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1. 发明专利

GB610139A Preparation of aromatic polyesters for melt-spinning 未知
公开(公告)号：GB610139A
公开(公告)日：1948-10-12
申请号：GB964246
申请日：1946-03-28
申请人： JAMES TENNANT DICKSON , ROYDEN LEWIS HEATH , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： D01D5/08
摘要： A molten fibre-forming aromatic polyester, obtained by heating a glycol with terephthalic acid or an ester-forming derivative thereof, is extruded or otherwise formed into a ribbon which is rapidly cooled and solidified and then cut into small pieces, chips, or flakes, suitable for feeding into a melt-spinning apparatus for the production of artificial filaments. The glycol used in making the polymer has the formula HO(CH2)nOH, where n is an integer greater than 1 but not exceeding 10. Instead of terephthalic acid there may be used an aliphatic, cycloaliphatic, or aryl ester, or an acid halide, ammonium, or amine salt of terephthalic acid. Rapid cooling of the ribbon may be effected by quenching with water or an aqueous liquid or by using a blast of cold or cooled air or other gas, or by directing the molten ribbon on to an intensely cooled surface such as a rotating and internally cooled metal cylinder or wheel or a moving metal band. In an example, polyethylene terephthalate is prepared in an autoclave provided with a valve and orifice from which the molten polymer is extruded as a thin ribbon. The ribbon impinges on a brass wheel and is quenched by jets of cold water. It is dried in warm air and then fed to a cutting machine. In another example, the molten polymer is forced between rotating nip-wheels set 1/16 inch apart and cooled internally. The ribbon thus formed is passed to a cutting machine. Specification 533,306 is referred to.

2. 发明专利

GB610137A Process for incorporating pigments or delustrants with highly polymeric linear esters 未知
公开(公告)号：GB610137A
公开(公告)日：1948-10-12
申请号：GB964046
申请日：1946-03-28
申请人： JAMES TENNANT DICKSON , ROYDEN LEWIS HEATH , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： C08G85/00 , C08L67/02
摘要： A finely-divided, inert, inorganic or organic substance or mixture of substances is incorporated with highly polymeric linear esters obtainable by heating glycols of the series HO(CH2)nOH, where n is greater than 1 and not greater than 10, with terephthalic acid or an ester-forming derivative of the acid by adding the substance or mixture of substances in the form of a dispersion in a glycol of the series HO(CH2)nOH, where n is an integer greater than 1 but not exceeding 10, preferably the glycol used in the polyester formation, to the mixture of polyester-forming reactants or to a low molecular weight product thereof and continuing the reaction to yield a highly polymerized product. The substances added may be titanium dioxide, zinc sulphide, barium titanate, barium sulphate, calcium sulphate extended with titanium dioxide, zinc titanate, magnesium titanate, calcium titanate, lithopone, zirconium dioxide, calcium sulphate, aluminium oxide, thorium oxide, talc, mica, kaolin, carbon black, phthalocyanine pigments, lead chromates, iron oxides, chromium oxides and ultramarine, and the particle size is not larger than 25 microns and preferably less than 5 microns. The substances are added in the form of a suspension formed by ball milling the inert filler in the glycol. Ten parts titanium dioxide are ball milled for three days with 115 parts of ethylene glycol, thus obtaining a dispersion of particle size 0.3-1.3 microns. The dispersion is mixed with dimethyl terephthalate, ethylene glycol and magnesium oxide in a closed flask heated to 197 DEG C. while circulating nitrogen therethrough and taking of methanol. The temperature is increased to 277 DEG C. under pressure of 0.3 mm. glycol, being distilled off and a melt obtained which can be extruded into fibres.

