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    Bleaching fibrous material of natural cellulose
    6.
    发明专利
    Bleaching fibrous material of natural cellulose 未知

    公开(公告)号：GB1073807A

    公开(公告)日：1967-06-28

    申请号：GB5219965

    申请日：1965-12-09

    Applicant: BASF AG

    Inventor： KIRNER UWE ,  HARTMARK BJARNE

    IPC: D06L3/00 ,  D06L4/00 ,  D06L4/30 ,  D06L4/70

    Abstract: Natural cellulosic fibrous materials, e.g. cotton fabrics, are bleached in the absence of oxidising agents by treating them at 90 DEG -150 DEG C. for from 30 seconds to 5 hours with an aqueous liquor containing (1) 4-13% by weight of an alkali metal hydroxide (2) 1-4% by weight of an alkali metal polyphosphate containing two or more phosphorus atoms in the molecule and/or a complex-forming aminopolycarboxylic acid or alkali metal salt thereof and (3) 0.5-3% by weight of an anion-active and/or nonionic wetting agent which is active in alkaline solution, the treatment temperature t (in DEG C) within the range of 90 DEG -150 DEG C. being so correlated to the treatment period #t (in minutes) that it is within the limits t1 and tu (inclusive) (t1 denoting the lower limit and tu denoting the upper limit) defined by the equations:-t1=100-20 (log #t-1.5) and tu=100-20 (log #t-4) or within the limits 90 DEG C to tu or t1 to 150 DEG C should either t1 be less than 90 DEG C or tu greater than 150 DEG C., and then freeing them from alkali metal hydroxide, all percentages being with reference to the liquor. The concentration c (in % by weight) of the alkali metal hydroxide may be correlated to the treatment temperature t (in DEG C) that it is between the limits C1 and Cu (inclusive) as defined by the equations:-C1=10-0.1 (t-100) Cu=12.5-0.1 (t-100) in the temperature range of 110 DEG -150 DEG C and C1=5.5-0.1 (t-100) Cu=8.5-0.1 (t-100) in the temperature range of 90 DEG -110 DEG C. The polyphosphate may be one having the formula Mn+2PnO3n+1 in which M is an alkali metal ion and n is an integer of 2-10, e.g. sodium or potassium pyrophosphate, tripolyphosphate, tetrapolyphosphate and hexapolyphosphate and the complex-forming aminopolycarboxylic acid may be one having the formula in which m is zero, 1 or 2 and Y is a -COOH or -CH2OH group. Suitable wetting agents are alkyl sulphonates, alkyl disulphonates, alkylaryl sulphonates, fatty acid condensates, proteinolysis products, sulphuric acid hemiesters of alkylphenol-ethylene oxide adducts or salts thereof and adducts of ethylene oxide to fatty alcohols, fatty acid amides, alkylnaphthols, and alkylphenols. Heating may be effected by steaming. The alkali metal hydroxide may be removed by rinsing first twice at boiling temperature and then once or twice at 60 DEG -80 DEG C and then acidifying with very dilute hydrochloric acid and rinsing once cold. The aqueous liquor may also contain a reducing agent, e.g. sodium dithionite, a -hydroxyalkane sulphinic acids and their salts and reaction products of a -hydroxyalkane sulphinic acids with ammonia or amines or salts thereof.

    Levelling agents for sulphur and vat dyeings
    9.
    发明专利
    Levelling agents for sulphur and vat dyeings 未知

