US2780566A - Process for water and flame proofing textiles - Google Patents
Process for water and flame proofing textiles Download PDFInfo
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- US2780566A US2780566A US550172A US55017255A US2780566A US 2780566 A US2780566 A US 2780566A US 550172 A US550172 A US 550172A US 55017255 A US55017255 A US 55017255A US 2780566 A US2780566 A US 2780566A
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- water
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- fibrous material
- radiation
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 16
- 238000000034 method Methods 0.000 title claims description 10
- 239000004753 textile Substances 0.000 title description 11
- 239000002657 fibrous material Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 25
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 21
- 230000005855 radiation Effects 0.000 claims description 19
- 229940046892 lead acetate Drugs 0.000 claims description 12
- 239000005871 repellent Substances 0.000 claims description 12
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 11
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 10
- 229960004011 methenamine Drugs 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 7
- 230000002940 repellent Effects 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 claims description 3
- 239000000463 material Substances 0.000 description 19
- 238000011282 treatment Methods 0.000 description 15
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 8
- 229940010048 aluminum sulfate Drugs 0.000 description 8
- 239000004744 fabric Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000000835 fiber Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 239000003063 flame retardant Substances 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 210000002268 wool Anatomy 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 2
- 229940009827 aluminum acetate Drugs 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002964 rayon Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229960001040 ammonium chloride Drugs 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000004900 laundering Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- 125000005402 stannate group Chemical group 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
-
- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/57—Sulfates or thiosulfates of elements of Groups 3 or 13 of the Periodic Table, e.g. alums
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
-
- 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
-
- 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
- Y10T442/2033—Coating or impregnation formed in situ [e.g., by interfacial condensation, coagulation, precipitation, etc.]
-
- 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
- Y10T442/2164—Coating or impregnation specified as water repellent
- Y10T442/2197—Nitrogen containing
-
- 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
- Y10T442/2721—Nitrogen containing
Definitions
- This invention relates to improved water-andflame proof fibrous materials and more particularly to' amethod for the production of waterproof and flame-proof textile materials.
- the prior treatments are well known to cause deterioration of cellulosic materials, due to light radiation in the presence of stannic oxide and some treatments have incorporated certain pigments to prevent this action.
- waterrepellent fibrous materials such as water-repellent. cotton, linen, silk, wool, rayon and similar textiles as well as felt, canvas, paper and the like.
- Another object is the production of water-repellent fibrous materials wherein the pores of the materials are not obstructed by undesired deposits.
- a further object is the production of fiame-and-water repellent textiles and similar fibrous materials having the fibers completely water-repellent throughout the body of the fabric.
- Yet another object is the provision of a rapid and economical treatment whereby textiles and similar fibrous materials are rendered both water-proof or water-repellent and fire-proof or fire-retardant.
- a fibrous material is treated with an aqueous mixture of aluminum sulfate, lead acetate and hexamethylenetetramine, thereafter exposing the thus-treated material to black rays of the infra-red radia- L FQFNGF 2,780,566 btented Feb. 5, 1957 tion.
- this invention contemplates the further treatment of the textile or other fibrous material with a soluble tinsalt while again exposing. the treated material to infra-red radiation, whereby a material is produced which is both water repe'llent and fire-resistant or fire-proof.
- a hot solution of lead acetate is admixed with a hot solution of aluminum sulfate;
- a precipitate is formed as it is well known that lead sulfate is not extensively soluble inhot water, but it is more soluble in hot water than: in cold Water, and more soluble in aluminum acetate solutions than it is in water.
- a small amount of hexamethylenetetramine is added which immediately dissolves that part of the precipitate remaining. in suspension.
- the then clear solution is separated from that part of the precipitate that had previously settled out.
- a suitable fibrous substance is then treated with the solution and thereafter exposed-to the black rays of the. infra-red beam.
- fibrous material of superior properties in which pores of each fibre are impregnated with-'the' treating agents, which material can be repeatedly laundered or'dry-cleaned'without losing its water-repellent and flame retardant characteristics.
