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41. 发明专利

DE1942585A1 未知
公开(公告)号：DE1942585A1
公开(公告)日：1970-03-26
申请号：DE1942585
申请日：1969-08-21
申请人： AJINOMOTO KK , NISSIN SPINNING CO LTD
发明人： IWATSUKI MAKOTO , TAKAGI YASUO , MORI SHIGEO , ITO KIYOSHI , TAKENISHI SOICHIRO
IPC分类号： D01F6/68 , D01F7/00

42. 发明专利

DE1495312A1 未知
公开(公告)号：DE1495312A1
公开(公告)日：1969-03-06
申请号：DE1495312
申请日：1963-07-25
申请人： COURTAULDS LTD
发明人： ARTHUR RANDALL ALAN
IPC分类号： A61K38/00 , A61L17/08 , A61L17/10 , C07K1/02 , C07K14/00 , C08G69/10 , D01F6/68 , A61L17/00
摘要： A process for making a synthetic polypeptide filament or film comprises forming a mixture of the N-carboanhydride derivatives of an lambda-imino acid and an lambda-amino acid in an inert solvent for the polypeptide, initiating the reaction of the derivatives to form the synthetic polypeptide with evolution of carbon dioxide and extruding the polypeptide dissolved in the solvent to form a filament or a film by contact with a coagulant or by evaporation of the solvent. The example describes the reaction of lambda-proline N-carboxy anhydride with g -methyl lambda-glutamate N-carboxy anhydride in the presence of ethyl acetate and methylene chloride, tri-n-butylamine being used as initiator.

43. 发明专利

AT262517B 未知
公开(公告)号：AT262517B
公开(公告)日：1968-06-10
申请号：AT678963
申请日：1963-08-23
申请人： COURTAULDS LTD
IPC分类号： A61K38/00 , A61L17/08 , A61L17/10 , C07K1/02 , C07K14/00 , C08G69/10 , D01F6/68
摘要： A process for making a synthetic polypeptide filament or film comprises forming a mixture of the N-carboanhydride derivatives of an lambda-imino acid and an lambda-amino acid in an inert solvent for the polypeptide, initiating the reaction of the derivatives to form the synthetic polypeptide with evolution of carbon dioxide and extruding the polypeptide dissolved in the solvent to form a filament or a film by contact with a coagulant or by evaporation of the solvent. The example describes the reaction of lambda-proline N-carboxy anhydride with g -methyl lambda-glutamate N-carboxy anhydride in the presence of ethyl acetate and methylene chloride, tri-n-butylamine being used as initiator.

44. 发明专利

GB1095211A Improvements in the treatment of polygamma methyl glutamate and polygamma ethyl glutamate fabrics 未知
公开(公告)号：GB1095211A
公开(公告)日：1967-12-13
申请号：GB4099763
申请日：1963-10-17
申请人： COURTAULDS LTD
发明人： WILLIAMS ROBERT JOHN
IPC分类号： D01F6/68 , D06M13/152
摘要： The handle, crush resistance and liveliness of fabrics containing fibres composed of at least 90% by weight of an optically active form of poly-gamma-methyl glutamate or poly-gamma-ethyl glutamate are improved by treating the fabric while it is free from creases and free from tension with an aqueous solution of benzyl alcohol or an aqueous suspension of benzyl alcohol part of which is dissolved in the water present for a period of time sufficient to cause the fibres to swell and then removing the benzyl alcohol from the fabric. When using a suspension of the benzyl alcohol a dispersing agent is generally added. The aqueous composition may contain 5-20% by weight of benzyl alcohol and the treatment may be effected at temperatures over 50 DEG C.

