公开(公告)号：CA833442A

公开(公告)日：1970-02-03

申请号：CA833442D

Applicant: BASF AG

Inventor： PETERSEN HARRO ,  RUETTIGER WILHELM ,  BILLE HEINZ

公开(公告)号：GB1126259A

公开(公告)日：1968-09-05

申请号：GB4930766

申请日：1966-11-03

Applicant: BASF AG

Inventor： FIKENTSCHER ROLF ,  BRANDEIS HANS ,  BILLE HEINZ

IPC: C07F9/44 ,  C07F9/6584 ,  D06M13/288 ,  D06M13/487

Abstract: 1,126,259. Halomethylphosphonic acid bisamides. BADISCHE ANILIN- & SODAFABRIK A.G. 3 Nov., 1966 [4 Nov., 1965], No. 49307/66. Heading C2C. [Also in Division D1] Novel compounds of the formula in which X is Cl or Br and R 1 and R 2 are the same or different and denote hydrogen atoms, unsubstituted C 1 -C 3 alkyl radicals or C 1 -C 3 chloro- or bromo-alkyl radicals or together denote a C 2 or C 3 alkylene radical are obtained by reacting a halomethyl phosphonic acid dichloride with ammonia or with appropriate primary mono-amines or diamines in an inert solvent, e.g. methylene chloride, benzene, dioxane, tetrahydrofuran or ether, in the presence of an excess of ammonia or of the said amines which is sufficient to bind the hydrogen chloride formed in the reaction or in the presence of other acid-binding agents, e.g. tertiary amines. The products are useful for flame-proofing cellulosic fibrous materials.

公开(公告)号：GB1093807A

公开(公告)日：1967-12-06

申请号：GB3491766

申请日：1966-08-04

Applicant: BASF AG

Inventor： PETERSEN HARRO ,  BILLE HEINZ ,  RUEMENS WILHELM

IPC: C07D239/10 ,  D06M15/423

Abstract: Novel compounds of the formula wherein R1 and R2 are H or C1- 5 alkyl and R3 and R4 are C1- 5 alkyl are prepared by reacting 2,2-dialkyl-1,3-propylene diamines with urea, phosgene or carbonic acid esters to form 5,5-dialkylhexahydropyrimidones - 2, adding on formaldehyde in the presence of alkaline reagents, and, if desired, etherifying the resultant N,N1-dihydroxymethyl derivatives with alcohols in the presence of an acid catalyst.ALSO:A finishing agent for textile materials consisting of or containing natural or regenerated cellulose comprises a solution of a compound of the formula: where R1 and R2 are H or C1-5 alkyl and R3 and R4 are C1-5 alkyl. The finishing agent is preferably used in aqueous solution together with an acid catalyst, and may be reacted with the textile material to form acetal bonds when wet or wholly or partly dried, either immediately or after storage in the impregnated but unreacted condition. The finishing agents may be used together with known finishing agents, e.g. dispersions of polymers such as a copolymer of n-butylacrylate, polyethylene, an ethylene oxide adduct, bleach, oxalic acid, NH4Cl and/or MgCl2. The finishing treatment preferably takes place at 130 to 160 DEG C, and the acidic catalyst may be a compound which decomposes to become acidic at these temperatures.