- Example I 325 grams of lead acetate are dissolved in one. half of a gallon of boiling water, preferably distilled Water, and
- Urotropin is dissolved in the previously prepared turbid mixture. The mixture then becomes clear, and a small amount of residue which. settles on the bottom isv discarded.
- the solution is filtered through a cloth and into this clear solution, is immersed the textile material'- to be treated, for example a khaki uniformv material of cotton, and the immersed material is exposed to the radiation from a suitable infra-red lamp, preferably for a time about fifteen to thirty minutes.
- the preparation of the solution and textile material is preferably carrie'ci' out in adark room, with of course, the exception of the infra-red treatment.
- the treatedmaterial is next withdrawn from the treatment solution,-and again exposed to infra-red radiation whereupon. it becomes water-repellent.
- a thin twill such as that used in army uniforms may be treated in twelve to fifteen minutes, while a heavy wool cloth, such as that used in army overcoats will take from fifteen to twenty-five minutes, twenty minutes being the preferred time.
- the invention is not limited to the specific material there described, but I can as well water-proof and flame-proof such absorbent fibrous materials as wool, silk, rayon (including regenerated cellulose and acetate rayon) and such synthetic polymeric fibrous materials as are absorbent.
- infra-red radiation is meant the range of radiation lighting beyond the visible spectrum on the red side, which has a Wave length shorter than the socalled short radio waves; The wave lengths Will depend upon the temperature of the filament in the infra-red lamps and it is well recognized that radiation of various wave lengths produce different chemical reactions. Some effect is obtained by any infra-red lamp, but it is preferred that the infra-red lamp having a filament temperature in the neighborhood of 1400 C. be used.
- the proportion of lead acetate can be varied between about one and five parts by weight to between about three and seven parts by weight of aluminum sulfate.
- the treatment mixture can be made more or less dilute than specified in the example, and I have found that a total treatment solution of between about one-half and five gallons can be employed using the stated proportions of lead acetate and aluminum sulfate.
- the quantity of hexamethylenetetramine employed as a catalyst is in general very small, although a large excess does not appear to do substantial harm to the resultant treated fabric.
- the stated proportion of five grains of catalyst to one gallon of prepared solution has beefi found very satisfactory, and as little as one grain produces some effect.
- My invention is eminently suitable for Water-and-flame proofing of uniforms, clothing, equipment, awnings, theater scenery and curtains, tents, upholstery, parachutes, balloon cloth, drapes, rugs, mattresses and many other fibrous materials too numerous to mention.
- One of the advantages of the fibrous material waterand-fiame-proofed, in accordance with this invention, is that there are no apparent changes in color, softness, and flexibility of the resulting fibrous materials.
- a process for the production of a Water repellent and flame-retardant fibrous material which comprises treating a fibrous material with a hot aqueous solution of a mixture of aluminum sulfate, lead acetate and hexamethylenetetramine, and exposing the thus treated material to infra-rec radiation during the treatment, and subsequently thereto with infra-red radiation.
- a process for the production of a water repellent and flame retardant fibrous material which comprises treating a fibrous material with a heated aqueous solution resulting from mixing solutions of aluminum sulphate, lead acetate and hexamethylene tetramine, and separating the precipitate, and exposing during treating the fibrous material with the black rays of the infra-red radiation.
- a water proof and flame retardant soft fibrous material having Within the pores of the fiber a reaction product of aluminum sulphate, lead acetate and hexamethylene tetramine.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
lflh l ti United! assignor to John P. Wetherill, Charles M. Trammell, and Alexander M. L. de Luxembourg, trustees No Drawing. Application November 30, 1955, S erialNo. 550,172
Claims. (Cl. 117-93) This invention relates to improved water-andflame proof fibrous materials and more particularly to' amethod for the production of waterproof and flame-proof textile materials.
