US2781281A - Flame-proofing of textiles - Google Patents
Flame-proofing of textiles Download PDFInfo
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- US2781281A US2781281A US510533A US51053355A US2781281A US 2781281 A US2781281 A US 2781281A US 510533 A US510533 A US 510533A US 51053355 A US51053355 A US 51053355A US 2781281 A US2781281 A US 2781281A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/423—Amino-aldehyde resins
- D06M15/43—Amino-aldehyde resins modified by phosphorus compounds
- D06M15/433—Amino-aldehyde resins modified by phosphorus compounds by phosphoric acids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S428/00—Stock material or miscellaneous articles
- Y10S428/92—Fire or heat protection feature
- Y10S428/921—Fire or flameproofing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
- Y10T442/2631—Coating or impregnation provides heat or fire protection
- Y10T442/2672—Phosphorus containing
- Y10T442/268—Phosphorus and nitrogen containing compound
Definitions
- ATTORNEYS p egnj n be hs e 1 95 1 6 "foret littlelsuitedespecially'for the treatmentof la e an undesirable way;
- textile fabrics can be rendered flame-proof; wlderf'a ing the above drawbacks to a great'extent by "t lj t abq 11 48'%j y., ve b a fro bout 24m 38 b we if m 'st tri'a zine, the ratio of component (1),. toco'fn" labbut vtwo hours. fln case the mixtureis "temperature in the n "g! period is advantageously ⁇ or even 8: v
- the reaction mixture used as component (1) may be prepared by heating an oxygen-containing compound of phosphorus of the group consisting of ortho -phospl oric acid, pyrophosphoric acid, metaphosphoric acid andammoniuni salts of said,acids, together anexces pf Qurea preferably in a. weightra'tio, of 3 parts oftthe ,to S 'to Sfpafts ofithellatter 'at 'a,temperature,p abput 100"? 'c. analzooz c.,1pI fr B1y at 155" 16 0130.
- mlide of "m ss b it t dam s t iazin a has .2- chloro-4z6-diamino-Iz3z5 triazine;" and also methylol compounds of guanaminessuch, for example, as those of benzo-guanamine- (2-pheny l -4:6- diarnino l: 3 :5.- tria z ine),
- components may be dissolved or dispersed ..in .'water, whereby-clear solutions or very finely ,divided .disp'ersions are obtained.
- finish is 'resistant'to water and thefeel and tensile strength of,'for example; a cotton fabricgiare notxz'hanged; "I'f'the drying iscarried out atja temperature" above 100 C.,"for example; at -160 C., or if 'thlfabric' is .dried at a' temperature beloWlOO. C., aindlthen after hardening is broughtabout at, for. example, 12()'-"160 .Cl'; theifi'ame proo'f finish" is ..also resistanttow'ashing with neutral washing" agents.
- An impregnating bath (containing about 36% of the above reaction mixture and 9% of the component (2) described below) is prepared by mixing 80 parts of the above described concentrated solution, with 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde (component (2)), and 20 parts of water, a small amount of a precipitate being formed which remains in a fine state of dispersion.
- Cotton is impregnated at ordinary temperature with the above bath, and the cotton is squeezed, then dried at 70 C. and subjected to a heat-treatment at 150 C. for five minutes. It is then thoroughly rinsed with cold water and again dried.
- the fabric dried at 70 C. can be impregnated a second time and dried again at 70 C.
- Example 2 A cotton fabric is impregnated in a bath having the following composition: 20 parts of water, 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde, (component (2) 80 parts of a solution obtained by dissolving about 30 parts of the reaction mixture (component (1)) described below in 50 parts of water.
- the impregnating bath thus contains about 27% of component (1) and 9% of component (2).
- the flame-proof finish so obtained is resistant to a washing treatment carried out at 70 C. for 30 minutes in a bath containing 1 gram per liter of a sulfonated washing agent having a neutral reaction. Washing can also be carried out at the boil when a washing agent free from ions is used.
- reaction mixture (component (1) is made by heating 30 parts of pyrophosphoric acid with 50 parts of urea for 30 minutes at 160 C.
- condensation product of unlimited solubility in water prepared from 1 molecular proportion of melamine and 2 to 3 molecular proportions of formaldehyde there may be used such a condensation product which is soluble in water only in the ratio of 1:1, or there may be used a condensation product of unlimited solubility in water prepared from 1 molecular proportion of melamine and 4 molecular proportions of formaldehyde.
- Example 3 The procedure is the same as that described in Example 2, except that the fabric after being dried at C. is subjected to a heat treatment at 120 C. for 20 minutes. Analysis shows a phosphorus content of 1.30% and a nitrogen content of 3.31%.
