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US4123574A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for flame retarding cellulosics

Assignee: Occidental Chemical Corp
•
Filing: 1976-09-02
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Granted: 1978-10-31
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Expires: 1996-09-02
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Abstract

Abstract An improved process for imparting durable flame retardancy to textile materials wherein said material is impregnated with a solution having a poly(hydroxymethyl) phosphonium cation content of from about 10 to about 60 percent by weight, dried to a moisture content of from about 0 to about 8 percent, aerated by passing air through the dried material, cured by polymerizing the monomer on and in the cellulose material with exposure in an enclosed chamber to an atmosphere containing gaseous ammonia and thereafter contacting with water, the improvement comprising, impregnating said material with a poly(hydroxymethyl) phosphonium cation containing solution and a basic catalyst, said solution having a pH of from about 2 to about 9, and after contacting said material with said water, further exposing said material to an atmosphere containing gaseous ammonia.

Inventors

  • 👤 George M. Wagner

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-06 17:04
CPC Classifications
D; D06; D06M; D06M15/00; D06M15/19; D06M15/37; D06M15/667; D06M13/00; D06M13/244; D06M13/282; D06M13/322; D06M13/46; D06M15/673; Y; Y10; Y10S; Y10S428/00; Y10S428/92; Y10S428/921; Y10T; Y10T442/00; Y10T442/20; Y10T442/2631; Y10T442/2672; Y10T442/2689