公开(公告)号：FR1491635A

公开(公告)日：1967-08-11

申请号：FR73279

申请日：1966-08-17

Applicant: BASF AG

Inventor： PETERSEN HARRO ,  BILLE HEINZ ,  RUEMENS WILHELM

IPC: C07D239/10 ,  D06M15/423

公开(公告)号：GB1066618A

公开(公告)日：1967-04-26

申请号：GB3766165

申请日：1965-09-03

Applicant: BASF AG

Inventor： BILLE HEINZ ,  OLSEN BJOERN

IPC: A41D27/06 ,  B32B27/00 ,  D06M15/59

Abstract: Heat sealable stiffening materials comprising a backing cloth and a layer of a polymide bonded therewith as a stiffening agent, is prepared by moistening the backing cloth with water and/or an organic solvent, dusted with a powder of a synthetic linear thermoplastic polyamide at the rate of from 20 to 80 grams per square metre of the backing cloth and then calendering. Examples of polyamides are polycondensates of lactams or of diamines and dicarboxylic acids, for example, caprolactam, piperidone - 2, pyrrolidone - 2, hexamethylene-diamine, 4, 4\sv - diaminodicyclohexylmethane, 4, 4\sv - diamino - dicyclohexylpropane and adipic acid, particularly those of softening point from 120 DEG to 200 DEG C. Copolymers exemplified are 1 part by weight of caprolactam and 2 to 11 parts of an equimolar mixture of (a) about equal parts by weight of hexamethylene-diamine and 4, 4\sv - diaminodicyclohexylmethane and (b) adipic acid and copolymers obtained from 40% by weight of capryllactam, 25% of octamethylene diammonium adipate and 35% of hexamethylene diammonium adipate. The polyamide may be obtained by grinding, reprecipitation or water digestion and should have a grain size as uniform as possible between 10 and 250 microns. The backing cloth may be of cotton, staple fibre or linen and it may have a shrinkproof finish and an area weight of from 120-250 grams per square metre. Water, methanol, ethanol, isopropanol or mixtures thereof may be used to moisten the backing cloth, as well as organic solvents such as methylene chloride. The powder may be applied by means of a vibrating screen. Calendering which may be carried out at 20 DEG C - 110 DEG C may be effected immediately after drying or after storing at room or elevated temperature.

公开(公告)号：FR1338749A

公开(公告)日：1963-09-27

申请号：FR914650

申请日：1962-11-07

Applicant: BASF AG

Inventor： NIESWANDT WERNER ,  PFAFF PETER ,  STUEBER GEORG ,  BILLE HEINZ

公开(公告)号：GB1141515A

公开(公告)日：1969-01-29

申请号：GB5287166

申请日：1966-11-25

Applicant: BASF AG

Inventor： BILLE HEINZ ,  RUETTIGER WILHELM

IPC: D06M15/423

Abstract: 1,141,515. Mixed aminoplast textile treating compositions. BADISCHE ANILIN- & SODAFABRIK A.G. 25 Nov., 1966 [27 Nov., 1965; 8 June, 1966], No. 52871/66. Heading C3R. [Also in Division D1] A composition suitable for use in the treatment of cellulosic fabrics comprises (a) at least one poly-N-methylol compound which condenses at a temperature less than 140‹ C., (b) at least one poly-N-methylol compound which condenses at a temperature of at least 140‹ C. and (c) at least one acid curing catalyst which forms an acid under the conditions of condensation. The poly-N-methylol compounds contain two or more hydroxymethyl or alkoxymethyl groups having 1-5 carbon atoms in the alkoxy group which are attached to nitrogen. The compounds (a) may have the formula in which each R 1 is a hydrogen atom or when taken together the two substituents R 1 denote and the substituents R 2 which may be the same or different are hydrogen atoms or alkyl groups having 1-4 carbon atoms and the compounds (b) may have the formula or in which R 3 is a hydrogen atom or alkyl group having 1-4 carbon atoms, R 4 is R 5 is a hydrogen atom, an alkyl group having 1-4 carbon atoms or a group of the formula R 3 O-CH 2 -, R 6 is an alkylene group having 2-4 carbon atoms, R 7 is methyl or ethyl and n is 0 or 1, the compounds containing at least two R 3 O-CH 2 - groups. The acid curing catalyst may be aluminium sulphate, zinc chloride, zinc nitrate, ammonium chloride, ammonium nitrate, ammonium phosphate and salts of ethanolamine, diethanolamine, 2- hydroxy - 2 - methylpropylamine with hydrochloric acid, magnesium chloride and magnesium sulphate. The compounds (a), (b) and (c) may be applied to the fabrics from an aqueous bath which may also contain wetting agents, e.g. salts of alkylnaphthalene sulphonic acids, alkali metal salts of sulphonated dioctyl succinate and adducts of alkylene oxides with fatty alcohols, alkyl phenols or fatty amines, water repelling agents, e.g. paraffin wax emulsions containing aluminium or zirconium, silicon containing formulations and perfluorinated aliphatic compounds, softeners, e.g. ethenoxylation products of high molecular weight fatty acids, fatty alcohols or fatty amides, high molecular weight polyglycol ethers and esters thereof, high molecular weight fatty acids, fatty alcohol sulphonates, stearyl-N,N-ethyleneurea and stearylamidomethyl pyridimium chloride, finishes, e.g. cellulose ethers and esters, alginates, polyamides, ether-oxylated polyamides, polyvinyl ethers, polyvinyl alcohol, polyacrylic or methacrylic acid or esters or amides thereof, polyvinyl propionate, polyvinyl pyrrolidone, copolymers of vinyl chloride and acrylic esters, butadiene and styrene or acrylonitrile, α-dichloroethylene, #-chloroalkyl acrylic esters or vinyl-#-chloroethyl ether and acrylamide or amides of crotonic or maleic acid, or N-methylolmethacrylamide and other polymerizable compounds, or polyethylene, and optical brighteners. In examples the aminoplast mixtures are: dimethylol ethyleneurea plus (1) dimethylol glyoxal monoureine or (2) dimethylol ethyl - urethane or (4) dimethylol urea and dimethylol glyoxal monoureine; or (3) dimethylol propyleneurea plus dimethylol 4-methoxy-5: 5- dimethylpropyleneurea; or (5) dimethylol glyoxal monoureine plus dimethylol 5-isobutyl hexahydro - 1: 3: 5 - triazinone - 2. These are used in aqueous solution containing MgCl 2 or Mg(SO 4 ) 2 and optionally polyethylene emulsion and/or a copolymer of butyl acrylate/butylene diacrylate / methylol methacrylamide / acrylamide and optionally ethoxylated iso-octylphenol.

