US3266918A - Viscose solutions for making flame retardant rayon - Google Patents
Viscose solutions for making flame retardant rayon Download PDFInfo
- Publication number
- US3266918A US3266918A US245653A US24565362A US3266918A US 3266918 A US3266918 A US 3266918A US 245653 A US245653 A US 245653A US 24565362 A US24565362 A US 24565362A US 3266918 A US3266918 A US 3266918A
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- US
- United States
- Prior art keywords
- viscose
- cellulose
- filaments
- phosphate
- flame retardant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
Definitions
- the present invention relates to viscose solutions for the production of flame retardant shaped bodies, such as filaments and fibers.
- afterglowresistant and flame-retardant regenerated cellulose filaments, fibers and other shaped products are formed from a viscose containing brominated triallyl phosphate, and more particularly the fully brominated material; namely, tri-(2,3 dibromopropyl) phosphate.
- the viscose and the spinning bath employed in making the shaped regenerated cellulose products of the present invention may be of conventional or known composition.
- the aging and spinnability of the viscose is apparently not aifected by the presence of the tri-(2,3 dibromopropyl) phosphate which may be added to and mixed with the viscose well in advance of spinning operations, or which may be injected into the viscose at the spinning machine, with or without being first dissolved in an alcohol or prepared as a water emulsion.
- the afterglow-resistant and flame-retardant properties of the resulting regenerated cellulose shaped products will, in general, vary with the amount of tri-(2,3 dibromopropyl) phosphate initially added to the viscose.
- To provide regenerated cellulose shaped products having selfextinguishing properties not less than about of the tri-( 2,3 dibromopropyl) phosphate, based upon the weight of the cellulose, should be incorporated into the viscose.
- Regenerated cellulose filaments and fibers which are not self-extinguishing but which do exhibit some flame retardant properties may be made by incorporating as little as 2% of the tri-(2,3 dibromopropyl) phosphate, based upon the weight of the cellulose.
- the amount of tri-(2,3 dibromopropyl) phosphate added to the viscose should perhaps not exceed more than 30% to 40%, again based upon the weight of the cellulose.
- the tri-(2,3 dibromopropyl) phosphate When incorporated into a conventional viscose, the tri-(2,3 dibromopropyl) phosphate disperses as an emulsified organic oil in a very finely divided condition. Generally, as much as to of the tri-(2,3 dibromo propyl) phosphate originally added to the viscose is retained by the finished regenerated cellulose filaments or fibers and appears as embedded oil particles which neither allect the hand, color, luster, dyeability nor launderability of such products.
- afterglow resistant and fire-retardant as used in the description and claims is intended to designate a structure which is resistant to the propagation of flame across its surface after the igniting flame has been removed (self-extinguishing) and which is also resistant to smoldering or the formation of a non-flaming combustion which manifests itself as a red glow.
- the viscose may be of conventional composition, containing from about 4% to about 10% cellulose, about 4% to about 8% caustic soda and from about 30% to about 50% carbon disulfide; based upon the weight of the cellulose.
- the modified viscose that is, the viscose containing the tri-(2,3 dibromopropyl) phosphate, may have any desired salt test at the time of spinning or extrusion.
- the viscose may contain other known additives so as to improve the physical properties of the regenerated cellulose products and to alter the fine structure of the cellulose as is commonly practiced in the industry.
- the viscose is formed in the conventional manner and either during its preparation or just prior to spinning may be further modified by the addition of a viscose or coagulation modifier.
- a viscose or coagulation modifier A large number of modifiers are known and are in use in the production of the various types of viscose rayon.
- modifiers include polyoxyalkylene glycols such as polyoxyethylene glycols, polyoxypropylene glycols and block copolymers of propylene and ethylene oxides; various amines including monoamines, diamines and polyamines such as diethylamine, dimethylamine, ethylene diamine and diethylene triamine; reaction products ozt alkylene oxides with fatty acids, fatty alcohols, fatty amines, aromatic acids, aromatic alcohols, aromatic amines, partial esters of fatty acids and polyhydric alcohols such as reaction products of ethylene oxide with lauryl alcohol, phenol, lauryl amine, glycerol monostearate, etc.; quaternary ammonium compounds and the like.