45. 发明专利

FR81497E 未知
公开(公告)号：FR81497E
公开(公告)日：1963-09-27
申请号：FR1228448D
申请日：1962-04-19
申请人： COURTAULDS LTD
IPC分类号： C08G69/10 , D01F6/60 , D01F6/68 , D01F6/76
摘要： Films of an optically-active form of polygamma methyl glutamate and poly-gamma ethyl glutamate are made by polymerizing an optically active gamma-methyl or gammaethyl glutamate N-carboxy anhydride in an organic liquid medium which is a solvent for the polypeptide formed, the polypeptide being composed of at least 90% by weight of units of the optically active glutamate ester, extruding a solution of the polypeptide while it is still in the solvated state through a slit into a setting medium so that the polypeptide is in the alphaconfiguration on extrusion, and stretching the resultant film while it is still in the alpha-configuration thereby converting the polypeptide substantially into the beta-configuration and substantially orienting the film in the direction of stretching, which is preferably longitudinal, but may also be transverse. Films may be p made by wet- or dry-spinning, or by casting, and the polymer solution is preferably made by polymerizing the glutamate in the solvent to be used for the film-forming step. Preferred solvents are methylene chloride, and mixtures thereof with dioxane or ethyl acetate, but any of the solvents described in the parent Specification may be used. Thus the polypeptide may be extruded into a coagulating bath which is a non-solvent for the polymer but a solvent for the polymer solvent, e.g. acetone containing 5% water, or into a gas which is preferably heated, or cast on to a moving surface, using a doctor blade to adjust the thickness of the film, or cast on a liquid surface, the liquid preferably being a coagulant. Films made by wet spinning may be stretched in the wet state, or first dried and then stretched. Films made by dry spinning or casting may be stretched in air or over rollers while still containing some solvent, or after drying has been completed, or may be stretched in steam. In examples (1) a solution of poly-gamma methyl-2-glutamate in a methylene chloride/dioxane mixture is extruded into a coagulant bath consisting of acetone containing about 5% of water, passed through a water bath to remove acetone and while still wet passed over a series of rollers to give a 90% stretch. (2) The solution of Example 1 is cast on glass as a film and allowed to dry, then passed through a bath of acetone and stretched over rollers and dried as in the previous example. The films so made are insoluble in the spinning solvent. Specification 917,956 also is referred to.

46. 发明专利

GB935396A Improvements in and relating to the production of poly-gamma-methyl glutamate and poly-gamma-ethyl glutamate films 未知
公开(公告)号：GB935396A
公开(公告)日：1963-08-28
申请号：GB1563761
申请日：1961-05-01
申请人： COURTAULDS LTD
发明人： BALLARD DENIS GEORGE HAROLD
IPC分类号： C08G69/10 , D01F6/60 , D01F6/68 , D01F6/76
摘要： Films of an optically-active form of polygamma methyl glutamate and poly-gamma ethyl glutamate are made by polymerizing an optically active gamma-methyl or gammaethyl glutamate N-carboxy anhydride in an organic liquid medium which is a solvent for the polypeptide formed, the polypeptide being composed of at least 90% by weight of units of the optically active glutamate ester, extruding a solution of the polypeptide while it is still in the solvated state through a slit into a setting medium so that the polypeptide is in the alphaconfiguration on extrusion, and stretching the resultant film while it is still in the alpha-configuration thereby converting the polypeptide substantially into the beta-configuration and substantially orienting the film in the direction of stretching, which is preferably longitudinal, but may also be transverse. Films may be p made by wet- or dry-spinning, or by casting, and the polymer solution is preferably made by polymerizing the glutamate in the solvent to be used for the film-forming step. Preferred solvents are methylene chloride, and mixtures thereof with dioxane or ethyl acetate, but any of the solvents described in the parent Specification may be used. Thus the polypeptide may be extruded into a coagulating bath which is a non-solvent for the polymer but a solvent for the polymer solvent, e.g. acetone containing 5% water, or into a gas which is preferably heated, or cast on to a moving surface, using a doctor blade to adjust the thickness of the film, or cast on a liquid surface, the liquid preferably being a coagulant. Films made by wet spinning may be stretched in the wet state, or first dried and then stretched. Films made by dry spinning or casting may be stretched in air or over rollers while still containing some solvent, or after drying has been completed, or may be stretched in steam. In examples (1) a solution of poly-gamma methyl-2-glutamate in a methylene chloride/dioxane mixture is extruded into a coagulant bath consisting of acetone containing about 5% of water, passed through a water bath to remove acetone and while still wet passed over a series of rollers to give a 90% stretch. (2) The solution of Example 1 is cast on glass as a film and allowed to dry, then passed through a bath of acetone and stretched over rollers and dried as in the previous example. The films so made are insoluble in the spinning solvent. Specification 917,956 also is referred to.

