公开(公告)号：DE1469821A1

公开(公告)日：1969-06-04

申请号：DE1469821

申请日：1959-06-24

Applicant: BASF AG

Inventor： WALTER STILZ DR ,  HORST POMMER DR ,  HEINZ FESSMANN DR ,  ERIKA WOLFF DR

IPC: C07C63/66 ,  C08G63/54 ,  C08K3/32 ,  C08K5/00 ,  C08K5/12

Abstract: An optically brightened and stabilized polyamide contains (A) a derivative of 1:4-bisstyrylbenzene having free carboxy groups, carboxylic acid ester groups, carboxylic acid amide groups and/or nitrile groups combined with both terminal phenyl radicals in the styryl groups as claimed in the parent Specification, and (B) an alkali or alkaline earth metal salt of phosphorous acid. The polyamides may contain additionally Ti(III) and cerium (III) salts, e.g. cerium (III) chloride and acetate and titanium (III) chloride hexahydrate, sulphate hexahydrate and acetate hexahydrate. Many polyamides and 1:4-bis-styryl benzene derivatives are specified. Specified phosphorus acid salts are sodium hydrogen phosphite and barium hydrogen phosphite. Examples (1) and (2) describe the addition to polyhexamethylene adipamide of:-(1) sodium phosphite pentahydrate, 1:4-bis(p-cyanostyryl)-benzene and titanium trichloride and (2) 1:4-bis-(p-carboxymethyl-styryl) benzene, sodium phosphite pentahydrate and titanium trichloride hexahydrate whist Examples (3) and (4) describe the addition to polycaprolactam of:-(3) the morpholide of 1:4-bis(p-carboxystyryl)-benzene, sodium phosphite and titanium trichloride hexahydrate and (4) sodium phosphite, 1:4-bis-(p-cyanostyryl) benzene and cerium trichloride heptahydrate.

公开(公告)号：DE1419003A1

公开(公告)日：1968-12-12

申请号：DE1419003

申请日：1959-11-06

Applicant: BASF AG

Inventor： WALTER STILZ DR ,  HORST POMMER DR ,  ROBERT GEHM DR ,  OSWALD SCHMIDT DR ,  HEINRICH MERTENS DR ,  HEHL MANFRED ,  GRUNWALD WOLFGANG

IPC: C11D1/00 ,  D06L3/12

Abstract: Substituted 1,4-bis-styryl benzenes of the general formula: in which X and X1 stand for carboxylic ester groups or N-alkyl carboxylic amide groups, are prepared by reacting terephthaladehyde with an ester of a carbalkoxy-benzylphosphonic acid or with an ester of a halogenmethylbenzoic acid, with the aid of a triarylphosphine and an alkali alcoholate, and if necessary converting the ester groups of the products into amide groups. These substituted 1,4-bis-styryl benzenes are optical brightening agents (Group IV(c)). In Example 1, the methyl ester of p-chlormethylbenzoic acid is stirred with triphenylphosphine in dimethylformamide at 80 DEG C. for 3 hours; and then terephthalaldehyde followed by sodium methylate are added. The product is 1,4-bis-(para-carbmethoxy-styryl)-benzene, and this is converted, by heating it with diethanolamine, into 1,4-bis-(para-carbodiethanolamidostyryl)-benzene Example 8 refers to 1,4-bis-(meta-carbdiethanolamido-styryl)-benzene. Example 9 describes the preparation of a mixture of 1,4-bis-(para-carbethoxy-styryl) - benzene, 1,4 - bis - (metacarbmethoxy-styryl)-benzene and 1-(para-carbmethoxy-styryl) - 4-(meta1-carbmethoxy-styryl)-benzene, by reacting terephthalaldehyde with a mixture of meta- and para-carbmethoxy-benzyl-phosphonic acid diethyl ester. The mixture of 1,4-bis-styryl-benzene diesters is then reacted with diethanolamine. Example 19 states that 1,4-bis-(meta-carb-N-cyclohexylisopropanol-amidostyryl)-benzene is obtained by reacting 1,4 - bis - (meta-carbmethoxy-styryl)-benzene with N-cyclohexyl-iso-propanolamine. It is stated that X and X1 in the general formula may stand for COO.C2H4OH, and similar groups. Compounds wherein the hydrogen atoms of the hydroxy groups in both the amides and the esters are substituted by glycol ether groups are obtained by the reaction of the amides or esters with ethylene oxide or propylene oxide. Specification 813,539 is referred to.ALSO:Substituted 1, 4-bis-styryl benzenes of the general formula in which X and X1 stand for carboxylic ester groups or N-alkyl carboxylic amide groups, act as brightening agents for textiles, paper and leather. The brightening agent is preferably used in aqueous medium in amounts of about 0,0015 to 0.05% with reference to the weight of the substrate to be brightened. In Example 1, previously bleached cotton fabric is treated, for 20 minutes, in a liquor, at 50 DEG to 60 DEG C., containing 0,003 to 0,01 grams per litre of the compound having the structure and 5 grams per litre of sodium sulphate decahydrate, the liquor to fabric ratio being 50:1. After rinsing and drying, the fabric has a dazzling whiteness of good fastness to light and washing. Examples 5, 6 and 7 relate to the use of the same compound for brightening polycaprolactam fabric, yellowish paper, and soiled clothing, respectively. Example 8 describes the use of 1, 4-bis-(metacarbdiethanolamidostyryl)-benzene for brightening cotton fabric. For the preparation of the brightening agents, (see Group IV(b)). Specification 813,539 is referred to.