- Example 4 200 parts of urea are melted at 140 C. parts of diammonium ortho-phosphate are gradually introduced while stirring. The mixture is then heated to 160 C. and maintained at that temperature for 30 minutes. There is obtained a clear melt. After cooling to C., 200 parts of water are added. When the solution is cooled to room temperature a small amount of insoluble matter precipitates and is removed by filtration. The filtrate is then adjusted to a pH value of 8 by means of ammonia.
- An impregnating bath is prepared by mixing 80 parts of the above described concentrated solution with 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde, and 20 parts of water.
- This impregnating bath contains 38% of the reaction mixture and 9% of the said methylol melamine.
- Cotton is impregnated with the above bath at ordinary temperature. Then it is sequeezed, dried at 70 C., subjected to a heat-treatment at C. for 10 minutes, rinsed with water and dried. Analysis shows a phosphorus content of 1.77% and a nitrogen content of 4.13%.
- Example 5 250 parts of urea and 100 parts of orthophosphoric acid of 75 percent strength are heated at C. A further 100 parts of ortho-phosphoric acid of 75 percent strength and 50 parts of urea are added to the reaction mixture at that temperature, and the mixture is then heated for 10 minutes at 160 C. After cooling to 110 C., 400 parts of water are added and the solution, after being cooled to room temperature, is adjusted to a pH value of 8 by means of ammonia.
- An impregnating bath is prepared by mixing 80 parts of the above described concentrated solution with 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde, and 20 parts of water.
- This impregnating liquid contains 32% of the above reaction mixture and 9% of the said methylol melamine.
- Example 4 The procedure is the same as that described in Example 4, except that the heat-treament is carried out at 140 C. for 6 minutes. Analysis shows a phosphorus content of 2.09% and a nitrogen content of 4.9%.
- the wool so treated has a very good flameproof property. Thefeelof the "fabric is not changed by the treatment.
- a process-for renderingtextile fabrics'flarneproof which comprises impregnating the fabric in an aqueous liquid which contains (1) about'12-48%by*weight of a reaction mixture obtained by heating an-excess of urea together with an oxygen-containing compound ofphosphorus selected from the group consisting of orthophosphoric 1 acid, pyrophosphoric acid, meta-phosphoric acid and armnoniumcsalts 'of ftheseflacids, ,at a high temperature, and (2) about 2-18% bytweight of ajmethylol- .tm'elarninefthe ratio of component (1): to component (2) ranging from 3:1 to 6:1, and .dryingthe impregnated 1 fabric, at a raised temperature.
- a process for rendering textile fabrics fiameproof which comprises impregnating the fabric in an aqueous liquid which contains 1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with pyrophosphoric acid at a high temperature, and (2) about 4-12% by weight of a methylol-melamine the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C.
- a process for rendering textile fabrics flameproof which comprises impregnating the fabric in an aqueous liquid which contains (1) about 27-37% by weight of a reaction mixture obtained by heating -8 parts of urea with 3 parts of pyrophosphoric acid at 160 C. for 30 minutes, and (2) 9% by weight of a condensation product of unlimited water-solubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at 70 C. and after-hardening the dried fabric at ISO-160 C.
- a process for rendering textile fabrics flameproof which comprises impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea o ether with d ammea um .at hg hosp a e a a hi vternperature,.and (2 aboutA-l-12% by weightof ameth- -y1ol-melamine, the ratio of component (1) to component r gi o Lan -dryin h impr gnats fabricat atemperature ranging from 70 C. to. 1I60 C. .6.
- a process ;for rendering ltextile fabrics flameproof which comprises impregnating the fabric in an aqueous liquid which contains 1) 3.8%, by..weight,of,areaction mixture obtained by,he ating,;6.partsofiureawith 3 parts of diammoniumortho-phosphateat 160. C. for.3 01rninutes, and (2) 9%Ibylweight of a c ondensationprodnct of unlimited water-solubility ,ofone, molof, melamine. with about 2-3 molsof formaldehyde, drying-the impregnated fabric, at 70 c. andafter-h ar-dening t dried fabric at 7.
- a process for renderingtextile;fabrics flarneproof which-comprises impregnating the fabric in an, aqueous liquid-which, contains, (1),.abput 241- 3876 byweight of .a reaction mixture obtained by heating an excessof urea togetherwith ortho phosphoric acidsat a-high temperature, and (2) .fabout-.,4- '12%. lay-weight of 1a methylolmelamine, the ratioof component: 1) -to compone nt (2) ranging from 3:1,to 6:1, andfirying,theimpregnated fabriofit a temperature ranging; from .70 C. to 160. C.
- a textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 12-48% by weight of a reaction mixture obtained by heating an excess of urea together with an oxygen-containing compound of phosphorus selected from the group consisting of ortho-phosphoric acid, pyrophosphoric acid, meta-phosphoric acid and ammonium salts of these acids, at a high temperature, and (2) about 2-18% by weight of a methylol-melamine, the ratio of component 1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a raised temperature, the amounts of phosphorus and nitrogen fixed in and on the fibers being about 13-40% of the former and about 2.8-6.0% of the latter.