47. 发明专利

FR1321856A 未知
公开(公告)号：FR1321856A
公开(公告)日：1963-03-22
申请号：FR896954
申请日：1962-05-09
申请人： COURTAULDS LTD
IPC分类号： D01F6/68

48. 发明专利

FR1228448A 未知
公开(公告)号：FR1228448A
公开(公告)日：1960-08-29
申请号：FR791765
申请日：1959-04-10
申请人： COURTAULDS LTD
IPC分类号： C08G69/10 , D01F6/60 , D01F6/68 , D01F6/76
摘要： Films of an optically-active form of polygamma methyl glutamate and poly-gamma ethyl glutamate are made by polymerizing an optically active gamma-methyl or gammaethyl glutamate N-carboxy anhydride in an organic liquid medium which is a solvent for the polypeptide formed, the polypeptide being composed of at least 90% by weight of units of the optically active glutamate ester, extruding a solution of the polypeptide while it is still in the solvated state through a slit into a setting medium so that the polypeptide is in the alphaconfiguration on extrusion, and stretching the resultant film while it is still in the alpha-configuration thereby converting the polypeptide substantially into the beta-configuration and substantially orienting the film in the direction of stretching, which is preferably longitudinal, but may also be transverse. Films may be p made by wet- or dry-spinning, or by casting, and the polymer solution is preferably made by polymerizing the glutamate in the solvent to be used for the film-forming step. Preferred solvents are methylene chloride, and mixtures thereof with dioxane or ethyl acetate, but any of the solvents described in the parent Specification may be used. Thus the polypeptide may be extruded into a coagulating bath which is a non-solvent for the polymer but a solvent for the polymer solvent, e.g. acetone containing 5% water, or into a gas which is preferably heated, or cast on to a moving surface, using a doctor blade to adjust the thickness of the film, or cast on a liquid surface, the liquid preferably being a coagulant. Films made by wet spinning may be stretched in the wet state, or first dried and then stretched. Films made by dry spinning or casting may be stretched in air or over rollers while still containing some solvent, or after drying has been completed, or may be stretched in steam. In examples (1) a solution of poly-gamma methyl-2-glutamate in a methylene chloride/dioxane mixture is extruded into a coagulant bath consisting of acetone containing about 5% of water, passed through a water bath to remove acetone and while still wet passed over a series of rollers to give a 90% stretch. (2) The solution of Example 1 is cast on glass as a film and allowed to dry, then passed through a bath of acetone and stretched over rollers and dried as in the previous example. The films so made are insoluble in the spinning solvent. Specification 917,956 also is referred to.