Claims Analysis

Total Claims: 24
Claim 1
Independent Claim 229 words
A process for rendering cellulosic-containing materials durably flame retardant comprising: a. Impregnating a cellulose-containing material with a flame retarding solution comprising from about 10 to about 40 percent by weight poly(hydroxymethyl) phosphonium cation and from about 0.5 to about 20 percent by weight of a basic catalyst, said solution having a pH of from about 2 to about 9; b. Drying the impregnated material at a temperature of less than 125° C., to a moisture content of from about 0 to about 8 percent by weight; c. Aerating the dried material by directing a current of air from about 1,000 to about 3,000 cubic feet per minute through the dried material to eliminate any formaldehyde formed in said drying step; d. Exposing the aerated material in an enclosed chamber for a period of at least about 5 seconds but less than about 60 seconds to an atmosphere containing at least about 50 percent by volume of gaseous ammonia to cure the phosphorus containing resin in and on the material; e. Contacting the material with water to a wet pick-up of from about 10 to about 60 percent by weight to render the material durably flame retardant; and f. Further exposing the water contacted material for a period of from about 1 to about 10 seconds to an atmosphere containing at least about 50 percent by volume of gaseous ammonia.
Claim 2
Dependent Claim 229 words
A process for rendering cellulosic-containing materials durably flame retardant comprising: a. Impregnating a cellulose-containing material with a flame retarding solution comprising from about 10 to about 40 percent by weight poly(hydroxymethyl) phosphonium cation and from about 0.5 to about 20 percent by weight of a basic catalyst, said solution having a pH of from about 2 to about 9; b. Drying the impregnated material at a temperature of less than 125° C., to a moisture content of from about 0 to about 8 percent by weight; c. Aerating the dried material by directing a current of air from about 1,000 to about 3,000 cubic feet per minute through the dried material to eliminate any formaldehyde formed in said drying step; d. Exposing the aerated material in an enclosed chamber for a period of at least about 5 seconds but less than about 60 seconds to an atmosphere containing at least about 50 percent by volume of gaseous ammonia to cure the phosphorus containing resin in and on the material; e. Contacting the material with water to a wet pick-up of from about 10 to about 60 percent by weight to render the material durably flame retardant; and f. Further exposing the water contacted material for a period of from about 1 to about 10 seconds to an atmosphere containing at least about 50 percent by volume of gaseous ammonia.
Claim 3
Dependent Claim 25 words
The process of claim 1 wherein said basic catalyst is at least one selected from the group consisting of carbonates, bicarbonates, acetates, phosphates and metasilicates.
Claim 4
Dependent Claim 31 words
The process of claim 2 wherein said basic catalyst is at least one selected from the group comprising sodium carbonate, sodium bicarbonate, potassium carbonate, mono-sodium phosphate, disodium phosphate and tri-sodium phosphate.
Claim 5
Dependent Claim 20 words
The process of claim 1 wherein said flame retarding solution has a pH of from about 4.0 to about 8.1.
Claim 6
Dependent Claim 19 words
The process of claim 1 wherein said water treatment step (e) occurs within the enclosed chamber of step (d).
Claim 7
Dependent Claim 20 words
The process of claim 1 wherein said ammonia atmosphere exposure step (f) occurs within the enclosed chamber of step (d).
Claim 8
Dependent Claim 24 words
The process of claim 1 wherein water treatment step (e) and ammonia atmosphere exposure step (f) occur within the enclosed chamber of step (d).
Claim 9
Dependent Claim 27 words
The process of claim 1 wherein water treatment step (e) and ammonia atmosphere exposure step (f) occur within a separate enclosed chamber from that of step (d).
Claim 10
Dependent Claim 17 words
The process of claim 1 wherein water is sprayed on the material in water treatment step (d).
Claim 11
Dependent Claim 20 words
The process of claim 1 wherein the material is passed through a trough of water in water treatment step (d).
Claim 12
Dependent Claim 15 words
The process of claim 10 wherein the material is squeezed after passing through said trough.
Claim 13
Dependent Claim 22 words
The process of claim 1 wherein the material is water treated by means of a kiss roll in water treatment step (d).
Claim 14
Dependent Claim 14 words
The process of claim 12 wherein water pick-up is regulated by a doctor blade.
Claim 15
Dependent Claim 27 words
The process of claim 1 wherein said cellulosic material is selected from the group consisting of cotton, rayon, paper, jute, ramie, wood, and mixtures and blends thereof.
Claim 16
Dependent Claim 19 words
The process of claim 14 wherein said cellulosic material is blended with proteinaceous fibers, synthetic fibers and mixtures thereof.
Claim 17
Dependent Claim 22 words
The process of claim 15 wherein said proteinaceous fiber is selected from the group consisting of wool, mohair, alpaca and mixtures thereof.
Claim 18
Dependent Claim 23 words
The process of claim 15 wherein said synthetic fiber is selected from the group consisting of polyester, nylon, acrylics, acetate and mixtures thereof.
Claim 19
Dependent Claim 29 words
The process of claim 1 wherein said poly(hydroxymethyl) phosphonium cation is prepared by reacting an aqueous solution of poly(hydroxymethyl)phosphonium salt with up to an equivalent quantity of a base.
Claim 20
Dependent Claim 29 words
The process of claim 18 wherein said poly(hydroxymethyl) phosphonium salt is selected from the group consisting of halides, sulfates, acetates, phosphates, carboxylates, oxalates, lactates, formates, sulfonates and mixtures thereof.
Claim 21
Dependent Claim 11 words
The process of claim 19 wherein said salt is tetrakis(hydroxymethyl)phosphonium sulfate.
Claim 22
Dependent Claim 53 words
The process of claim 1 wherein said flame retarding solution comprises a reaction product of a poly(hydroxymethyl)phosphonium cation with a nitrogen containing material selected from the group consisting of urea, guanidines, substituted ureas, melamines, amino and amido function containing organic materials and the reaction product of the said nitrogen containing materials with aldehydes.
Claim 23
Dependent Claim 10 words
The process of claim 21 wherein said aldehyde is formaldehyde.
Claim 24
Dependent Claim 14 words
The process of claim 1 wherein said cellulosic containing material is a cotton/polyester blend.

References Cited (Backward Citations)

US2772188A Cited
US3096201A Cited
US3310419A Cited
US3607356A Cited
US4068026A Cited
US3919439A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-10-30 1982-05-01 1982-10-31 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-10-30 1986-05-01 1986-10-31 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-10-30 1990-05-01 1990-10-31 $7700.00 Window Closed / Lapsed

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