- the amount of modifier may vary from about 2% to about 5%, based on the weight of the cellulose.
- a combination of modifiers such as a monoamine and a polyoxyalkylene glycol or a polyoxyalkylene glycol ether of an aromatic alcohol or of a polyhydric alcohol wherein the glycol or ether has a molecular weight of between about 600 and about 4000 to 6000; for example, dimethylamine and a polyoxyethylene glycol or a polyethylene glycol ether of phenol or of sorbitol having a molecular weight within the stated range.
- the rnonoamine is added in an amount of from about 1.5% to 3.5% and the glycol or ether in an amount of from about 1% to 3%, both proportions being based upon the Weight of the cellulose.
- the spinning bath employed in coagulating the modified viscose may also be of conventional composition and 3 may include from about 5% to sulfuric acid, from about 3% to zinc sulfate, and from about 10% to sodium sulfate, preferably from 4% to 9% zinc sulfate and 15% to 22% sodium sulfate.
- Other metal sulfates, such as iron, manganese, nickel and the like may be present and may replace some of the zinc sulfate.
- the temperature of the spinning bath may vary from 25 C. to about 80 C., and is preferably between C. and 70 C. to insure that the resulting regenerated cellulose filaments and fibers possess good physical properties, and especially tensile strength which sutfers somewhat as compared with conventional filaments, as will be more apparent hereafter.
- the filaments may be passed through a stretch bath and stretched from about 25% to 145% during their passage through the bath.
- the stretch bath is maintained at a temperature between about 85 C. and 100 C. and may be a hot water bath or may contain 1% to 5% sulfuric acid with or without from about 1% to 4% zinc sulfate and from about 4% to 7% sodium sulfate.
- the filaments are then subjected to the usual aftertreatments which include washing and desulfurizing and, if desired, bleaching either before or after collection of the filaments.
- the filaments may or may not be provided with a yarn finish before being dried.
- the regenerated cellulose shaped products, such as filaments and fibers, formed in accordance with the present invention may be converted into fabrics using conventional processes and equipment.
- filaments and fibers are used alone or, at most, blended with only a negligible amount of conventional filaments or fibers when it is desired to preserve the full benefit of their afterglow-resistant and flame-retardant properties.
- the invention may be further illustrated by reference to the preparation of regenerated cellulose filaments from a viscose containing about 5.0% cellulose, about 6.0% caustic soda, and having a total carbon disulfide content of about 38.0%, based on the weight of the cellulose.
- the viscose solution was prepared by xanthating alkali cellulose by the introduction of 38.0% carbon disulfide based on the weight of the cellulose and churning for about 2 /2 hours. The cellulose xanthate was then dissolved in caustic soda solution.
- a second viscose was prepared which was substantially the same as that described above with the exception that no tri-(2,3 dibromopropyl) phosphate was added.
- a fabric was woven having afterglow-resistant and flame-retardant filaments, which were formed as described above, in both warp and filling, and a similar fabric was formed using the control filaments. Both yarns processed satisfactorily through warping and weaving, and the fabrics processed without difiiculty through jig scouring and frame drying. Additionally, both fabrics appeared to possess substantially the same dyeing properties.
- the above described woven fabrics were also subjected to sunshine exposure tests wherein uncovered samples and samples covered with glass were exposed to sunlight for different periods.
- the glass employed in this test was ordinary window glass of good quality having a thickness of 2.5 mm.