Heretofore various solutions of metallic salts have been used for flame-proofing and water-proofing fibrous materials. Lead acetate, calcium acetate and ammonium chloride solution and mixtures thereof have been usedfor many years. A later development having the same genera-l objects included theuse of stannate as apreliminary impregnating material, followed by the use of a solution of a soluble salt; that would react therewith, that would produce a precipitate. A still later development also required a double impregnation, first with a solutionof aluminum, nickel, chromium, lead etc. and then treating with a solution of amineniumhydroxi'de toprecipitate the hydroxide of the metal. A development abroad, approximately fift'y years ago, describes the treatment of a textile material with a solution of metallic salts and then with a second solution capable of acting on this metallic salt to produce a precipitate.
It has long been recognized that all of these processes depend on the production of an insoluble compound ad-- jac'ent to the fibers composing the substance so treated, and render the same harsh and non-yielding to the touch and have universally proven unsatisfactory.
It is an object of the present invention to treat a fibrous material with a solution of a soluble substance so as to incorporate this substance within the fiber cells andthen treat in such a manner as to cause this substance to render the cloth permanently water-proof and flameproof. The prior treatments are well known to cause deterioration of cellulosic materials, due to light radiation in the presence of stannic oxide and some treatments have incorporated certain pigments to prevent this action.
it is another object of this invention toproduce waterrepellent fibrous materials, such as water-repellent. cotton, linen, silk, wool, rayon and similar textiles as well as felt, canvas, paper and the like.
Another object is the production of water-repellent fibrous materials wherein the pores of the materials are not obstructed by undesired deposits.
A further object is the production of fiame-and-water repellent textiles and similar fibrous materials having the fibers completely water-repellent throughout the body of the fabric.
Yet another object is the provision of a rapid and economical treatment whereby textiles and similar fibrous materials are rendered both water-proof or water-repellent and fire-proof or fire-retardant.
Other and further objects will be apparent or will appear as the ensuing description proceeds.
The foregoing objects are accomplished in accordance with this invention wherein a fibrous material is treated with an aqueous mixture of aluminum sulfate, lead acetate and hexamethylenetetramine, thereafter exposing the thus-treated material to black rays of the infra-red radia- L FQFNGF 2,780,566 btented Feb. 5, 1957 tion. Additionally, this invention: contemplates the further treatment of the textile or other fibrous material with a soluble tinsalt while again exposing. the treated material to infra-red radiation, whereby a material is produced which is both water repe'llent and fire-resistant or fire-proof.
In the practice of my invention a hot solution of lead acetate is admixed with a hot solution of aluminum sulfate; A precipitate is formed as it is well known that lead sulfate is not extensively soluble inhot water, but it is more soluble in hot water than: in cold Water, and more soluble in aluminum acetate solutions than it is in water. Thereafter, a small amount of hexamethylenetetramine is added which immediately dissolves that part of the precipitate remaining. in suspension. The then clear solution is separated from that part of the precipitate that had previously settled out. A suitable fibrous substance is then treated with the solution and thereafter exposed-to the black rays of the. infra-red beam. There results by this treatment a fibrous material of superior properties in which pores of each fibre are impregnated with-'the' treating agents, which material can be repeatedly laundered or'dry-cleaned'without losing its water-repellent and flame retardant characteristics. The
textile thenbe'comes fiam'e proof for about four years and is not. thereafter'damaged by visible light rays as are the products of the prior art.
lncarrying out my invention, I have found the procedure of the following example to give very satisfactory results. In the example", parts and proportions are by weight unless otherwise designated.
. Example I] 325 grams of lead acetate are dissolved in one. half of a gallon of boiling water, preferably distilled Water, and
admixed with a solution of grams of aluminum sul fate in one-half gallon of'hot water, preferably'distilled' water. The resulting turbid solution or mixture has'the color and consistency of milk. Thereafter, a five grain tablet of hexamethylenetetramine, sold under the trade.
name Urotropin, is dissolved in the previously prepared turbid mixture. The mixture then becomes clear, and a small amount of residue which. settles on the bottom isv discarded. The solution is filtered through a cloth and into this clear solution, is immersed the textile material'- to be treated, for example a khaki uniformv material of cotton, and the immersed material is exposed to the radiation from a suitable infra-red lamp, preferably for a time about fifteen to thirty minutes. The preparation of the solution and textile material is preferably carrie'ci' out in adark room, with of course, the exception of the infra-red treatment. The treatedmaterial is next withdrawn from the treatment solution,-and again exposed to infra-red radiation whereupon. it becomes water-repellent.