公开(公告)号：FR1481604A

公开(公告)日：1967-05-19

申请号：FR63514

申请日：1966-05-31

Applicant: BASF AG

Inventor： WILHELM HANS ,  BILLE HEINZ ,  HANN ERNST WILHELM ,  DACHS KARL

IPC: C08J3/07 ,  C08L77/00 ,  D06M15/59

Abstract: A composition suitable for use in the treatment of textiles comprises an aqueous dispersion containing (a) a polyamide which is a co-condensate of 25-40% by weight of one or more lactams having 6-12 carbon atoms in the lactam ring or of equivalent omega-aminocarboxylic acids, 25-40% by weight of one or more salts of hexamethylene diamine with linear dicarboxylic acids having 6-12 carbon atoms, 25-40% by weight of one or more salts of 4,41-diamino-dicyclohexylmethane with linear dicarboxylic acids having 6-12 carbon atoms and 0-10% by weight of one or more other polyamide-forming substances and (b) a protective colloid which is a water-soluble copolymer having a K value of at least 90 and derived from 10-35% by weight of acrylic and/or methacrylic acid, 57.5-90% by weight of a mixture consisting of acrylamide and 5-40% by weight (on the whole of the monomers) of methacrylamide and 0-7.5% by weight of one or more other monomers. Suitable other polyamide-forming substances are dicarboxylic acids, omega-aminocarboxylic acids or diamines which are branched or contain a hetero atom in the chain, and C-substituted lactams. The other monomers in the protective colloid may be a -chloro-acrylic, phenylacrylic, crotonic, maleic, fumaric, itaconic, citraconic, mesaconic or vinylsulphonic acid or an anhydride, salt or ester thereof, methyl or ethyl acrylate or methacrylate, vinyl acetamide, N-dimethylacrylamide, N-methylacrylamide, N-ethylacrylamide or a vinyl lactam. Particularly preferred protective colloids contain 0.005-1% by weight of copolymerizable monomers containing N-methylol groups, e.g. derivatives of urea, melamine, dicyandiamide and guanidine containing N-methylol groups and groups with polymerizable olefinic double bonds and particularly N-methylolmethacrylamide and N-methylolacrylamide. The dispersion may contain 0.5-5% by weight of the protective colloid based on the weight of the polyamide. The dispersions may be prepared by mixing a solution of the polyamide in an organic solvent, e.g. ethanol, isopropanol, butanol or a mixture thereof, with water which contains the protective colloid and, if desired, distilling off all or part of the solvent. The dispersion may also contain polyolefines, polyacrylates, water repellents, dyes, pigments, thickening agents, organic solvents and reaction products, which may be etherified with alcohols containing up to four carbon atoms, of formaldehyde with urea, melamine, ethyleneurea, trimethyleneurea, 4,5-dihydroxy imidazolidone-(2), triazone (2) and its 5-alkyl and 5-hydroxy-alkyl derivatives having up to four carbon atoms in the alkyl or hydroxyl alkyl radical, 5-hydroxytrimethyleneurea or urones. In one example, the dispersion also includes an acrylonitrile-methyl acrylate (50/50) copolymer which has been incompletely hydrolysed with ammonia.ALSO:Fabrics e.g. of cotton, are coated with an aqueous dispersion containing (a) a polyamide which is a cocondensate of 25-40% by weight of one or more lactams having 6-12 carbon atoms in the lactam ring or of equivalent omega-aminocarboxylic acids, 25-40% by weight of one or more salts of hexamethylene diamine with linear dicarboxylic acids having 6-12 carbon atoms, 25-40% by weight of one or more salts of 4, 41-diaminodicyclohexylmethane with linear dicarboxylic acids having 6-12 carbon atoms and 0-10% by weight of one or more other polyamide-forming substances and (b) a protective colloid which is a water-soluble copolymer having a K value of at least 90 and derived from 10-35% by weight of acrylic and/or methacrylic acid, 57.5-90% by weight of a mixture consisting of acrylamide and 5-40% by weight (on the whole of the monomers) of methacrylamide and 0-7.5% by weight of one or more other monomers, and then dried and heated to at least 100 DEG C. Suitable other polyamide-forming substances are dicarboxylic acids, omega-aminocarboxylic acids or diamines which are branched or contain a hetero atom in the chain, and C-substituted lactams. The other monomers in the protective colloid may be a -chloro-acrylic, phenylacrylic, crotonic, maleic, fumaric, itaconic, citraconic, mesaconic or vinylsulphonic acid or an anhydride, salt or ester thereof, methyl or ethyl acrylate or methacrylate, vinyl acetamide, N-dimethylacrylamide, N-methyl acrylamide, N-ethyl-acrylamide or a vinyl lactam. Particularly preferred protective colloids contain 0.005-1% by weight of copolymerizable monomers containing N-methylol groups, e.g. derivatives of urea, melamine dicyandiamide and guanidine containing N-methylol groups, and groups with polymerizable olefinic double bonds and particularly N-methylolmethacrylamide and N-methylolacrylamide. The dispersion may contain 0.5-5% by weight of the protective colloid based on the weight of the polyamide. The dispersions may be prepared by mixing a solution of the polyamide in an organic solvent, e.g. ethanol, isopropanol, butanol or a mixture thereof, with water which contains the protective colloid and if desired distilling off all or part of the solvent. The dispersion may also contain polyolefines, poly-acrylates, water repellents, dyes, pigments, thickening agents, organic solvents and reaction products, which may be etherified with alcohols containing up to four carbon atoms, of formaldehyde with urea, melamine, ethyleneurea, trimethyleneurea, 4, 5-dihydroxy imidazolidone-(2), triazone (2) and its 5-alkyl and 5-hydroxyalkyl derivatives having up to four carbon atoms in the alkyl or hydroxyl alkyl radical, 5-hydroxytrimethyl-eneurea or uranes.ALSO:Textile material, e.g. cotton fabric, is finished and non-woven fabrics bonded by treating them with an aqueous dispersion containing (a) a polyamide which is a cocondencate of 25-40% by weight of one or more lactams having 6-12 carbon atoms in the lactam ring or of equivalent omega-aminocarboxylic acids, 25-40% by weight of one or more salts of hexamethylene diamine with linear dicarboxylic acids having 6-12 carbon atoms, 25-40% by weight of one or more salts of 4, 41-diaminodicyclohexylmethane with linear dicarboxylic acids having 6-12 carbon atoms and 0-10% by weight of one or more other polyamide-forming substances and (b) a protective colloid which is a water-soluble copolymer having a K value of at least 90 and derived from 10-35% by weight of acrylic and/or methacrylic acid, 57.5-90% by weight of a mixture consisting of acrylamide and 5-40% by weight (on the whole of the monomers) of methacrylamide and 0-7.5% by weight of one or more other monomers, and then drying and heating the treated material to at least 100 DEG C. Suitable other polyamide-forming substances are dicarboxylic acids, omega-aminocarboxylic acids or diamines which are branched or contain a hetero atom in the chain, and C-substituted lactams. The other monomers in the protective colloid may be a -chloro-acrylic, phenylacrylic, crotonic, maleic, fumaric, itaconic, citraconic, mesaconic or vinylsulphonic acid or an anhydride, salt or ester thereof, methyl or ethyl acrylate or methacrylate, vinyl acetamide, N-dimethylacrylamide, N-methyl acrylamide, N-ethylacrylamide or a vinyl lactam. Particularly preferred protective colloids contain 0.005-1% by weight of copolymerizable monomers containing N-methylol groups, e.g. derivatives of urea, melamine, dicyandiamide and guanidine containing N-methylol groups, and groups with polymerizable olefinic double bonds and particularly N-methylolmethacrylamide p and N-methylolacrylamide. The dispersion may contain 0.5-5% by weight of the protective colloid based on the weight of the polyamide. The dispersions may be prepared by mixing a solution of the polyamide in an organic solvent, e.g. ethanol, isopropanol, butanol or a mixture thereof, with water which contains the protective colloid and if desired distilling off all or part of the solvent. The dispersion may also contain polyolefines, poly-acrylates, water repellents, dyes, pigments, thickening agents, organic solvents and reaction products, which may be etherified with alcohols containing up to four carbon atoms, of formaldehyde with urea, melamine, ethyleneurea, trimethyleneurea, 4, 5-dihydroxy imidazolidone-(2), triazone-(2) and its 5-alkyl and 5-hydroxyalkyl derivatives having up to four carbon atoms in the alkyl or hydroxyl alkyl radical, 5-hydroxytrimethyleneurea or uronea.