- the test results were as follows:
- 3,266,918 5 We claim: about 10% to 40% by weight, based on said cellulose, 1.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Description
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US245653A US3266918A (en) | 1962-12-19 | 1962-12-19 | Viscose solutions for making flame retardant rayon |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US245653A US3266918A (en) | 1962-12-19 | 1962-12-19 | Viscose solutions for making flame retardant rayon |
Publications (1)
Publication Number | Publication Date |
---|---|
US3266918A true US3266918A (en) | 1966-08-16 |
Family
ID=22927543
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US245653A Expired - Lifetime US3266918A (en) | 1962-12-19 | 1962-12-19 | Viscose solutions for making flame retardant rayon |
Country Status (1)
Country | Link |
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US (1) | US3266918A (en) |
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3412052A (en) * | 1963-10-15 | 1968-11-19 | Fmc Corp | Novel flame retardant plastic compositions |
US3455713A (en) * | 1966-07-21 | 1969-07-15 | Fmc Corp | Flame-retardant regenerated cellulose |
US3471318A (en) * | 1960-11-28 | 1969-10-07 | Nelson Silk Ltd | Finished flame-resistant textile materials |
US3505087A (en) * | 1969-04-25 | 1970-04-07 | Fmc Corp | Flame-retardant rayon containing halogenated phosphonitrilate polymer |
US3532526A (en) * | 1969-07-14 | 1970-10-06 | Fmc Corp | Flame - retardant rayon containing mercapto-phosphonitrilate polymer |
US3732683A (en) * | 1971-03-25 | 1973-05-15 | Fmc Corp | Regenerated cellulose filaments containing a flame-retardant phosphonitrilate polymer and an organic phosphate salt to reduce filament to metal friction |
US3886683A (en) * | 1970-11-27 | 1975-06-03 | Princeton Chemical Res Inc | Degradable plastic |
US3974251A (en) * | 1973-03-07 | 1976-08-10 | Hoechst Aktiengesellschaft | Production of flameproof fibers of regenerated cellulose |
US4021406A (en) * | 1973-05-21 | 1977-05-03 | M & T Chemicals Inc. | Flame retardant compositions |
US4062687A (en) * | 1975-05-30 | 1977-12-13 | Sandoz Ltd. | Phosphoric acid derivatives as flameproofing agents |
US4063883A (en) * | 1974-08-20 | 1977-12-20 | Hoechst Aktiengesellschaft | Manufacture of flame-retardant regenerated cellulose fibres |
US4148782A (en) * | 1976-05-26 | 1979-04-10 | Sandoz Ltd. | Phosphonic acid derivatives as flameproofing agents |
US20100190402A1 (en) * | 2009-01-28 | 2010-07-29 | Lenzing Aktiengesellschaft | Process for the production of flame-retardant viscose fibres |
WO2012083318A1 (en) | 2010-12-20 | 2012-06-28 | Lenzing Ag | Fireproof cellulosic man-made fibers |
EP2767180A1 (en) | 2013-02-18 | 2014-08-20 | W.L. Gore & Associates GmbH | Flame protective fabric structure |
EP3476985A1 (en) | 2017-10-27 | 2019-05-01 | Lenzing Aktiengesellschaft | Fireproof cellulosic man-made fibres |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2574515A (en) * | 1948-11-26 | 1951-11-13 | Glenn L Martin Co | Organic compounds containing phosphorus and bromine |
US2816004A (en) * | 1951-06-30 | 1957-12-10 | Monsanto Chemicals | Cellulosic solutions containing fire retardant and method of extruding |
-
1962
- 1962-12-19 US US245653A patent/US3266918A/en not_active Expired - Lifetime
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2574515A (en) * | 1948-11-26 | 1951-11-13 | Glenn L Martin Co | Organic compounds containing phosphorus and bromine |
US2816004A (en) * | 1951-06-30 | 1957-12-10 | Monsanto Chemicals | Cellulosic solutions containing fire retardant and method of extruding |
Cited By (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3471318A (en) * | 1960-11-28 | 1969-10-07 | Nelson Silk Ltd | Finished flame-resistant textile materials |
US3412052A (en) * | 1963-10-15 | 1968-11-19 | Fmc Corp | Novel flame retardant plastic compositions |
