CN102965750B - Method for preparing flame retardant viscose fiber - Google Patents
Method for preparing flame retardant viscose fiber Download PDFInfo
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Abstract
The invention discloses a method for preparing flame retardant viscose fiber. The method comprising the following steps: A) mixing nano fiber having a flame retardant function, basic magnesium sulfate whisker, basic magnesium chloride whisker and magnesium salt whisker, then roasting the mixture in an oven of 400 DEG C, carrying out dispersion in absolute ethyl alcohol containing sodium hexametaphosphate, carrying out plasma treatment at normal pressure, carrying out ultrasonic dispersion and cleaning, filtering by a filter of 400 meshes and drying; B) uniformly mixing and drying the whisker and a titanate coupling reagent, adding and mixing antimonous oxide, hexabromocyclododecane, (HDPE+SEBS)-g-MAH and calcium stearate, and then adding cellulose spinning viscose to prepare flame retardant cellulose spinning viscose; and C) preparing the flame retardant viscose fiber by means of a wet or dry process spinning technology. The flame retardant viscose fiber is good in strength, stiffness, abrasive resistance and flame retardance.
Description
Technical field
The present invention relates to a kind of manufacture method of fire resistant viscose acetal fibre, described fire resistant viscose acetal fibre, comprise cellulose spinning viscose, alkali magnesium sulfate crystal whisker, magnesium salt whisker, basic magnesium chloride whisker, antimonous oxide, hexabromo-Cyclododecane, belong to textile fabric manufacturing technology field.
Background technology
Viscose acetal fibre belongs to regenerated celulose fibre.It is taking native cellulose as raw material, makes spinning viscose through operations such as alkalization, aging, yellows, makes through wet spinning.Viscose has cellulosic structure and performance.Hygroscopicity, gas permeability, flexibility are good, comfortable and easy to wear; Have the smooth characteristic such as nice and cool, antistatic, its fabric is comfortable and easy to wear, health, graceful, bright-coloured, has many fibers performance can't be obtained.Along with the raising of living standards of the people; with clothing and home decoration upper returning nature; will drive viscose acetal fibre taking native cellulose as raw material to tencel development such as high-performance, differential, functionalization and environmental protection, meet the colourful requirement of downstream product.But at present viscose acetal fibre kind is also very single, taking conventional variety as main, lack non-ly taking, the exploitation in high-grade application field.
Whisker is to approach the theoretical value of perfect crystal with the grow diameter very little (0.1～10um), atomic arrangement high-sequential, the intensity that form of monocrystalline form.In macromolecular material, add a small amount of whisker just can give the functions such as intensity is high, heat-resisting, fire-retardant, antibacterial.There is the alkali magnesium sulfate crystal whisker of anti-flaming function, because the crystallization water in its molecule time dehydration occurs in burning, can absorb a large amount of heat energy and reduce the temperature of base material.In addition, the water vapour of generation can dilute the concentration of flame-zone reaction gas, can absorb again smog, plays effect fire-retardant and that eliminate smoke.Basic magnesium chloride whisker, magnesium salt whisker all have good flame retardant effect.More more superior than conventional fire proofing.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, a kind of manufacture method that has good intensity, well-pressed degree, abrasion-resistant flame-retardant viscose acetal fibre is provided.
The object of the invention is to complete by following technical solution, a kind of manufacture method of fire resistant viscose acetal fibre, it adopts following steps:
A) getting 8-12 part characterization parameter diameter by mass fraction is 0.1-1.5um, length is the alkali magnesium sulfate crystal whisker of 5-10um, 6-10 part characterization parameter diameter is 0.2-1um, length is the basic magnesium chloride whisker of 6-12um, 8-12 part characterization parameter diameter is 0.2-0.8um, length is the magnesium salt whisker of 6-10um, after above-mentioned three kinds of whiskers are mixed, calcination 4-6h in 350-450 DEG C of vacuum drying oven, after cooling containing dispersed with stirring 30-45min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 10-20min, loose in the 60-70 DEG C of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion again, clean 25-35min, getting solution upper strata suspension whisker filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 3-5 time until filtering, after filtering, dry at vacuum drying oven, obtain modified crystal whiskers,
B) get 0.8-1.2 part titanate coupling agent by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted with isopropyl alcohol, mix, then add 10-15 part steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30-45min under 70-80 DEG C of condition, dry, then add antimonous oxide 1-1.5 part, hexabromo-Cyclododecane 2-3 part, (HDPE+SEBS)-g-MAH bulking agent 1.5-2 part, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 30-45min under 65-75 DEG C of condition, add again cellulose spinning viscose 90-110 part, airtight stirring reaction 45-60min, obtain fire-retardant cellulose spinning viscose,
C) by step B) stirring on special viscose equipment of fire-retardant cellulose spinning viscose, mixing, filtration, deaeration, the maturation that obtain; Adopt wet method or dry spinning technology to make a kind of fire resistant viscose acetal fibre.