- a textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with an oxygen-containing compound of phosphorus selected from the group consisting of ortho-phosphoric acid, pyrophosphoric acid, meta-phosphoric acid and ammonium salts of these acids, at a high temperature, and (2) about 4-12% by weight of a methylol-melamine, the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a raised temperature, the amounts of phosphorus and nitrogen fixed in and on the fibers being about 134.0% ofthe former and about 2.8-6.0% of the latter.
- a textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with pyrophosphoric acid at a high temperature, and (2) about 4-12% by weight of a methylol-melamine the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.34.0% of the former and about 2.8-6.0% of the latter.
- a textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 27-37% by weight of a reaction mixture obtained by heating -8 parts of urea with 3 parts of pyrophosphoric acid at 160 C. for 30 minutes, and (2) 9% by weight of a condensation product of unlimited water-solubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at 70 C. and after-hardening the dried fabric at ISO-160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being 2.52.9% of the former and 4.8-5.3% of the latter.
- a textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with diammonium ortho-phosphate at a high temperature, and, (2) about 4-12% by weight of a methylol melamine, the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.3-4.0% of the former and about 2.8-6.0% of the latter.
- a textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) 38% by weight of a reaction mixture obtained by heating 6 parts of urea with 3 parts of 'diammonium ortho-phosphate at 160 C. for 30 minutes, and (2) 9% by weight of a condensation product unlimited water-solubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at C. and after-hardening the dried fabric at C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.7-1.8% of the former and about 4.142% of the latter.
- a textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by Weight of a reaction mixture obtained by heating an excess of urea together with ortho-phosphoric acid at a high temperature, and (2) about 4-12% by weight of a methylol-melamine, the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.3-4.0% of the former and about 2.8-6.0% of the latter.
- a textile fabric which has a fiameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) 32% by weight of a reaction mixture obtained by heating 6 parts of urea with 3 parts of orthophosphoric acid at 160 C. for 10 minutes, and, (2) 9% by weight of a condensation product of unlimited watersolubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at 70 C. and after-hardening the dried fabric at C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 2.1% of the former and about 5.0% of the latter.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
Feb. 12, 1957 A. BERGER 2,781,281
FLAME-PROOFING OF TEXTILES Filed May 23, 1955 Textile Material Flame-Pmofed with the aid of (I) Reaction product of urea and 0- containing compound of phosphorus, and
(2) Methylolmelamine INVENTOR ALFRED BERGER BY WM,
ATTORNEYS p egnj n be hs e 1 95 1 6 "foret littlelsuitedespecially'for the treatmentof la e an undesirable way;
textile fabrics can be rendered flame-proof; wliilef'a ing the above drawbacks to a great'extent by "t lj t abq 11 48'%j y., ve b a fro bout 24m 38 b we if m 'st tri'a zine, the ratio of component (1),. toco'fn" labbut vtwo hours. fln case the mixtureis "temperature in the n "g! period is advantageously} or even 8: v
i p v dii e'bs fi 's v iw i stint 2.1 l concentrated.stockisolutions.
1 pounds. of 224.:6-triamino-l :3 z-triazine finally methylolcompounds.which,are partiall etherit ied 227 1 :ELAME-PRQOFWG, 0F TEXTILES A r -B L tae l; Sw tze land, s gn r o b ited, Basel, Switzerland, a Swiss firm Application May 23, (1955, Serial No. 510,533 31 cla m (C nk-135) This is a continuation in part of my U. S. patent application Serial No. 301,377,;filed July 28, 1952, now am de Know pro s e fo /r nde n ex e-pt o t h t jdi a van gth ej i 11y: sable an batches of texti leflfabrics, or thetenslile' the feel of the textiles are changed th ,The present invention is based on the observati on that ing the fabric with an aqueous l iquidwhich, on ins lp 'e r'ably gobtained by heating an jexcess "of u'rea ether an .oxygen-co'ntaining" compound offphos rus s ected from the'group consisting bf ort'lio-p liosphor'id ,acid, jpyr;o-
phosphoric acid, meta-phosphoric acid and ammonium salts of these acids, at a high temperatureg'and (2) fro n about 2 to 18% by weight, and preferably-from 'bo' t'4 to 12%.,by weight of'a'methylol compound of a ranging from 3:1 to 6zl, and drying the fabric at a raised temperature.
The reaction mixture used as component (1) may be prepared by heating an oxygen-containing compound of phosphorus of the group consisting of ortho -phospl oric acid, pyrophosphoric acid, metaphosphoric acid andammoniuni salts of said,acids, together anexces pf Qurea preferably in a. weightra'tio, of 3 parts oftthe ,to S 'to Sfpafts ofithellatter 'at 'a,temperature,p abput 100"? 'c. analzooz c.,1pI fr B1y at 155" 16 0130.
