![]() Method of obtaining fire-proof fibre
专利摘要:
A method for producing a fireproof fiber by mixing acrylonitrile copolymers with a sulfonic monomer and vinylidene chloride in a solvent, and introducing antimony oxide in the resulting solution. particles of 10–20 µm, by molding into an aqueous precipitation bath containing the indicated solvent, by rinsing, drawing and drying, characterized in that, in order to increase the stability of the molding J in fire resistance and glossiness of the fiber, a mixture solution is used a, containing 96.07 mol.% acrylonitrile and 3.93 mol.% on the trivium salt of 2-acrylamido-2-propanesulfonic acid with a copolymer containing 69.09 mol.% acrylonitrile and 30.91 mol.% vinylidene chloride at a ratio of 20:80 in dimethylforma mamide, and antimony dioxide is introduced into the solution in 6.76% colloidal dispersion in a water-dimethylformamide solvent containing 30% of water at 60 ° C. 公开号:SU1128845A3 申请号:SU802891155 申请日:1980-03-07 公开日:1984-12-07 发明作者:Каццаро Джорджо;Салан Антонио;Кавалларо Антонио;Матера Джанкарло 申请人:Сниа Вискоза Сочиета Национале Индустрия Аппликациони Вискоза С.П.А (Фирма); IPC主号:
专利说明:
IN9 00 00 4 Invention 1 relates to the field of technology for producing modified acrylic fibers, characterized by high gloss, high stability: during heat treatments with high flame retardancy. antimony oxide solution, molded into an aqueous precipitation bath containing the indicated solvent, washing, extracting and flj essence. However, in the fiber production process, it is necessary to frequently change the spinnerets, as occurs. blocking them, a significant amount of the fibers are glued together and cuts, which leads to twisting in the subsequent processing stages, the fiber is obtained opaque or matte with the limiting oxygen index (PKI) -26 with a gloss degree of 83. The purpose of the invention is to increase the stability of the molding, The goal is achieved by the fact that according to the method of obtaining flame-retardant in the fiber by mixing copolymers of acrylonitrile with sulfonic monomer 1I with vinylidene chloride, in a solvent, by introducing nny solution of antimony oxide particle size 10-20 microns in molding. an aqueous precipitation bath containing the indicated solvent, washing, extracting. and dryly using a 25% solution of the mixture with; a polymer containing 96.07 mol,% acrylonitrile and 3.93 mol,% sodium salt 2-acrylamido-2-propanesulfone acids with a copolymer containing 69.09 mol,% acrylonitrile and: 30.91 mol, vinylidene chloride at a ratio of 20:80 in dimethylformamide, and antimony dioxide is introduced into the solution in the form of 6.75% colloidal dispersion in water dimethylformamide solvent containing 30% water at 60 ° C. Example, Two double c} 1 C 1 -mears are obtained, designated as L and B, the first from acrylonitrile (AKHj and the 2-acrylamido-2-propanesulfonic acid sodium salt of the formula CH CH- € 0H-C (CH,) 2.-CH -SO Na. Which is hereinafter referred to as SAMPS for simplicity, the latter from AKN and 45I vinylidene chloride. The conditions for preparing these polymers and the preparation of the paste are shown below: The composition of the mixture to be polymerized, weight, h, , 20 24.75 SAMPS,% 4.80,% - 20.25 NgO,% 2.00, 6.00 DMF,% 66.00 49.00 Total percent of monomers in the mixture32 45 Weight percent of various comonomers included in composition according to of the existing polymerizable mixtures Type of copolymer A B ACN,% 85 55,% - 45 SAMPS,% 15 Polymerization conditions Type of copolymer A B Temperature, s 67 52 Duration, hours 11 13 AIBI (azoisobutyronitrile) catalyst,% 0.027 Stabilizer, X 0.015 1) {: mixture characteristics after polymerisation is completed Copolymer A B Dry residue,% 21 19.1 Percentage of monomers in polymer65, 6 42.4 Percentage of SAMPS conversion: I to copolymer 65.6 Polymer composition Copolymer B AKN, wt.