The preferred technical scheme of the present invention is:
Steps A) to get 10 parts of characterization parameter diameters by mass fraction be 0.1-1.5um, length is the alkali magnesium sulfate crystal whisker of 5-10um, 8 parts of characterization parameter diameters are 0.2-1um, length is the basic magnesium chloride whisker of 6-12um, 10 parts of characterization parameter diameters are 0.2-0.8um, length is the magnesium salt whisker of 6-10um, after these three kinds of whiskers are mixed, calcination 5h in 400 DEG C of vacuum drying ovens, after cooling containing dispersed with stirring 38min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 15min, loose in 65 DEG C of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion again, clean 30min, getting solution upper strata suspension whisker filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering, after filtering, dry at vacuum drying oven, obtain modified crystal whiskers,
Step B) get 1.0 parts of titanate coupling agents by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted with isopropyl alcohol, mix, then add 12 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 38min under 75 DEG C of conditions, dry, then add 1.2 parts of antimonous oxides, 2.5 parts of hexabromo-Cyclododecane, (HDPE+SEBS)-1.8 parts of g-MAH bulking agents, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 38min under 70 DEG C of conditions, add again 100 parts of cellulose spinning viscoses, airtight stirring reaction 52min, obtain fire-retardant cellulose spinning viscose.
The present invention adds alkali magnesium sulfate crystal whisker that nanoscale has fiber reinforcement, fire retardation, magnesium salt whisker, basic magnesium chloride whisker, antimonous oxide, hexabromo-Cyclododecane etc. in cellulose spinning viscose liquid; By viscose mix, viscose filtration, evacuation of viscose, viscose maturation, then make fire resistant viscose acetal fibre through wet spinning technology; This cellulose fire resistant viscose acetal fibre, has good intensity, well-pressed degree, ABRASION RESISTANCE, anti-flammability; Can be widely used in fire-fighting, thermal technology, carpet, curtain, bedding, automobile cushion and indoor decoration etc., be specially adapted to the public area of fire safety requirement.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail: the manufacture method of a kind of fire resistant viscose acetal fibre of the present invention, and this manufacture method adopts following steps:
A) getting 8-12 part characterization parameter diameter by mass fraction is the alkali magnesium sulfate crystal whisker that 0.1-1.5um, length are 5-10um, 6-10 part characterization parameter diameter is the basic magnesium chloride whisker that 0.2-1um, length are 6-12um, and 8-12 part characterization parameter diameter is the magnesium salt whisker that 0.2-0.8um, length are 6-10um; After above-mentioned three kinds of whiskers are mixed, calcination 4-6h in 350-450 DEG C of vacuum drying oven, after cooling containing dispersed with stirring 30-45min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 10-20min,, cleaning 25-35min loose in the 60-70 DEG C of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion again, getting solution upper strata suspension whisker filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 3-5 time until filtering, after filtering, dry at vacuum drying oven, obtain modified crystal whiskers;
B) get 0.8-1.2 part titanate coupling agent by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted with isopropyl alcohol, mix, then add 10-15 part steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30-45min under 70-80 DEG C of condition, dry, then add antimonous oxide 1-1.5 part, hexabromo-Cyclododecane 2-3 part, (HDPE+SEBS)-g-MAH bulking agent 1.5-2 part, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 30-45min under 65-75 DEG C of condition, add again cellulose spinning viscose 90-110 part, airtight stirring reaction 45-60min, obtain fire-retardant cellulose spinning viscose,
C) by step B) stirring on special viscose equipment of fire-retardant cellulose spinning viscose, mixing, filtration, deaeration, the maturation that obtain; Adopt wet method or dry spinning technology to make a kind of fire resistant viscose acetal fibre.