H 1 i P i s m l a gissfr a qsts me p ss t fi 'b re lus j As; inetliylolfi compounds 7 .of .an aminotriazine used; as
component "(2) there maybe used the methylol-,cgm-= ine); and
@156; me'thylol compounds of thosel de A s tof m elamine'vwhichtstiil' contain at least one am group and l adyantageously at least 1 two, amino, groups; J for fexample,
methylolwcompounds .of s.mel am,,,rnelem, ammeline; am-
mlide of "m ss b it t dam s t iazin a has .2- chloro-4z6-diamino-Iz3z5 triazine;" and also methylol compounds of guanaminessuch, for example, as those of benzo-guanamine- (2-pheny l -4:6- diarnino l: 3 :5.- tria z ine),
,aceto' guanamine Kl-methyl 4:6 amino. t or fo rrno-Igu anamine' (4,: 6-diamino- 1'; 3 :5 -t ne) with aliphatic alcoholsflof low, molecular weight such as groups, inwhich 2 to 6 'inethylol groups'are et herified.
:: :1 Patented t 2 ad ant e y methy p zmelamin a e u d 4 1M52 cially se wh c a .o 'un imit olu lit a Very suitable condensationproducts are those of unlimited solubility in Water which are obtainable from one molecular proportion of melamine and about 2"to 3 molecular "proportions of "formaldehyde. ,Obviously .there may-alsoibe .usedmixturesof'such aminotriazine c'ondensationproducts'. W
lFor "preparing the aqueous impregnating liquids the individual; components may be dissolved or dispersed ..in .'water, whereby-clear solutions or very finely ,divided .disp'ersions are obtained.
tThe 'textileifabricsrriay be impregnated with therbath by means of the known methods and'apparatusIforimpregnatingf fabrics. .There are advantageously used cbn- "centrated impregnating baths which are rendered slightly alkaline,';for example, by adjustment to a pH value of 8. In this manner the impregnation produces1a -large increaseiih the weight of the fabric, so thatgthefiamej'proof effectds considerably enhanced. .Wetting' agents may alsotbe'added to tlieibath'in' order to improve :the wetting o'f the fabricHQThere are advantageously used bathsthaviiigatdry content of about 30-50 'percent. v-Siichtbathstare'stable 'for long periods, for example, from 4. hours to several" days, that is to say, no'wat'er- 'insohiblefcompuurids'are formedwhen thef'baths areallowed' tol'stand "at ordinary/temperature", orqif insoluble compounds were formed at the outset the amount thereof jincreases slowly and .theiundissolved portions remain in a"finely..dispersed.form. ,Duringthe drying'of the'rfab'ric at "a raised temperature .there are :f'oin1ed-:from-the various components of "the'iinpregnatiiigi bath" andprobably also with the assistance of the textile fibers, insoluble compoundswhich produce .theifiame-proof cited. The StrengthWitlfWhich th'efin'ishis fixed onithe fibrous materialideperids .onith'e td'r'ying temperature? If tlie' tlry- 'ing'is carried out at a temperature below C.'; for example, a'til70" VCQ, the. flame-proof: finish is 'resistant'to water and thefeel and tensile strength of,'for example; a cotton fabricgiare notxz'hanged; "I'f'the drying iscarried out atja temperature" above 100 C.,"for example; at -160 C., or if 'thlfabric' is .dried at a' temperature beloWlOO. C., aindlthen after hardening is broughtabout at, for. example, 12()'-"160 .Cl'; theifi'ame proo'f finish" is ..also resistanttow'ashing with neutral washing" agents. (,One or other method of dfying'is used dependingon the L purpose for whili' the treated fabric is t'o be'ii'sed'. The quality of the fiame-proofifinish depends not'only o'n-the conditions of drying or hardening but, as stated above, also on the amount of theifnpregnating substances fixed on :th rfibcr. ,jExpejrirnents have shown fth-at it is oPadvantage to carry out the impregnation in such manner nfil a n rease i iwei ht of not, substantially less than about 6 percent; occurs. At increases in weight ranging from .-l 0715 percent. there "are. obtained very good flamet prooieffectsT. 'Dh'e impregnation 'may also bec'arriedout more Zsjtrongly so as'jto produce, for examplefanfinc'rease in weight of about 20 "percent; '(The iii'crease's'in" :ei'ght arecalculated 'on'thematerial after it has been "dried, hardened, rinsed andfagain" dried; the untreated :fa b ric "serving as the s'tar'ti ngfpbint) 'fThe uantity :of the phosphoi' usfixed "on and iii the'fibjers i s' eachfii me" bout aasmsr illustrates textile material flame-proof'ed according to the Example 1 15 parts of pyrophosphoric acid and 80 parts of urea are slowly heated to 140 C., and at 140-145 C. a further 15 parts of pyrophosphoric acid are added, the temperature is raised to 160 C. and this temperature is maintained for 30 minutes. The mixture is then allowed to cool to about 100 C. and 90 parts of water are added to the reaction mixture, whereby a clear solution is obtained. The whole is then allowed to cool to -15 C., whereupon a small amount of biuret crystallizes out. The mixture is filtered to remove this precipitate, and the filtrate is mixed with ammonia until the solution has a pH value of 8. The solution is stable at ordinary temperature and can be used for the preparation of impregnating baths.