% 85 , 44 44 AKN, mole,% 96.07 69j09 SAMPS, weight,% 15 SAMPS, mole,% 3.93 CHj, CCl2, weight,% - 45 ml.% - 30.91 The final viscous solution for the preparation is obtained laugh after the removal of unreacted monomers, 0 hours, of polymer solution A and 80 hours. In a conventional static or dynamic mixer used for highly viscous polymer solutions, this sequence of distillation and mixing is: reverse, To a solution for a series, thus obtained containing approximately 25Z of the olimer, the colloid suspension is added. the following composition, wt.%: DMF 63,25. This dispersion is obtained by adding 13.5 parts by weight. aqueous colloidal -dispersion of 50% SbnOj (particle size 10-20 µm1 to 86.5 parts by weight of a solution containing 26.9% water and 73.1% DMF. The said dispersion is then added to a paste, which is heated to about 75% C, using a turbine-type mechanical mixer. The dispersion is also heated to about just before adding it to the mixer. The resulting paste has the following composition, wt%: Polymer 22.5 HjO3 SbjOj 0.675 DMF 73.825 This viscous solution is formed in a known manner, in a 12–13 bath, with a constant water and daph content of 50 and 50%, respectively; The button is collected, washed with water, drawn to a draw ratio of 5.5, dried, and a percent is carried out in accordance with known methods for treating acrylic fiber. The following fiber is obtained from tava, wt.%: Vinylidene chloride, which has a PCD of 30% oxygen, gr | gloss glossiness 93. 5 Comparative example. The fiber is produced according to example 1, however, the average particle diameter of SbgOc is less than 20 µm, and the polymer composition (concentration 10.5%) has the following composition, wt%: Acrylonitrile 82.5 Vinilidene chloride 9j2. Methacrylate 8 Methyl sodium sulfonate 0.3. The dies made of Au / Pt 70/30 alloy with 5000 holes 150 μm in diameter were used. The stretching conditions were similar. The difficulties that had to be. to be encountered when drawn into a coagulation bath, caused mainly by breaking of the fibers, their twisting and sticking. Checking the nozzles revealed that about 5% of the holes were clogged. With a fiber number of 3.2, calculated from the number of revolutions of the feed hoop, the average value of the fiber number was actually 3.6. Dies required frequent replacement (approximately every 10-11 hours). The oxygen index of the fiber obtained was 26, and the degree of glossiness (gloss) measured with a Zeiss photogoniometer was 83. Thus, using the invention improves the stability of fiber spinning, degree of fire resistance and glossiness.
权利要求:
Claims (1) [1] METHOD FOR PRODUCING FIRE-RESISTANT FIBER by mixing copolymers of acrylonitrile with a sulfone monomer and vinylidene chloride in a solvent, introducing antimony oxide into the resulting solution. particles of 10-20 μm, by molding in an aqueous precipitation bath containing the specified solvent, by washing, drawing and drying, characterized in that, in order to increase the molding stability * degree of fire resistance and gloss of the fiber, a 25% copolymer mixture solution is used, containing 96.07 mol% .-% acrylonitrile and 3.93 mol% sodium salt of 2-acrylamido-2-propanesulfonic acid with a copolymer containing 69.09 mol% acrylonitrile and 30.91 mol% vinylidene chloride in a ratio of 20 : 80 in dimethylformamide, and antimony dioxide is introduced into the solution in the form of: 6.76% -N colloidal dispersion in a water-dimethylformamide solvent containing 30% water at 60 ° C. SU "1128845
类似技术:
公开号 | 公开日 | 专利标题 SU1128845A3|1984-12-07|Method of obtaining fire-proof fibre US3502607A|1970-03-24|Art of making dyeable polyacrylonitrile products US3288888A|1966-11-29|Acrylonitrile vinylidene chloride polymer blend compositions US4287148A|1981-09-01|Process for producing glossy fibres of the modacrylic type having reduced inflammability KR880000287B1|1988-03-19|Acrylic wef spinning process US3607817A|1971-09-21|Production of dyeable polyacrylonitrile compositions and articles US2970977A|1961-02-07|Method of preparing an acrylonitrile polymer inter-linked by a metal alcoholate, composition thereof, and filament therefrom CA1079916A|1980-06-24|Gloss-stable modacrylic fibres and a process for their production US3706707A|1972-12-19|Adducts of a polymer of a cyclic ether and a sultone US2868756A|1959-01-13|Acrylonitrile-containing terpolymers, composition thereof, and textiles made therefrom US3736304A|1973-05-29|Production of polymers comprising acrylonitrile and a tertiary amino alkyl ester of an unsaturated acid US2719136A|1955-09-27|Compositions from polymerizing acrylonitrile in the presence of maleic anhydride copolymers US3366711A|1968-01-30|Polymers for acrylic fibers having improved dyeability US2541011A|1951-02-13|Ternary interpolymers comprising acrylonitrile and fumaric acid US2571777A|1951-10-16|Acrylonitrile polymer mixed with copolymer of vinyl acetate and isopropenyl acetate US3507823A|1970-04-21|Art of preparing dyeable polyacrylonitrile products US3784511A|1974-01-08|Color stabilization of fibers from acrylonitrile polymers US4226824A|1980-10-07|Process for spinning modacrylic fiber having high retraction and reduced inflammability US3475364A|1969-10-28|Art of producing dyeable acrylonitrile copolymer compositions and articles US2697088A|1954-12-14|Acrylonitrile polymer mixed with formylated polyvinyl alcohol CA1053835A|1979-05-01|Modacrylic filaments with improved coloristic properties US3402235A|1968-09-17|Manufacture of shaped articles from acrylonitrile polymers by wet spinning US3376276A|1968-04-02|Low shrinkage modacrylic interpolymer US3939120A|1976-02-17|Acrylonitrile copolymers suitable for making flame-resisting fibers US3887676A|1975-06-03|Polyvinylchloride graft vinyl chloride onto amido backbone and polyvinyl alcohol as film or fiber
同族专利:
公开号 | 公开日 DE3008753C2|1989-07-06| ZA801163B|1981-03-25| FR2450886B3|1982-01-29| IT7920850D0|1979-03-09| TR21243A|1984-02-14| US4285900A|1981-08-25| DE3008753A1|1980-09-11| JPS55142715A|1980-11-07| IT1110513B|1985-12-23| GB2045273A|1980-10-29| FR2450886A1|1980-10-03| GB2045273B|1983-04-20| GR67012B|1981-05-18|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 BE548451A|1955-06-08| US3410819A|1963-06-28|1968-11-12|American Cyanamid Co|Addition of insoluble additives to fibers during manufacture| CA960824A|1969-12-20|1975-01-14|American Cyanamid Company|Wet-spinning polymer solution containing dispersion of solid in insoluble liquid| JPS5022613B1|1971-06-29|1975-08-01| US4077929A|1975-03-06|1978-03-07|E. I. Du Pont De Nemours And Company|Process for producing flame-resistant filaments| JPS5315170B2|1975-07-04|1978-05-23| US4169876A|1978-04-24|1979-10-02|E. I. Du Pont De Nemours And Company|Process for spinning flame-resistant acrylonitrile polymer fibers|US4354994A|1980-11-19|1982-10-19|Celanese Corporation|Spinning process for antimony oxide/halogenated aromatic polyester composition| JPS6257912A|1985-08-21|1987-03-13|Kanebo Ltd|Production of highly flame-retardant modacrylic yarn| JPS62162012A|1986-01-07|1987-07-17|Kanebo Ltd|Production of modacryl fiber of high flame retardancy| JPH0215642B2|1986-11-17|1990-04-12|Mitsubishi Rayon Co| US20050245163A1|2004-04-30|2005-11-03|Aneja Arun P|Fire blocker fiber composition, high loft web structures, and articles made therefrom| US20050245164A1|2004-04-30|2005-11-03|Aneja Arun P|Fire blocker fiber composition, high loft web structures, and articles made therefrom| CN102154725A|2011-02-25|2011-08-17|抚顺瑞华纤维有限公司|Ultrahigh flame-retardant AN-VDC copolymer fiber and production method thereof|
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申请号 | 申请日 | 专利标题 IT20850/79A|IT1110513B|1979-03-09|1979-03-09|PROCEDURE FOR THE MANUFACTURE OF MODACRYLIC FIBERS WITH GLOSS, STABILITY TO HEAT TREATMENTS AND HIGHER FLAME RESISTANCE| 相关专利
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