49. 发明专利

DE900125C 未知
公开(公告)号：DE900125C
公开(公告)日：1953-12-21
申请号：DEC0001038
申请日：1950-05-20
申请人： COURTAULDS LTD
发明人： BAMFORD CLEMENT HENRY , HANBY WILLIAM EDWARD
IPC分类号： C07K1/02 , D01F6/60 , D01F6/68 , D01F6/76
摘要： A solution of a synthetic polypeptide, obtained by the process of Specification 675,298, in a solvent consisting of or comprising a lower aliphatic carboxylic acid (1-5 carbon atoms), a halogen-substituted lower aliphatic carboxylic acid, or a monohydric phenol, is extruded into a setting medium to form artificial fibres. The polypeptides used are derived from anhydrocarboxy amino acids. The solvent may be phenol, meta-cresol, formic acid, or di- or tri-chloracetic acid. A mixture of 3 parts by weight of trichloracetic acid and 1 part of dichloracetic acid may be used. Diluents such as water, benzene, and chloroform may be present. The solutions may be dry or wet spun. For wet-spinning the preferred coagulants are water, methyl or ethyl alcohol or aqueous solutions of these alcohols, or diethyl ether or petroleum ether. In an example, anhydrocarboxy - d,l - b - phenylalanine and the gamma-methyl ester of anhydrocarboxy-l-glutamic acid are dissolved in nitrobenzene containing N - (aminoacetyl)-dimethylamine as polymerization initiator. After standing for 15 days at 50 DEG C., the resultant gel is washed with petroleum ether to remove the nitrobenzene and is then dried. The synthetic polypeptide obtained is dissolved in m-cresol to form a 15 per cent solution. The solution is extruded into ethyl alcohol to form fibres. In another example anhydrocarboxy-d,l-b -phenylalanine is polymerized while dissolved in nitrobenzene containing N-(a -amino-b - phenyl - propionyl) - dimethylamine. A solution of the synthetic polypeptide in m-cresol is extruded at 70 DEG C. into ethyl alcohol to form fibres. In another example, anhydrocarboxy - d,l - b - phenylalanine and anhydrocarboxy-a -aminoisobutyric acid are copolymerized and the synthetic polypeptide obtained is dissolved in a mixture of trichloracetic acid and water. The solution is extruded into water, ethyl alcohol, or aqueous alcohol. In other examples, solutions of the copolymer of d,l-b -phenyl-alanine and glycine, of the copolymer of d,l-valine and a -amino-isobutyric acid, and of a polymer of d,l-valine, in m-cresol, formic acid, and dichloracetic acid are extruded into ethyl alcohol and ether mixture, and water. The second Provisional Specification refers also to the use of cupriethylene diamine as a solvent for the synthetic polypeptide.

50. 发明专利

FR1037034A 未知
公开(公告)号：FR1037034A
公开(公告)日：1953-09-14
申请号：FR1037034D
申请日：1951-05-11
申请人： COURTAULDS LTD
IPC分类号： D01F6/60 , D01F6/68 , D01F6/76
摘要： Fibres are produced from synthetic polypeptides, of the kind described in Specification 675,298, by extruding through a jet into a setting medium a solution of the polypeptide in benzene, methylene chloride, meta-cresol, dichloracetic acid or trichloracetic acid, whereby the fibres so formed have an a molecular configuration, and then treating the fibres in a bath comprising an aliphatic mono-carboxylic acid containing from one to six carbon atoms per molecule or a like acid containing, on the a carbon atom, a bromine atom or a phenyl or mercaptan group, so that at least part of the fibres is converted into the b -molecular configuration. The synthetic polypeptides are made by polymerizing anhydro-carboxyamino-acids of the formula R1, R2 and R3 being hydrogen or alkyl, aryl or aralkyl groups, which may be substituted or unsubstituted. Formic, acetic, propionic, normal or iso-butyric acid, normal or iso-caproic acid or crotonic acid; a -bromo acetic, propionic, butyric or n-valeric acid; phenylacetic acid or thioglycollic acid, may be used for treating the synthetic polypeptide fibres. If desired, the extruded fibres may be stretched, e.g. in steam, before the acid treatment. The polypeptide solutions may be dry or wet spun. Specified coagulants are water, methyl alcohol, ethyl alcohol and aqueous alcohols. The treatment may be carried out at room temperature for a period of 1-3 minutes. In an example, a copolymer of dl-b -phenylalanine and dl-leucine is dissolved in trichloracetic acid containing 10 per cent of water and the solution is extruded into water. The fibres so formed are passed through a bath of formic acid and then dried. The fibres obtained have a b -configuration and are insoluble in benzene or carbon tetrachloride. Other examples describe the production and treatment of fibres of copolymers of dl-b -phenylalanine with g -methyl-l-glutamate or with dl-leucine and g -benzyl-dl-glutamate. Specification 675,299 also is referred to.

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