In treating, the cloth as set forth above, consideration must be given to the weight of the cloth. A thin twill, such as that used in army uniforms may be treated in twelve to fifteen minutes, while a heavy wool cloth, such as that used in army overcoats will take from fifteen to twenty-five minutes, twenty minutes being the preferred time.
Although the example describes the treatment of a cotton khaki uniform material, the invention is not limited to the specific material there described, but I can as well water-proof and flame-proof such absorbent fibrous materials as wool, silk, rayon (including regenerated cellulose and acetate rayon) and such synthetic polymeric fibrous materials as are absorbent.
Although I have secured superior results by the employment of a solution of lead acetate admixed with aluminum sulfate, and believe that this particular reaction mixture possesses peculiar virtues, solutions of aluminum acetate and hexamethylenetetramine otherwise prepared can also be employed.
I have found that the small amount of hexamethylenetetramine employed appears to act as a unique catalytic agent in aiding the fixation of the chemicals on the fibrous materials under the influence of the black rays of the infra-red radiation. Other amino compounds such as urea and ethylamine, may be used in catalytic quantities with somewhat inferior results.
I have found that in general the preparation of the treatment mixture should be carried out in the dark or with red bulb lights, that is to say while excluding sunlight and artificial light, and that the exclusion of light during the initial preparation and treatment facilitates the production of a superior product.
Although any suitable source of infra-red radiation may be employed I have found that most excellent results are secured when the radiation is beamed upon the textile fibers or other materials undergoing treatment. By the expression in infra-red radiation is meant the range of radiation lighting beyond the visible spectrum on the red side, which has a Wave length shorter than the socalled short radio waves; The wave lengths Will depend upon the temperature of the filament in the infra-red lamps and it is well recognized that radiation of various wave lengths produce different chemical reactions. Some effect is obtained by any infra-red lamp, but it is preferred that the infra-red lamp having a filament temperature in the neighborhood of 1400 C. be used. This will produce radiation of about one micron in wave length, and will produce results better than that obtainable by a 7- micron radiation. Much higher frequency may be used than the one micron radiation and has been found to work satisfactorily to produce the necessary chemical reaction between the various constituents of the treating solution.
While I have found that three parts of lead acetate is a preferred proportion to employ with five parts by weight of aluminum sulfate, these proportions can be varied considerably to secure some improvement in water-repellent properties. For example, the proportion of lead acetate can be varied between about one and five parts by weight to between about three and seven parts by weight of aluminum sulfate. The treatment mixture can be made more or less dilute than specified in the example, and I have found that a total treatment solution of between about one-half and five gallons can be employed using the stated proportions of lead acetate and aluminum sulfate. The quantity of hexamethylenetetramine employed as a catalyst is in general very small, although a large excess does not appear to do substantial harm to the resultant treated fabric. The stated proportion of five grains of catalyst to one gallon of prepared solution has beefi found very satisfactory, and as little as one grain produces some effect.
By the practice of my invention, new water and flameproof articles are prepared wherein the entire fiber is rendered water-and-flame proof and not merely the outer surface thereof.
My invention is eminently suitable for Water-and-flame proofing of uniforms, clothing, equipment, awnings, theater scenery and curtains, tents, upholstery, parachutes, balloon cloth, drapes, rugs, mattresses and many other fibrous materials too numerous to mention.
From the foregoing, it is apparent that I have provided new water-repellent fibrous materials and a simple, economical process for their preparation. The materials treated by my invention are stable to repeated laundering and dry cleaning, and my process largely involves only the consumption of cheap and readily obtainable chemicals.