    公开(公告)号：GB920149A

    公开(公告)日：1963-03-06

    申请号：GB3816361

    申请日：1961-10-25

    Applicant: BASF AG

    Inventor： HARTMARK BJARNE ,  REPPE HANS-GERHARD ,  ROKOHL RUDOLF ,  SEEFELDER MATTHIAS

    IPC: D06P1/22 ,  D06P1/30 ,  D06P1/52

    Abstract: Water-soluble polyamides are derived from (a) an aliphatic, cycloaliphatic or aromatic polyamine or a heterocyclic compound which contains at least two acylatable nitrogen atoms and (b) an a ,b -unsaturated carboxylic acid, an aliphatic polycarboxylic acid, an aliphatic polycarboxylic acid containing one or more hetero atoms or functional derivatives of these such as halides, anhydrides, amides or esters which are capable of amide formation. They are employed as levelling agents in dyeing with vat and sulphur dyes (see Group IV(c)). Specified (a) are phenylene diamines, xylylene diamines, toluylene diamines, 4,41-diaminodiphenylmethane, N,N1-di-(sec-butyl)-p-phenylene diamine, 1,5-naphthylene diamine and their hydrogenation products, 2-methylpiperazine, 2,5-diethylpiperazine and especially polyamines of the general formula: wherein R1 and R3 are hydrogen, alkyl or hydroxyalkyl radicals of 1-4 C-atoms or, when x is 2 and n is 0, together represent an ethylene radical; R2 is a hydrogen, alkyl or hydroxy-alkyl radical of 1-4 C-atoms; x and y are integers from 1 to 6 and n is an integer from 0 to 20, the sum of x and n being greater than or equal to 2. Especially preferred compounds of this type are ethylene diamine, hydroxyethyl-ethylene diamine, hexamethylene diamine, di-(aminopropyl)-ethylene diamines, diethylene triamine, N-propyl-diethylene diamine, triethylene tetramine, dipropylene triamine, tripropylene tetramine, N-methyl-dipropylene triamine, di-(ethylaminoethyl)-amine and piperazine. The specified compounds (b) are the acids: acrylic, methacrylic, crotonic, tiglic, malonic, succinic, glutaric, adipic, pimelic, suberic, maleic and fumaric also dipropyl ether-g ,g 1-dicarboxylic acid, thiodibutyric acid, ethylene diamine tetraacetic acid and nitrilotriacetic acid. The watersoluble polyamides may be prepared by condensing substances (a) with substances (b) in the presence or absence of inert solvents such as glycerol, polyglycols of b.p. above 160 DEG C. and tetrahydronaphthalene at 180 DEG -200 DEG C. for 30-60 minutes. The preferred proportions of reactants are chosen so that there are 1 to 1,5 1 DEG and/or 2 DEG amino groups for each carboxyl group or when using an unsaturated acid 1 to 1,5 1 DEG and/or 2 DEG amino groups for each carboxyl group and each reactive double bond. When using a ,b -unsaturated carboxylic acids small amounts of polymerization inhibitors such as hydroquinone and methylene blue may be added. The condensation of amines with acid halides may be carried out at room temperature in the presence of a proton acceptor such as pyridine or a 3 DEG aliphatic amine. The polyamides so formed have mean molecular weights of 600 to 1,500. Examples of the preparation of a number of compounds using some of the above-named reactants are given.ALSO:Water-soluble polyamides are derived from (a) an aliphatic, cycloaliphatic or aromatic polyamine or a heterocyclic compound which contains at least two acylatable nitrogen atoms and (b) an a ,b -unsaturated carboxylic acid, an aliphatic polycarboxylic acid, an aliphatic polycarboxylic acid containing one or more hetero atoms or functional derivatives of these such as halides, anhydrides, amides or esters which are capable of amide formation. They are employed as levelling agents in dyeing with vat and sulphur dyes (see Group IV(c)). Specified (a) are phenylene diamines, xylylene diamines, toluylene diamines, 4,41-diaminodiphenylmethane, N,N1-di-(sec-butyl)-p-phenylene diamine, 1,5-naphthylene diamine and their hydrogenation products, 2-methylpiperazine, 2,5-diethylpiperazine and especially polyamines of the general formula: Wherein R1 and R3 are hydrogen, alkyl or hydroxyalkyl radicals of 1-4 C-atoms or, when x is 2 and n is 0, together represent an ethylene radical; R2 is a hydrogen, alkyl or hydroxyalkyl radical of 1-4 C-atoms; x and y are integers from 1 to 6 and n is an integer from 0 to 20, the sum of x and n being greater than or equal to 2. Especially preferred compounds of this type are ethylene diamine, hydroxyethyl-ethylene diamine, hexamethylene diamine, di-(aminopropyl)-ethylene diamine, diethylene triamine, N-propyl-di-ethylene diamine, triethylene tetramine, di-propylene triamine, tripropylene tetramine, N-methyl-dipropylene triamine, di-(ethylamino-ethyl)-amine and piperazine. The specified compounds (b) are the acids: acrylic, methacrylic, crotonic, tiglic, malonic, succinic, glutaric, adipic, pimelic, suberic, maleic and fumaric also dipropyl ether-g ,g 1-dicarboxylic acid, thiodibutyric acid, ethylene diamine tetra-acetic acid and nitrilotriacetic acid. The water-soluble polyamides may be prepared by condensing substances (a) with substances (b) in the presence or absence of inert solvents such as glycerol, polyglycols of b.p. above 160 DEG C. and tetrahydronaphthalene at 180-200 DEG C. for 30-60 minutes. The preferred proportions of reactants are chosen so that there are 1 to 1.5 1 DEG and/or 2 DEG amigo groups for each carboxyl group or when using an unsaturated acid 1 to 1.5 1 DEG and/or 2 DEG amino groups for each carboxyl group and each reactive double bond. When using a ,b -unsaturated carboxylic acids small amounts of polymerization inhibitors such as hydroquinone and methylene blue may be added. The condensation of amines with acid halides may be carried out at room temperature in the presence of a proton acceptor such as pyridine or a 3 DEG aliphatic amine. The polyamides so formed have mean molecular weights of 600 to 1500. Examples of the preparation of a number of compounds using some of the above-named reactants are given.ALSO:Levelling agents for use in dyeing natural or regenerated cellulose or wool with vat or sulphur dyestuffs comprise water-soluble polyamides derived from (a) an aliphatic, cycloaliphatic or aromatic polyamine or a heterocyclic compound containing at least two acylatable nitrogen atoms and (b) an a ,b -unsaturated carboxylic acid or an aliphatic carboxylic acid which may contain one or more hetero atoms or a functional derivative of these which is capable of amide formation (see Groups IV(a) and IV(b)). The levelling agents are soluble in alkaline medium and may be applied at a concentration of 0,2-1,0 g./l. during or subsequently to dyeing. Shading, i.e. adding further small amounts of dye to the hot vat during dyeing, may be effectively accomplished. Also present in the dye-bath may be conventional dispersing agents and protective colloids. Examples are given of the dyeing of viscose staple yarn, cotton yarn and cotton knitted and woven fabrics.

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