3. 发明专利

GB605106A New laminated safety glass 未知
公开(公告)号：GB605106A
公开(公告)日：1948-07-15
申请号：GB3389245
申请日：1945-12-14
申请人： REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： B32B17/10 , C08G63/199
摘要： As interlayers in compound glass there are used the films consisting of highly polymeric esters of ethylene glycol and cyclohexane-1 : 4-dicarboxylic acid, which may contain up to 25 per cent of esters of other glycols, e.g. propylene, diethylene, trimethylene, or p-xylylene glycol, with other acids, e.g. adipic or terephthalic acid. Films may be prepared separately or in situ by drying on the glass solutions of the esters, e.g. in ethyl acetate, chloroform, acetone, methyl ethyl ketone, or mixtures thereof. Specification 461,236 is referred to.

4. 发明专利

GB596704A Production of coloured masses and articles from organic filament-forming materials 未知
公开(公告)号：GB596704A
公开(公告)日：1948-01-08
申请号：GB2835247
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： The process of Specification 569,170 is applied to polythene instead of to nylon. In an example, a copper phthalocyanine pigment is dispersed in the low-molecular polyester-amide described in example (1) of the above Specification and the dispersion is milled with polythene at the melting temperature.

5. 发明专利

GB503168A Dyeing of cellulosic material 未知
公开(公告)号：GB503168A
公开(公告)日：1939-03-30
申请号：GB1947838
申请日：1937-06-30
申请人： JOHN GWYNANT EVANS , HENRY ALFRED PIGGOTT , REGINALD JOHN WILLIAM REYNOLDS , JOHN DONALD ROSE , ERIC EVERARD WALKER , ICI LTD
IPC分类号： D06P1/66

6. 发明专利

GB497485A Manufacture of substituted acid amides 未知
公开(公告)号：GB497485A
公开(公告)日：1938-12-19
申请号：GB1691537
申请日：1937-06-17
申请人： REGINALD JOHN WILLIAM REYNOLDS , ERIC EVERARD WALKER , ICI LTD
IPC分类号： C07D213/89
摘要： Amides containing a tertiary amino or a quaternary ammonium group are obtained by the action of a heterocyclic secondary amine, or an aliphatic or heterocyclic tertiary amine which is unsubstituted or substituted only by hydrocarbon radicles, on an amide of either of the formulae XRCONHR1 or XR11(CONHR1)2, where X is chlorine or bromine, R is an alkylene group of not more than seven carbon atoms, R1 is hydrogen or hydroxymethyl, and R11 is a trivalent saturated aliphatic hydrocarbon radicle. Specified amides which may be treated are chloracetamide, chloromalonamide, b -bromopropionamide and N-hydroxymethyl-chloracetamide. Specified amines which may be used are piperidine, morpholine, triethylamine, trimethylamine, N-methylpiperidine, N-cetylpiperidine, N-benzylpiperidine, pyridine, a -picoline and quinoline. Examples are given in which (1) piperidine and chloracetamide yield piperidylacetamide, (2) pyridine and chloromalonamide yield di(carbamyl)methylpyridinium chloride, (3) pyridine and N-hydroxymethylchloracetamide yield (N-hydroxymethylcarbamyl)methylpyridinium chloride, (4) pyridine and b -bromopropionamide yield b -carbamylethylpyridinium bromide, (5) pyridine and chloracetamide yield carbamyl-methylpyridinium chloride, (6) benzylpiperidine and chloracetamide yield carbamylmethylbenzylpiperidinium chloride, (7) triethylamine and chloracetamide yield carbamylmethyltriethylammonium chloride. The products are useful in the treatment of textiles. b -Bromopropionamide is obtainable from ammonia and b -bromopropionyl chloride, which may be prepared from b -bromopropionic acid and thionyl chloride.

7. 发明专利

GB469476A Improvements in the treatment of cellulosic material 未知
公开(公告)号：GB469476A
公开(公告)日：1937-07-26
申请号：GB3577935
申请日：1935-12-24
申请人： ALFRED WILLIAM BALDWIN , REGINALD JOHN WILLIAM REYNOLDS , ERIC EVERARD WALKER , CLARENCE SYDNEY WOOLVIN , ICI LTD
IPC分类号： D06M13/322
摘要： 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.