公开(公告)号：FR1474278A

公开(公告)日：1967-03-24

申请号：FR54278

申请日：1966-03-21

Applicant: BASF AG

Inventor： BILLE HEINZ ,  PETERSEN HARRO ,  RUEMENS WILHELM

IPC: D06M15/423

公开(公告)号：GB1029044A

公开(公告)日：1966-05-11

申请号：GB1768964

申请日：1964-04-29

Applicant: BASF AG

Inventor： BILLE HEINZ ,  DISTLER HARRY ,  DITTUS GEORG ,  MUELLER WERNER ,  RUETTIGER WILHELM

IPC: D06M13/252 ,  D06M13/278

Abstract: The invention comprises compounds having the general formula wherein A represents a radical having one of the following formulae:- p represents one of the whole numbers 1 to 4, q represents one of the whole numbers 2 to 4, r represents one of the whole numbers 2 to 4, s represents one of the whole numbers 0, 1 or 2 and M\s3 represents an alkali metal or ammonium ion. They may be obtained by reacting a dichloride of the formula Cl-A-Cl with twice the molar amount of b -hydroxyethylmercaptan with elimination of HCl to give HO-CH2-CH2-S-A-S-CH2-CH2-OH, reacting this compound with twice the molar amount of b -chloroethanol, and esterifying the compound of the formula with H2SO4, ClSO3H or oleum and subsequently neutralizing the product with an alkali. An example is given for the preparation of the compound of the formula The products are suitable for crease-proofing textile materials containing reactive hydrogen atoms (see Division D1).ALSO:Textile materials of fibre forming substances containing reactive hydrogen atoms are finished by treating the material in any sequence with a solution of a sulphur-containing organic compound of the general formula:- wherein A represents a radical having one of the following formulae:- p represents one of the whole numbers 1 to 4, q represents one of the whole numbers 2 to 4, r represents one of the whole numbers 2 to 4, s represents one of the whole numbers 0, 1 or 2 and M\sJ represents an alkali metal or ammonium ion (see Division C2 for preparation); and with an alkaline reacting substance. Conventional crosslinking resin finishing agents and also acid or potentially acid catalysts may be used in the process-Polymer dispersions or solutions may be added to aqueous solutions of compounds of the above formula which may also contain conventional cross-linking finishing agents. Specified polymer dispersions being homopolymers and copolymers of acrylic esters or polyethylene. Specified polymer solutions are polyacrylamide solutions. Softening agents may also be added. Examples are given for the treatment of textiles with compounds of the above formula.