An impregnating bath (containing about 36% of the above reaction mixture and 9% of the component (2) described below) is prepared by mixing 80 parts of the above described concentrated solution, with 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde (component (2)), and 20 parts of water, a small amount of a precipitate being formed which remains in a fine state of dispersion.
Cotton is impregnated at ordinary temperature with the above bath, and the cotton is squeezed, then dried at 70 C. and subjected to a heat-treatment at 150 C. for five minutes. It is then thoroughly rinsed with cold water and again dried.
Analysis shows a phosphorus content of 2.85% and a nitrogen content of 5.25% by weight based on the dry weight of the untreated textile fabric. The flame-proof effect is very good. The material does not after flame or after glow. The tensile strength is not affected by the treatment and the feel of the material remains unaltered.
Instead of the above mentioned heat treatment at 150 C., the fabric dried at 70 C. can be impregnated a second time and dried again at 70 C.
The treated material of this and the subsequent examples is tested for its flame-proof quality by means of the vertical Bunsen burner test. This test is described for example, in the book by R. W. Little (Flame-Proofing of Textile Fabrics, Reinhold Publishing Corporation, New York, 1947, page 111 et seq.).
Example 2 A cotton fabric is impregnated in a bath having the following composition: 20 parts of water, 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde, (component (2) 80 parts of a solution obtained by dissolving about 30 parts of the reaction mixture (component (1)) described below in 50 parts of water.
The impregnating bath thus contains about 27% of component (1) and 9% of component (2).
After squeezing the fabric, it is dried at 70 C., subjected to a heat-treatment at 160 C. for 3 minutes and then rinsed with water and again dried. Analysisshows a phosphorus content of 2.53% and a nitrogen content of 4.85%.
The flame-proof finish so obtained is resistant to a washing treatment carried out at 70 C. for 30 minutes in a bath containing 1 gram per liter of a sulfonated washing agent having a neutral reaction. Washing can also be carried out at the boil when a washing agent free from ions is used.
The above mentioned reaction mixture (component (1) is made by heating 30 parts of pyrophosphoric acid with 50 parts of urea for 30 minutes at 160 C.
Instead of the above mentioned condensation product of unlimited solubility in water prepared from 1 molecular proportion of melamine and 2 to 3 molecular proportions of formaldehyde, there may be used such a condensation product which is soluble in water only in the ratio of 1:1, or there may be used a condensation product of unlimited solubility in water prepared from 1 molecular proportion of melamine and 4 molecular proportions of formaldehyde.
Example 3 The procedure is the same as that described in Example 2, except that the fabric after being dried at C. is subjected to a heat treatment at 120 C. for 20 minutes. Analysis shows a phosphorus content of 1.30% and a nitrogen content of 3.31%.
Example 4 200 parts of urea are melted at 140 C. parts of diammonium ortho-phosphate are gradually introduced while stirring. The mixture is then heated to 160 C. and maintained at that temperature for 30 minutes. There is obtained a clear melt. After cooling to C., 200 parts of water are added. When the solution is cooled to room temperature a small amount of insoluble matter precipitates and is removed by filtration. The filtrate is then adjusted to a pH value of 8 by means of ammonia.
An impregnating bath is prepared by mixing 80 parts of the above described concentrated solution with 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde, and 20 parts of water.
This impregnating bath contains 38% of the reaction mixture and 9% of the said methylol melamine.
Cotton is impregnated with the above bath at ordinary temperature. Then it is sequeezed, dried at 70 C., subjected to a heat-treatment at C. for 10 minutes, rinsed with water and dried. Analysis shows a phosphorus content of 1.77% and a nitrogen content of 4.13%.
Example 5 250 parts of urea and 100 parts of orthophosphoric acid of 75 percent strength are heated at C. A further 100 parts of ortho-phosphoric acid of 75 percent strength and 50 parts of urea are added to the reaction mixture at that temperature, and the mixture is then heated for 10 minutes at 160 C. After cooling to 110 C., 400 parts of water are added and the solution, after being cooled to room temperature, is adjusted to a pH value of 8 by means of ammonia.
An impregnating bath is prepared by mixing 80 parts of the above described concentrated solution with 10 parts of a condensation product of unlimited solubility in water from 1 molecular proportion of melamine and about 2 to 3 molecular proportions of formaldehyde, and 20 parts of water.
This impregnating liquid contains 32% of the above reaction mixture and 9% of the said methylol melamine.