8. 发明专利

GB614993A Treatment of polymeric materials 未知
公开(公告)号：GB614993A
公开(公告)日：1948-12-30
申请号：GB2307246
申请日：1946-08-02
申请人： DAVID AUGUSTINE HARPER , BERNARD JAMES HABGOOD , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： C08G18/60 , C08G18/84
摘要： In a process for improving the properties of modified polyesters or polyesteramides as set forth in the parent Specification, an aromatic tri-isocyanate-modified polyesteramide is used in place of the organic di-isocyanate-modified polyesteramide. Suitable aromatic tri-isocyanates are benzene - 1,3,5 - tri - isocyanate, toluene - 2,4,6 - tri - isocyanate, ethylbenzene - 2,4,6-tri-isocyanate, monochlorobenzene-2,4,6-tri-isocyanate, triphenylmethane-4,41,411-tri-isocyanate and diphenyl-2,4,41-tri-isocyanate. In the example, a polyesteramide is prepared from ethylene glycol, adipic acid and monoethanolamine and modified with benzene-1,3,5-tri-isocyanate and with toluene-2,4,6-tri-isocyanate. Mixes containing dark substitute, carbon black, stearic acid and one of the tri-isocyanate-modified polyesteramides are then made and their curing properties tested without added curing agent and after addition of paraformaldehyde and phthalic anhydride. Specification 553,733 also is referred to.

9. 发明专利

GB610140A Melt blending of aromatic polyesters with other polymeric materials 未知
公开(公告)号：GB610140A
公开(公告)日：1948-10-12
申请号：GB964746
申请日：1946-03-28
申请人： JAMES TENNANT DICKSON , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： C08L67/02
摘要： Blends of aromatic polyesters of the kind obtainable by heating glycols of the series HO-(CH2)n-OH, where n is an integer greater than 1 but not exceeding 10, with terephthalic acid, with other synthetic linear condensate polymers are obtained by heating them together at a temperature above their melting points at least until a homogeneous blend is obtained. The synthetic linear condensation polymers may be polyamides and interpolyamides such as polyhexamethylene adipamide, polyhexamethylene sebacamide, the polyamides from caprolactam, interpolyamides from caprolactam and hexamethylene diammonium adipate, interpolyamides from hexamethylene diammonium adipate, hexamethylene diammonium sebacate and caprolactam; polyesters and interpolyesters such as polytrimethylene terephthalate, polydiethylene glycol terephthalate, polyethylene-1 : 2-ethane bis - (phenoxy - p - carboxylate), polyethylene adipate, polyethylene sebacate and polyethylene hexahydroterephthalate, polyurethanes and polyureas. The heated melt may be stirred, the heating may be effected under reduced pressures, a stream of oxygen-free gas, e.g. nitrogen, may be passed through the melt, or the blending may be preceded by a drying operation. In the examples, blends are made from polyethylene terephthalate and (1) polyhexamethylene adipamide; (2) the interpolyamide formed from hexamethylene diammonium adipate, hexamethylene diammonium sebacate and caprolactam; (3) polyethylene adipate; (4) the polyurethane obtainable from tetramethylene glycol and hexamethylene diisocyanate; (5) polyethylene-1 : 2-ethane bis-(phenoxy-p-carboxylate); and (6) polyethylene hexahydroterephthalate.