US3455713A (en) * | 1966-07-21 | 1969-07-15 | Fmc Corp | Flame-retardant regenerated cellulose |
US3505087A (en) * | 1969-04-25 | 1970-04-07 | Fmc Corp | Flame-retardant rayon containing halogenated phosphonitrilate polymer |
US3532526A (en) * | 1969-07-14 | 1970-10-06 | Fmc Corp | Flame - retardant rayon containing mercapto-phosphonitrilate polymer |
US3886683A (en) * | 1970-11-27 | 1975-06-03 | Princeton Chemical Res Inc | Degradable plastic |
US3732683A (en) * | 1971-03-25 | 1973-05-15 | Fmc Corp | Regenerated cellulose filaments containing a flame-retardant phosphonitrilate polymer and an organic phosphate salt to reduce filament to metal friction |
US3974251A (en) * | 1973-03-07 | 1976-08-10 | Hoechst Aktiengesellschaft | Production of flameproof fibers of regenerated cellulose |
US4021406A (en) * | 1973-05-21 | 1977-05-03 | M & T Chemicals Inc. | Flame retardant compositions |
US4063883A (en) * | 1974-08-20 | 1977-12-20 | Hoechst Aktiengesellschaft | Manufacture of flame-retardant regenerated cellulose fibres |
US4062687A (en) * | 1975-05-30 | 1977-12-13 | Sandoz Ltd. | Phosphoric acid derivatives as flameproofing agents |
US4148782A (en) * | 1976-05-26 | 1979-04-10 | Sandoz Ltd. | Phosphonic acid derivatives as flameproofing agents |
US20100190402A1 (en) * | 2009-01-28 | 2010-07-29 | Lenzing Aktiengesellschaft | Process for the production of flame-retardant viscose fibres |
US8070996B2 (en) * | 2009-01-28 | 2011-12-06 | Lenzing Aktiengesellschaft | Process for the production of flame-retardant viscose fibres |
WO2012083318A1 (en) | 2010-12-20 | 2012-06-28 | Lenzing Ag | Fireproof cellulosic man-made fibers |
US9988743B2 (en) | 2010-12-20 | 2018-06-05 | Lenzing Ag | Process of making flame retardant cellulosic man-made fibers |
US10577723B2 (en) | 2010-12-20 | 2020-03-03 | Lenzing Ag | Flame retardant cellulosic man-made fibers |
EP2767180A1 (en) | 2013-02-18 | 2014-08-20 | W.L. Gore & Associates GmbH | Flame protective fabric structure |
EP3476985A1 (en) | 2017-10-27 | 2019-05-01 | Lenzing Aktiengesellschaft | Fireproof cellulosic man-made fibres |
WO2019081617A1 (en) | 2017-10-27 | 2019-05-02 | Lenzing Aktiengesellschaft | Flame retardant cellulosic man-made fibres |
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Legal Events
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AS | Assignment |
Owner name: NEW ENGLAND MUTUAL LIFE INSURANCE COMPANY 501 BOYL Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: PAUL REVERE LIFE INSURANCE COMPANY THE C/O THE PAU Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: JOHN HANCOCK MUTUAL LIFE INSURANCE COMPANY JOHN HA Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: WALTER E. HELLER & COMPANY, INC., A CORP. OF DEL. Free format text: AGREEMENT WHEREBY AETNA RELEASES AVTEX FROM ALL MORTAGES AND SECURITY INTERESTS IN SAID INVENTIONS AS OF JANUARY 11,1979, AND ASSIGNS TO ASSIGNEE THE ENTIRE INTEREST IN SAID MORTAGE AGREEMENT TO ASSIGNEE;ASSIGNORS:AETNA BUSINESS CREDIT, INC., A CORP. OF N.Y.;AVTEX FIBERS, INC, A CORP. OF NY;KELLOGG CREDIT CORP., A CORP. OF DEL.;REEL/FRAME:003959/0250 Effective date: 19800326 Owner name: KELLOGG CREDIT CORPORATION A DE CORP. Free format text: AGREEMENT WHEREBY SAID HELLER AND RAYONIER RELEASES ALL MORTGAGES AND SECURITY INTERESTS HELD BY AVTEX ON APRIL 28, 1978, AND JAN. 11, 1979, RESPECTIVELY AND ASSIGNS ITS ENTIRE INTEREST IN SAID MORT-AGAGE AGREEMENT TO ASSIGNEE;ASSIGNORS:WALTER E. HELLER & COMPANY, INC. A NY CORP.;ITT RAYONIER INCORPORATED, A DE CORP.;AVTEX FIBERS INC., A NY CORP.;REEL/FRAME:003959/0350 Effective date: 19800326 Owner name: PROVIDENT ALLIANCE LIFE INSURANCE COMPANY C/O THE Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: BALBOA INSURANCE COMPANY C/O THE PAUL REVERE EQUIT Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: WESTERN AND SOUTHERN LIFE INSURANCE COMPANY THE C/ Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 |