulphuric esters of higher alcohols. The following 2 - alkylmercaptobenzthiazoles are mentioned: 2-octadecyl, 2-dodecyl and 2-octadecenyl mercaptobenzthiazoles containing methyl or methoxy in the 6-position, or methyl in the 4-position.ALSO:Products stated to have emulsifying properties are obtained by reacting lower (up to C4) alkyl esters of inorganic acids with a mercaptobenzthiazole which has an alkyl group containing at least eight carbon atoms in the 2-position and may carry substitutent such as methyl, methoxy or ethoxy in the benzene nucleus. In examples 2-octadecylmercaptoand 2 - dodecylmercapto - benzthiazoles are treated with dimethylsulphate. The following 2-alkylmercapto benzthiazoles are mentioned: 2-octadecyl-, 2-dodecyl- and 2-octadecenyl-benzthiazoles containing methyl or methoxy in the 6-position or methyl in the 4-position.