10. 发明专利

GB597326A Treatment of polymeric materials 未知
公开(公告)号：GB597326A
公开(公告)日：1948-01-23
申请号：GB1529741
申请日：1941-11-27
申请人： DAVID AUGUSTINE HARPER , REGINALD JOHN WILLIAM REYNOLDS , ICI LTD
IPC分类号： C08G69/50
摘要： The properties of synthetic linear polyamides are modified by mixing the polyamide with a formaldehyde-liberating substance, not in preponderating amount, and then heating said mixture whilst or after forming it into shaped articles. It is preferred to include in the mixture an acid, an acid anhydride or an acid-reacting salt, or there may be included a material which is neutral and remains so during mixing, but which develops acidity on heating. Specified formaldehyde-liberating substances are paraformaldehyde, trioxane, dimethylolurea, trimethylolmelamine, hexamethylolmelamine, diphenylolpropane tetraalcohol, 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 -hydroxy-ethyl) formal and hexamethylenetetramine-zinc chloride complexes. Specified acid substances which may be added, are formic, glycollic, oxalic, succinic, maleic, stearic, adipic, tartaric, salicylic, anthranilic, phthalic, citric, tannic, boric and phosphoric acids, phthalic and maleic anhydrides, phthalimide, and ammonium, potassium and sodium dihydrogen phosphate. Specified neutral materials developing acidity on heating are butadiene sulphone, 2 : 3-dimethylbutadiene sulphone, butadiene tetrabromide, 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 -dibromopropionate, b -chloroethyl a : b -dibromoisobutyrate, ethyl a -bromopropionate, phenyl trichloroacetate, a : a : b -trichloropropionitrile trichloroacetamide, trichloroacetyldiethylamide, N - trichloroacetylanilide, N : N1-di-(trichloroacetyl)methylene-diamine, N : N1 - di - (trichloroacetyl)ethylenediamine, interpolymers of asymmetrical dichloroethylene and vinyl chloride, and chloranil. Plasticizers, anti-oxidants, pigments and fillers may be added to the mix. According to examples: (1) an interpolyamide from o -aminocaproic acid and hexamethylenediammonium sebacate is milled with paraformaldehyde and phthalic anhydride at 60-70 DEG C., and the compounded material is heated in a mould, under pressure, at 141 DEG C. for 25 minutes; (2) the paraformaldehyde in (1) is replaced by dimethylolurea dimethylol ether; (3) a film is cast from a solution of an interpolyamide from hexamethylenediammonium adipate and caprolactam, dimethylolurea dimethyl ether and phthalic anhydride in aqueous ethanol, and the film is then heated at 110 DEG C. for 25 minutes; (4) an interpolyamide from hexamethylenediammonium adipate, hexamethylenediammonium sebacate and caprolactam is plasticized with butylphthalyl butyl glycollate and diphenylol octadecane, and then milled with dimethylolurea dimethyl ether and phthalic anhydride at 50-60 DEG C. The compounded material is heated in a mould, under pressure, at 141 DEG C. for 15 minutes; (5) the interpolyamide of (4) is dissolved, with dimethylolurea dimethyl ether, in aqueous ethanol, and a film, cast from the solution, is heated at 150 DEG C. for 25 minutes; (6) an interpolyamide from 12-amino-stearic acid and o -aminocaproic acid is milled with phthalic anhydride and paraformaldehyde at 70-80 DEG C., and the compounded material is heated in a mould, under pressure, at 141 DEG C. for 30 minutes; (7) a polyamide from 12-amino-stearic acid is milled with paraformaldehyde and phthalic acid, and the compounded material is heated in a mould, under pressure, at 141 DEG C. for 30 minutes; (8) an interpolyamide from hexamethylenediammonium sebacate and 12-amino stearic acid is treated as in (7); (9) a polyester-amide from hexamethylene diammonium adipate, ethylene glycol and adipic acid is compounded with carbon black, paraformaldehyde and phthalic anhydride at 60-80 DEG C., and the compounded material is heated in a mould, under pressure, at 141 DEG C.; (10) an interpolyamide from hexamethylenediammonium sebacate and N : N1-dimethyl-hexamethylene diammonium sebacate is milled, at 70-90 DEG C., with paraformaldehyde and 1-bromo-2-naphthol. The compounded material is heated in a mould, under pressure, at 125 DEG C. for 45 minutes. Specifications 461,237, 534,698, 540,135, 540,576, 557,544 and 580,524 are referred to.

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