The procedure is the same as that described in Example 4, except that the heat-treament is carried out at 140 C. for 6 minutes. Analysis shows a phosphorus content of 2.09% and a nitrogen content of 4.9%.
the temperature increasing to 160 C. When the addition Example 6 400 parts of urea are melted and at 140' C. parts of meta-phosphoric acid are slowly introduced into the melt,
Example 7 Inorder to improve its absorptive capacity wool gab- -ardine is treated for 30 minutes -at '45-.50 C. in a bath which contains-1 cccr-of ammonia solution of ZO-percent =st-rength; and 'l -gram-'- of a sulfonated washing agent per liter, and the fabric is rinsed and dried. The fabric is then impregnated with the bath described in Example 1, dried -at"80 C., again impregnated and dried for 30 minutes at '80" C., and then Wellrinse'd.
"The wool so treated has a very good flameproof property. Thefeelof the "fabric is not changed by the treatment.
What is claimedis:
1. A process-for renderingtextile fabrics'flarneproof, which comprises impregnating the fabric in an aqueous liquid which contains (1) about'12-48%by*weight of a reaction mixture obtained by heating an-excess of urea together with an oxygen-containing compound ofphosphorus selected from the group consisting of orthophosphoric 1 acid, pyrophosphoric acid, meta-phosphoric acid and armnoniumcsalts 'of ftheseflacids, ,at a high temperature, and (2) about 2-18% bytweight of ajmethylol- .tm'elarninefthe ratio of component (1): to component (2) ranging from 3:1 to 6:1, and .dryingthe impregnated 1 fabric, at a raised temperature.
-2. "A process for rendering textilefabrics fiameproof, -which' comprises impregnating the. fabric in an aqueous liquid which contains 1) about 24-38% by weight of a reaction mixture obtained by'heatin-g an excess of urea I together: with an oxygen-containing; compound ofephosphorus selected from the group consisting of orthophosphoric acid, pyrophosphoric acid, meta-phosphoric acid and ammonium salts of these acids, at a high temperature, and (2) about 4-12% by Weight of a methylolmelamine, the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a raised temperature.
3. A process for rendering textile fabrics fiameproof, which comprises impregnating the fabric in an aqueous liquid which contains 1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with pyrophosphoric acid at a high temperature, and (2) about 4-12% by weight of a methylol-melamine the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C.
4. A process for rendering textile fabrics flameproof, which comprises impregnating the fabric in an aqueous liquid which contains (1) about 27-37% by weight of a reaction mixture obtained by heating -8 parts of urea with 3 parts of pyrophosphoric acid at 160 C. for 30 minutes, and (2) 9% by weight of a condensation product of unlimited water-solubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at 70 C. and after-hardening the dried fabric at ISO-160 C.
5. A process for rendering textile fabrics flameproof, Which comprises impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea o ether with d ammea um .at hg hosp a e a a hi vternperature,.and (2 aboutA-l-12% by weightof ameth- -y1ol-melamine, the ratio of component (1) to component r gi o Lan -dryin h impr gnats fabricat atemperature ranging from 70 C. to. 1I60 C. .6. A process ;for rendering ltextile fabrics flameproof, which comprises impregnating the fabric in an aqueous liquid which contains 1) 3.8%, by..weight,of,areaction mixture obtained by,he ating,;6.partsofiureawith 3 parts of diammoniumortho-phosphateat 160. C. for.3 01rninutes, and (2) 9%Ibylweight of a c ondensationprodnct of unlimited water-solubility ,ofone, molof, melamine. with about 2-3 molsof formaldehyde, drying-the impregnated fabric, at 70 c. andafter-h ar-dening t dried fabric at 7. A process for renderingtextile;fabrics flarneproof, which-comprises impregnating the fabric in an, aqueous liquid-which, contains, (1),.abput 241- 3876 byweight of .a reaction mixture obtained by heating an excessof urea togetherwith ortho phosphoric acidsat a-high temperature, and (2) .fabout-.,4- '12%. lay-weight of 1a methylolmelamine, the ratioof component: 1) -to compone nt (2) ranging from 3:1,to 6:1, andfirying,theimpregnated fabriofit a temperature ranging; from .70 C. to 160. C.
"8. A process for re ndering textile fabrics-fiameproof, which comprises impregnatiiigdhe fabric in an, aqueous liquidwhich contains '(1) 32%.. ,by:Weight of a reaction ,mixture obtained by heatingd parts ,of. ureawith B parts of ortho-phosphoric acid at 1,60"v C. for 10 minutes, and (2) 9% by weight ,of. a, condensation product .of unlimited water-solubility of one mol of melamine-with "about 2-3 ,rnols of, formaldehyde, drying the impregnated fabric at.70 C. and, after-hardening .the driedfabric at 9. A processhfor rendering textile fabr ics.flameproof,
which Comprisesimpregnating-the fabric in an. aqueous liquid which containstl) rabout 24-3 8% byweig htpfa reaction mixture obtained \by heating an excesslo f urea together withmeta-P 1Osphoric;acid at a high temperature,
amine, the ratio of, component (.1),,to1comppnent (2) ranging from. 3 :1 to 6: 1, and dryingthe impregnated fabric at a temperature ranging from 70 C.; to .1 60- C.
