Patent GB-1243990-A (GB)
Title: Process for treating cellulosic materials
IPC: D06M16/00
Filed: 1968-11-29
Abstract: 1,243,990. Water- and fireproofing; optically brightening; protecting against U-V light. E. I. DU PONT DE NEMOURS & CO. 29 Nov., 1968, No. 56884/68. Heading D1P. [Also in Division A5] A cellulosic material or blend thereof with a synthetic material is treated with at least one agent selected from fire- or waterproofing agents, biocides, U-V light absorbers and fluorescent brighteners by contacting it in any sequence with: (1) sufficient water to swell the cellulose; (2) one or more of said agents, each said agent being used in an amount of at least 20 times its solubility in 1 litre of boiling water, expressed in grams and; (3) a solvent in an amount sufficient to dissolve said agent(s) and to maintain swelling of the cellulose if water is removed and which (a) is at least 2.5% by weight soluble in water at 25‹C, (b) boils above 150‹C at atmospheric pressure, (c) is a solvent for the agent at some temperature in the range 0-225‹C and (d) has the formula where n is 0 or 1 ; m is an integer; R is H, C 1-8  alkyl, C 7-15  aralkyl or alkaryl, R<SP>2</SP>CO-, R<SP>2</SP>SO 2 -, R<SP>2</SP>OCO-; R<SP>1</SP> is -OH, -OR<SP>2</SP>, -SR<SP>2</SP>, -NHR<SP>2</SP>, -NR<SP>2</SP> (C 1-8  alkyl), -OCOR<SP>2</SP>, -NR<SP>2</SP>(C 7-15  aralkyl or alkaryl), -OSO 2 R<SP>2</SP>, -OCOOR<SP>2</SP>, -NH(phenyl), or -NH(naphthyl); R<SP>2</SP> is C 1-8  alkyl, C 5-10  cycoalkyl, C 7-15  aralkyl or alkaryl, C 6  aryl, C 10  aryl or furfuryl; A is ROCH 2 CHORCH 2 -, -CH 2 CHORCH 2 -, -CH 2 -CHCH 2 -, -CH 2 C(CH 2 OR) 3 , (-CH 2 ) 2  C(CH 2 OR) 2 , (-CH 2 ) 3 CCH 2 OR, (-CH 2 ) 4 C, -CH 2 (CHOR) y CH 2 OR or -CH 2  (CHOR) y-z  (-CH) z CH 2 -; x is the number of unsatisfied valencies in A; and y is 2, 3 or 4 and z is 0, 1, 2, 3 or 4 no greater than y; provided that at some stage during the process the interior of the swollen cellulose is contacted with a solution of the agent in solvent or aqueous solvent. Solvents used in examples are di- and tri-ethylene glycol diacetate, methoxypolyethylene glycol and dipropylene glycol. Exemplified agents are: fluorescent brighteners, 2-(m-chloro styryl)naphth[2,1-d]oxazole, α,#- dibenzoxazolyl ethylene which may be methyl or cyclohexyl substituted, 4,4'-bis(2,4-dimethoxybenzoylamino)stilbene, and 4,4'-bis(phenylureido)stilbene-2,2'-disulphonamide; flame retarders, trimeric phosphonitrilic anilide, N,N', N"'-tris(3,4-dichlorophenyl)phosphoramide and its N,N'N"'-trimethyl derivative, bis (p-bromophenyl)chloromethylphosphonate and 2,2-bis(3, 5-dibromo-4-hydroxyphenyl)propane; U-V absorbers, 2-(2-hydroxy-5-methylphenyl)-2,1,3- benzotriazole, 4-dodecycloxy-2-hydroxybenzophenone and [2,2'-(2,3,5,6-tetramethylterephthalogldiimino)-o-phenylene]-bis-2,1,3-benzotria - zole; water proofing agent, a condensate of C 15-21  fatty acid and hexamethoxymethylmelamine at 6:1 molar ratio; biocides are tribromosalicylanilide and doecyl quanidine terephthalate. Exemplified materials are cotton or cotton/ polyester fabrics. In Example 15 the washfastness of cotton impregnated with tribromosalicylanilide is improved by treatment with a resin of the dimethyloldihydroxyimidazolone type. The process may be effected by padding with an aqueous bath containing all the ingredients, or by two stage padding, following which the impregnated material is squeezed and heated, e.g. at 125-225‹C.