Embodiment 1: the manufacture method of fire resistant viscose acetal fibre of the present invention, it adopts following steps:
Steps A) to get 10 parts of characterization parameter diameters by mass fraction be the alkali magnesium sulfate crystal whisker that 0.1-1.5um, length are 5-10um, 8 parts of characterization parameter diameters are the basic magnesium chloride whisker that 0.2-1um, length are 6-12um, 10 parts of characterization parameter diameters are 0.2-0.8um, the magnesium salt whisker that length is 6-10um; After these three kinds of whiskers are mixed, calcination 5h in 400 DEG C of vacuum drying ovens, after cooling containing dispersed with stirring 38min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 15min, then, cleaning 30min loose in 65 DEG C of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
Step B) get 1.0 parts of titanate coupling agents by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted with isopropyl alcohol, mix, then add 12 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 38min under 75 DEG C of conditions, dry, then add 1.2 parts of antimonous oxides, 2.5 parts of hexabromo-Cyclododecane, (HDPE+SEBS)-1.8 parts of g-MAH bulking agents, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 38min under 70 DEG C of conditions, add again 100 parts of cellulose spinning viscoses, airtight stirring reaction 52min, obtain fire-retardant cellulose spinning viscose,
C) by step B) stirring on special viscose equipment of fire-retardant cellulose spinning viscose, mixing, filtration, deaeration, the maturation that obtain; Adopt wet method or dry spinning technology to make a kind of fire resistant viscose acetal fibre.
Embodiment 2: the manufacture method of a kind of fire resistant viscose acetal fibre of the present invention, it adopts following steps:
A) getting 8 parts of characterization parameter diameters by mass fraction is the alkali magnesium sulfate crystal whisker that 0.1-1.5um, length are 5-10um, 6 parts of characterization parameter diameters are the basic magnesium chloride whisker that 0.2-1um, length are 6-12um, and 8 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um; After above-mentioned three kinds of whiskers are mixed, calcination 4h in 350 DEG C of vacuum drying ovens, after cooling containing dispersed with stirring 30min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 10min, then, cleaning 25min loose in 60 DEG C of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 3 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) get 0.8 part of titanate coupling agent by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted, mixed with isopropyl alcohol, then add 10 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30min, oven dry under 70 DEG C of conditions, then add 1 part of antimonous oxide, 2 parts of hexabromo-Cyclododecane, 1.5 parts of (HDPE+SEBS)-g-MAH bulking agents, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 30min under 65 DEG C of conditions, add again 90 parts of cellulose spinning viscoses, airtight stirring reaction 45min, obtains fire-retardant cellulose spinning viscose;
C) by step B) stirring on special viscose equipment of fire-retardant cellulose spinning viscose, mixing, filtration, deaeration, the maturation that obtain; Adopt wet method or dry spinning technology to make a kind of fire resistant viscose acetal fibre.
Embodiment 3: the manufacture method of a kind of fire resistant viscose acetal fibre of the present invention, it adopts following steps:
A) getting 12 parts of characterization parameter diameters by mass fraction is the alkali magnesium sulfate crystal whisker that 0.1-1.5um, length are 5-10um, 10 parts of characterization parameter diameters are the basic magnesium chloride whisker that 0.2-1um, length are 6-12um, and 12 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um; After above-mentioned three kinds of whiskers are mixed, calcination 6h in 450 DEG C of vacuum drying ovens, after cooling containing dispersed with stirring 45min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 20min, then, cleaning 35min loose in 70 DEG C of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 5 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) get 1.2 parts of titanate coupling agents by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted, mixed with isopropyl alcohol, then add 15 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 45min, oven dry under 80 DEG C of conditions, then add 1.5 parts of antimonous oxides, 3 parts of hexabromo-Cyclododecane, 2 parts of (HDPE+SEBS)-g-MAH bulking agents, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 45min under 75 DEG C of conditions, add again 110 parts of cellulose spinning viscoses, airtight stirring reaction 60min, obtains fire-retardant cellulose spinning viscose;
C) by step B) stirring on special viscose equipment of fire-retardant cellulose spinning viscose, mixing, filtration, deaeration, the maturation that obtain; Adopt wet method or dry spinning technology to make a kind of fire resistant viscose acetal fibre.
Embodiment of the present invention is not limited to the above three embodiment, by aforementioned disclosed number range, in specific embodiment, replaces arbitrarily, thereby can obtain numerous embodiment, and this is not exemplified one by one.
Claims (2)
1. a manufacture method for fire resistant viscose acetal fibre, is characterized in that this manufacture method adopts following steps:
A) getting 8-12 part characterization parameter diameter by mass fraction is that 0.1-1.5 μ m, length are the alkali magnesium sulfate crystal whisker of 5-10 μ m, 6-10 part characterization parameter diameter is that 0.2-1 μ m, length are the basic magnesium chloride whisker of 6-12 μ m, and 8-12 part characterization parameter diameter is that 0.2-0.8 μ m, length are the magnesium salt whisker of 6-10 μ m; After above-mentioned three kinds of whiskers are mixed, calcination 4-6h in 350-450 DEG C of vacuum drying oven, after cooling containing dispersed with stirring 30-45min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 10-20min,, cleaning 25-35min loose in the 60-70 DEG C of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion again, getting solution upper strata suspension whisker filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 3-5 time until filtering, after filtering, dry at vacuum drying oven, obtain modified crystal whiskers;
B) get 0.8-1.2 part titanate coupling agent by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted, mixed with isopropyl alcohol; Then add 10-15 part steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30-45min, oven dry under 70-80 DEG C of condition, then add 0.3 part of antimonous oxide 1-1.5 part, hexabromo-Cyclododecane 2-3 part, (HDPE+SEBS)-g-MAH bulking agent 1.5-2 part, dispersant calcium stearate, airtight mix and blend reaction 30-45min under 65-75 DEG C of condition, add again cellulose spinning viscose 90-110 part, airtight stirring reaction 45-60min, obtains fire-retardant cellulose spinning viscose;
C) by step B) stirring on special viscose equipment of fire-retardant cellulose spinning viscose, mixing, filtration, deaeration, the maturation that obtain; Adopt wet spinning technology to make a kind of fire resistant viscose acetal fibre.