, 10,. A procession rendering-,textile fabrics flameproof,
mixture obtained by heating 8 parts of urea with 3 parts of meta-phosphoric acid at 160 C. for about 15 minutes, and (2) 9% by weight of a condensation product of unlimited water-solubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at 70 C. and after-hardening the dried fabric at C.
11. A textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 12-48% by weight of a reaction mixture obtained by heating an excess of urea together with an oxygen-containing compound of phosphorus selected from the group consisting of ortho-phosphoric acid, pyrophosphoric acid, meta-phosphoric acid and ammonium salts of these acids, at a high temperature, and (2) about 2-18% by weight of a methylol-melamine, the ratio of component 1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a raised temperature, the amounts of phosphorus and nitrogen fixed in and on the fibers being about 13-40% of the former and about 2.8-6.0% of the latter.
12. A textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with an oxygen-containing compound of phosphorus selected from the group consisting of ortho-phosphoric acid, pyrophosphoric acid, meta-phosphoric acid and ammonium salts of these acids, at a high temperature, and (2) about 4-12% by weight of a methylol-melamine, the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a raised temperature, the amounts of phosphorus and nitrogen fixed in and on the fibers being about 134.0% ofthe former and about 2.8-6.0% of the latter.
13. A textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with pyrophosphoric acid at a high temperature, and (2) about 4-12% by weight of a methylol-melamine the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.34.0% of the former and about 2.8-6.0% of the latter.
14. A textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 27-37% by weight of a reaction mixture obtained by heating -8 parts of urea with 3 parts of pyrophosphoric acid at 160 C. for 30 minutes, and (2) 9% by weight of a condensation product of unlimited water-solubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at 70 C. and after-hardening the dried fabric at ISO-160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being 2.52.9% of the former and 4.8-5.3% of the latter.
15. A textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by weight of a reaction mixture obtained by heating an excess of urea together with diammonium ortho-phosphate at a high temperature, and, (2) about 4-12% by weight of a methylol melamine, the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.3-4.0% of the former and about 2.8-6.0% of the latter.
16. A textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) 38% by weight of a reaction mixture obtained by heating 6 parts of urea with 3 parts of 'diammonium ortho-phosphate at 160 C. for 30 minutes, and (2) 9% by weight of a condensation product unlimited water-solubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at C. and after-hardening the dried fabric at C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.7-1.8% of the former and about 4.142% of the latter.
17. A textile fabric which has a flameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) about 24-38% by Weight of a reaction mixture obtained by heating an excess of urea together with ortho-phosphoric acid at a high temperature, and (2) about 4-12% by weight of a methylol-melamine, the ratio of component (1) to component (2) ranging from 3:1 to 6:1, and drying the impregnated fabric at a temperature ranging from 70 C. to 160 C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 1.3-4.0% of the former and about 2.8-6.0% of the latter.
18.A textile fabric which has a fiameproof dressing obtained by impregnating the fabric in an aqueous liquid which contains (1) 32% by weight of a reaction mixture obtained by heating 6 parts of urea with 3 parts of orthophosphoric acid at 160 C. for 10 minutes, and, (2) 9% by weight of a condensation product of unlimited watersolubility of one mol of melamine with about 2-3 mols of formaldehyde, drying the impregnated fabric at 70 C. and after-hardening the dried fabric at C., the amounts of phosphorus and nitrogen fixed in and on the fibers being about 2.1% of the former and about 5.0% of the latter.