One of the advantages of the fibrous material waterand-fiame-proofed, in accordance with this invention, is that there are no apparent changes in color, softness, and flexibility of the resulting fibrous materials.
Since many apparently differing embodiments of the invention will occur to one skilled in the art, various changes can be made in the details illustrated and described without departing from the spirit and scope of the invention.
What is claimed is:
1. A process for the production of a Water repellent and flame-retardant fibrous material, which comprises treating a fibrous material with a hot aqueous solution of a mixture of aluminum sulfate, lead acetate and hexamethylenetetramine, and exposing the thus treated material to infra-rec radiation during the treatment, and subsequently thereto with infra-red radiation.
2. A process as claimed in claim 1, wherein the infra red radiation has a wave length of about 1 micron, the material being exposed for approximately 12 to minutes.
3. A process for the production of a water repellent and flame retardant fibrous material, which comprises treating a fibrous material with a heated aqueous solution resulting from mixing solutions of aluminum sulphate, lead acetate and hexamethylene tetramine, and separating the precipitate, and exposing during treating the fibrous material with the black rays of the infra-red radiation.
4. A process as claimed in claim 3 wherein the infrared radiation has a wave length of about 1 micron.
5. A water proof and flame retardant soft fibrous material having Within the pores of the fiber a reaction product of aluminum sulphate, lead acetate and hexamethylene tetramine.
References Cited in the file of this patent UNITED STATES PATENTS 2,343,186 Hopkinson Feb. 29, 1944 2,520,103 Loukomsky Aug. 22, 1950 2,542,064 Tilden Feb. 20, 1951
Claims (1)
- 3. A PROCESS FOR THE PRODUCTION OF A WATER REPELLENT AND FLAME RETARDENT FIBROUS MATERIAL, WHICH COMPRISES TREATING A FIBROUS MATERIAL WITH A HEATED AQUEOUS SOLUTION RESULTING FROM MIXING SOLUTIONS OF ALUMINUM SULPHATE, LEAD ACETATE AND HEXAMETHYLENE TETRAMINE, AND SEPARATING THE PRECIPITATE, AND EXPOSING DURING TREATING THE FIBROUS MATERIAL WITH THE BLACK RAYS OF THE INFRA-RED RADIATION.
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US550172A US2780566A (en) | 1955-11-30 | 1955-11-30 | Process for water and flame proofing textiles |
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US550172A US2780566A (en) | 1955-11-30 | 1955-11-30 | Process for water and flame proofing textiles |
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US2780566A true US2780566A (en) | 1957-02-05 |
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US550172A Expired - Lifetime US2780566A (en) | 1955-11-30 | 1955-11-30 | Process for water and flame proofing textiles |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3475199A (en) * | 1966-04-14 | 1969-10-28 | Tri Wall Containers Inc | Fire-retardant coating |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2343186A (en) * | 1940-08-12 | 1944-02-29 | Hopkinson Harry | Fireproofing plasticizers |
US2520103A (en) * | 1949-02-15 | 1950-08-22 | American Cyanamid Co | Method of treating fibrous cellulosic materials to impart flame resistance thereto, compositions therefor, and products thereof |
US2542064A (en) * | 1946-05-10 | 1951-02-20 | Permafuse Corp | Apparatus for making means to attach friction material to brake shoes and the like |
-
1955
- 1955-11-30 US US550172A patent/US2780566A/en not_active Expired - Lifetime
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2343186A (en) * | 1940-08-12 | 1944-02-29 | Hopkinson Harry | Fireproofing plasticizers |
US2542064A (en) * | 1946-05-10 | 1951-02-20 | Permafuse Corp | Apparatus for making means to attach friction material to brake shoes and the like |
US2520103A (en) * | 1949-02-15 | 1950-08-22 | American Cyanamid Co | Method of treating fibrous cellulosic materials to impart flame resistance thereto, compositions therefor, and products thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3475199A (en) * | 1966-04-14 | 1969-10-28 | Tri Wall Containers Inc | Fire-retardant coating |
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