2. according to the manufacture method of the fire resistant viscose acetal fibre described in claim 1, it is characterized in that in described step:
Steps A) to get 10 parts of characterization parameter diameters by mass fraction be 0.1-1.5 μ m, length is the alkali magnesium sulfate crystal whisker of 5-10 μ m, 8 parts of characterization parameter diameters are 0.2-1 μ m, length is the basic magnesium chloride whisker of 6-12 μ m, 10 parts of characterization parameter diameters are 0.2-0.8 μ m, length is the magnesium salt whisker of 6-10 μ m, after these three kinds of whiskers are mixed, calcination 5h in 400 DEG C of vacuum drying ovens, after cooling containing dispersed with stirring 38min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 15min, loose in 65 DEG C of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion again, clean 30min, getting solution upper strata suspension whisker filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering, after filtering, dry at vacuum drying oven, obtain modified crystal whiskers,
Step B) get 1.0 parts of titanate coupling agents by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted with isopropyl alcohol, mix, then add 12 parts of A) modified crystal whiskers that obtains, airtight mix and blend reaction 38min under 75 DEG C of conditions, dry, then add 1.2 parts of antimonous oxides, 2.5 parts of hexabromo-Cyclododecane, (HDPE+SEBS)-1.8 parts of g-MAH bulking agents, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 38min under 70 DEG C of conditions, add again 100 parts of cellulose spinning viscoses, airtight stirring reaction 52min, obtain fire-retardant cellulose spinning viscose.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| ITTO20130670A1 (en) * | 2013-08-05 | 2015-02-06 | Torcitura Padana S P A | CELLULOSIC SUBSTRATE WITH ANTI-FLAME PROPERTIES AND RELATED PRODUCTION PROCEDURE |
| CN104562683B (en) * | 2015-02-04 | 2017-01-11 | 青岛福基纺织有限公司 | Preparation method of waterproof fire-resistant textile |
| CN106381564B (en) * | 2016-09-21 | 2018-11-23 | 东华大学 | A kind of preparation method of functional regeneration cellulose fibre |
| CN110016726A (en) * | 2019-04-23 | 2019-07-16 | 杭州墨舞神韵文化艺术集团有限公司 | A kind of preparation method of high-strength corrosion-resisting viscose fiber |
| CN110184666B (en) * | 2019-06-20 | 2021-11-16 | 宜宾屏山辉瑞油脂有限公司 | Method for producing flame-retardant cellulose fiber and spinneret used in the production process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068352C (en) * | 1998-07-09 | 2001-07-11 | 厦门大学 | Production of composite material with stereospecific whisker strengthened polymer |
| CN1377995A (en) * | 2002-04-17 | 2002-11-06 | 东华大学 | Process for preparing anti-static polyacrylonitrile fibre |
| CN1483863A (en) * | 2003-07-29 | 2004-03-24 | 东华大学 | Method for preparing whisker material to make modification treatment of spinning chemical fibre |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068352C (en) * | 1998-07-09 | 2001-07-11 | 厦门大学 | Production of composite material with stereospecific whisker strengthened polymer |
| CN1377995A (en) * | 2002-04-17 | 2002-11-06 | 东华大学 | Process for preparing anti-static polyacrylonitrile fibre |
| CN1483863A (en) * | 2003-07-29 | 2004-03-24 | 东华大学 | Method for preparing whisker material to make modification treatment of spinning chemical fibre |
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Effective date of registration: 20200525 Address after: 314502 Industrial Park, Puyuan Town, Tongxiang, Jiaxing City, Zhejiang Province Patentee after: Jiaxing diaoshai Clothing Co., Ltd Address before: Hangzhou City, Zhejiang province 310018 Xiasha Higher Education Park No. 2 Street No. 5 Patentee before: ZHEJIANG SCI-TECH University |