Reference Cited in the file of this patent UNITED STATES PATENTS 2,089,697 Groebe Aug. 10, 1937 2,305,035 Rosser Dec. 15, 1942 2,452,054 Jones et al. Oct. 26, 1948 2,464,342 Pollak Mar. 15, 1949 2,488,034 Pingree Nov. 15, 1949 2,537,840 McLean Jan. 9, 1951 FOREIGN PATENTS 638,434 Great Britain June 7, 1950
Claims (1)
1. A PROCESS FOR RENDERING TEXTILE FABRICS FLAMEPROOF, WHICH COMPRISES IMPREGNATING THE FABRIC IN AN AQUEOUS LIQUID WHICH CONTAINS (U) ABOUT 12-48% BY WEIGHT OF A REACTION MIXTURE OBTAINED BY HEATING AN EXCESS OF UREA TOGETHER WITH AN OXYGEN-CONTAINING COMPOUND OF PHOSPHORUS SELECTED FROM THE GROUP CONSISTING OF ORTHOPHOSPHORIC ACID, PYROPHOSPHORIC ACID, META-PHOSPHORIC ACID AND AMMONIUM SALTS OF THESE ACIDS, AT A HIGH TEMPERATURE, AND (2) ABOUT 2-18% BY WEIGHT OF A METHYLOLMELAMINE, THE RATIO OF COMPONENT (1) TO COMPONENT (2) RANGING FROM 3:1 TO 6:1, AND DRYING THE IMPREGNATED FABRIC AT A RAISED TEMPERATURE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US510533A US2781281A (en) | 1955-05-23 | 1955-05-23 | Flame-proofing of textiles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US510533A US2781281A (en) | 1955-05-23 | 1955-05-23 | Flame-proofing of textiles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2781281A true US2781281A (en) | 1957-02-12 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US510533A Expired - Lifetime US2781281A (en) | 1955-05-23 | 1955-05-23 | Flame-proofing of textiles |
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| Country | Link |
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| US (1) | US2781281A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2859134A (en) * | 1956-06-05 | 1958-11-04 | Wilson A Reeves | Flame resistant organic textiles and method of production |
| US2891877A (en) * | 1956-06-05 | 1959-06-23 | Leon H Chance | Flame resistant organic textiles and method of production |
| US2911325A (en) * | 1956-06-05 | 1959-11-03 | Jr George L Drake | Flame resistant organic textiles and method of production |
| US3333921A (en) * | 1963-12-06 | 1967-08-01 | Olin Mathieson | Anhydrous ammonium polyphosphate process |
| US3513114A (en) * | 1966-01-07 | 1970-05-19 | Monsanto Co | Intumescent coating compositions |
| US3617193A (en) * | 1967-09-12 | 1971-11-02 | Stevens & Co Inc J P | Flame-retardant bis(epoxyalkyl) methylphosphonate treated substrate and process therefor |
| US3632297A (en) * | 1970-03-12 | 1972-01-04 | Stevens & Co Inc J P | Process for rendering cellulose-containing fabrics durably flame-retardant by wet-curing a melamine resin and a phosphoric acid amide on the fabric |
| US3645675A (en) * | 1969-12-19 | 1972-02-29 | Monsanto Co | Ammonium pyrophosphates, processes for preparing, and uses |
| US3816212A (en) * | 1970-11-13 | 1974-06-11 | American Cyanamid Co | Process for bonding and flame proofing webs of synthetic fibers |
| US3885912A (en) * | 1972-03-30 | 1975-05-27 | Hooker Chemicals Plastics Corp | Method of rendering textiles flame retardant with phosphorus containing melamine |
| US4196260A (en) * | 1977-03-03 | 1980-04-01 | Ciba-Geigy Corporation | Process for flameproofing cellulosic fibrous material |
| US4396586A (en) * | 1980-10-15 | 1983-08-02 | Hoechst Aktiengesellschaft | Process for making long-chain ammonium polyphosphate |
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| US2089697A (en) * | 1934-06-25 | 1937-08-10 | Gen Electric | Electrical insulation and method of making the same |
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| US2859134A (en) * | 1956-06-05 | 1958-11-04 | Wilson A Reeves | Flame resistant organic textiles and method of production |
| US2891877A (en) * | 1956-06-05 | 1959-06-23 | Leon H Chance | Flame resistant organic textiles and method of production |
| US2911325A (en) * | 1956-06-05 | 1959-11-03 | Jr George L Drake | Flame resistant organic textiles and method of production |
| US3333921A (en) * | 1963-12-06 | 1967-08-01 | Olin Mathieson | Anhydrous ammonium polyphosphate process |
| US3513114A (en) * | 1966-01-07 | 1970-05-19 | Monsanto Co | Intumescent coating compositions |
| US3617193A (en) * | 1967-09-12 | 1971-11-02 | Stevens & Co Inc J P | Flame-retardant bis(epoxyalkyl) methylphosphonate treated substrate and process therefor |
| US3645675A (en) * | 1969-12-19 | 1972-02-29 | Monsanto Co | Ammonium pyrophosphates, processes for preparing, and uses |
| US3632297A (en) * | 1970-03-12 | 1972-01-04 | Stevens & Co Inc J P | Process for rendering cellulose-containing fabrics durably flame-retardant by wet-curing a melamine resin and a phosphoric acid amide on the fabric |
| US3816212A (en) * | 1970-11-13 | 1974-06-11 | American Cyanamid Co | Process for bonding and flame proofing webs of synthetic fibers |
| US3885912A (en) * | 1972-03-30 | 1975-05-27 | Hooker Chemicals Plastics Corp | Method of rendering textiles flame retardant with phosphorus containing melamine |
| US4196260A (en) * | 1977-03-03 | 1980-04-01 | Ciba-Geigy Corporation | Process for flameproofing cellulosic fibrous material |
| US4396586A (en) * | 1980-10-15 | 1983-08-02 | Hoechst Aktiengesellschaft | Process for making long-chain ammonium polyphosphate |
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