CN102965750A - Method for preparing flame retardant viscose fiber - Google Patents
Method for preparing flame retardant viscose fiber Download PDFInfo
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- CN102965750A CN102965750A CN2012104888770A CN201210488877A CN102965750A CN 102965750 A CN102965750 A CN 102965750A CN 2012104888770 A CN2012104888770 A CN 2012104888770A CN 201210488877 A CN201210488877 A CN 201210488877A CN 102965750 A CN102965750 A CN 102965750A
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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 take 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.Raising along with living standards of the people; with clothing and home decoration upper returning nature; will drive viscose acetal fibre take native cellulose as raw material to the development of the tencels such as high-performance, differential, functionalization and environmental protection, satisfy the colourful requirement of downstream product.But at present the viscose acetal fibre kind is also very single, take conventional variety as main, lack non-ly take, the exploitation in high-grade application field.
Whisker be the diameter that forms with monocrystalline form growth very little (0.1～10um), atomic arrangement high-sequential, intensity be near the theoretical value of perfect crystal.In macromolecular material, add a small amount of whisker and just can give intensity height, the function such as heat-resisting, fire-retardant, antibiotic.Alkali magnesium sulfate crystal whisker with anti-flaming function because the crystallization water in its molecule when burning dehydration occurs, can absorb the temperature that a large amount of heat energy reduces base material.In addition, the water vapour of generation can dilute the concentration of flame-zone reaction gas, again can absorbing smoke, play effect fire-retardant and that eliminate smoke.Basic magnesium chloride whisker, magnesium salt whisker all have good flame retardant effect.More more superior than fire proofing commonly used.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, a kind of preferably manufacture method of intensity, well-pressed degree, abrasion-resistant flame-retardant viscose acetal fibre that has is provided.
The objective of the invention is to finish 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 ℃ of vacuum drying oven, cooling is dispersed with stirring 30-45min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 10-20min, loose the 60-70 that contains calcium stearate dispersion ℃ of deionized water for ultrasonic wavelength-division again, clean 25-35min, getting solution upper strata suspension whisker filters through 160 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
B) get 0.8-1.2 part titanate coupling agent by mass fraction, with isopropyl alcohol titanate coupling agent 1 ﹕ 3 is diluted, mixing, then add 10-15 part steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30-45min under 70-80 ℃ of condition, oven 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 ℃ of condition, add again cellulose spinning viscose 90-110 part, airtight stirring reaction 45-60min obtains fire-retardant cellulose spinning viscose;
C) with step B) stirring on the viscose equipment of special use 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) getting 10 parts of characterization parameter diameters by mass fraction is 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 ℃ of vacuum drying ovens, cooling is dispersed with stirring 38min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 15min, loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion again, clean 30min, getting solution upper strata suspension whisker filters through 160 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
Step B) gets 1.0 parts of titanate coupling agents by mass fraction, with isopropyl alcohol titanate coupling agent 1 ﹕ 3 is diluted, mixing, then add 12 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 38min under 75 ℃ of conditions, oven 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 ℃ of conditions, add again 100 parts of cellulose spinning viscoses, airtight stirring reaction 52min obtains 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 mixing, viscose filtration, evacuation of viscose, viscose maturation, then make fire resistant viscose acetal fibre through the wet spinning technology; This cellulose fire resistant viscose acetal fibre has preferably 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. are specially adapted to the public area of fire safety requirement.
The specific embodiment
The present invention will be described in detail below in conjunction with specific embodiment: 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 that 0.1-1.5um, length are the alkali magnesium sulfate crystal whisker of 5-10um, 6-10 part characterization parameter diameter is that 0.2-1um, length are the basic magnesium chloride whisker of 6-12um, and 8-12 part characterization parameter diameter is that 0.2-0.8um, length are the magnesium salt whisker of 6-10um; After above-mentioned three kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, cooling is dispersed with stirring 30-45min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 10-20min, fall apart, clean again 25-35min the 60-70 that contains calcium stearate dispersion ℃ of deionized water for ultrasonic wavelength-division, getting solution upper strata suspension whisker filters through 160 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
B) get 0.8-1.2 part titanate coupling agent by mass fraction, with isopropyl alcohol titanate coupling agent 1 ﹕ 3 is diluted, mixing, then add 10-15 part steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30-45min under 70-80 ℃ of condition, oven 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 ℃ of condition, add again cellulose spinning viscose 90-110 part, airtight stirring reaction 45-60min obtains fire-retardant cellulose spinning viscose;
C) with step B) stirring on the viscose equipment of special use 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, and it adopts following steps:
Steps A) getting 10 parts of characterization parameter diameters by mass fraction is that 0.1-1.5um, length are the alkali magnesium sulfate crystal whisker of 5-10um, 8 parts of characterization parameter diameters are that 0.2-1um, length are the basic magnesium chloride whisker of 6-12um, 10 parts of characterization parameter diameters are 0.2-0.8um, and length is the magnesium salt whisker of 6-10um; After these three kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, cooling is dispersed with stirring 38min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 15min, and, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 160 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
Step B) gets 1.0 parts of titanate coupling agents by mass fraction, with isopropyl alcohol titanate coupling agent 1 ﹕ 3 is diluted, mixing, then add 12 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 38min under 75 ℃ of conditions, oven 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 ℃ of conditions, add again 100 parts of cellulose spinning viscoses, airtight stirring reaction 52min obtains fire-retardant cellulose spinning viscose;
C) with step B) stirring on the viscose equipment of special use 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, and it adopts following steps:
A) getting 8 parts of characterization parameter diameters by mass fraction is that 0.1-1.5um, length are the alkali magnesium sulfate crystal whisker of 5-10um, 6 parts of characterization parameter diameters are that 0.2-1um, length are the basic magnesium chloride whisker of 6-12um, and 8 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um; After above-mentioned three kinds of whiskers are mixed, calcination 4h in 350 ℃ of vacuum drying ovens, cooling is dispersed with stirring 30min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 10min, and, cleaning 25min loose in 60 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 160 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 3 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get 0.8 part of titanate coupling agent by mass fraction, with isopropyl alcohol with titanate coupling agent 1 ﹕ 3 dilution, mixing, then add 10 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30min, oven dry under 70 ℃ 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 ℃ of conditions, add again 90 parts of cellulose spinning viscoses, airtight stirring reaction 45min obtains fire-retardant cellulose spinning viscose;
C) with step B) stirring on the viscose equipment of special use 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, and it adopts following steps:
A) getting 12 parts of characterization parameter diameters by mass fraction is that 0.1-1.5um, length are the alkali magnesium sulfate crystal whisker of 5-10um, 10 parts of characterization parameter diameters are that 0.2-1um, length are the basic magnesium chloride whisker of 6-12um, and 12 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um; After above-mentioned three kinds of whiskers are mixed, calcination 6h in 450 ℃ of vacuum drying ovens, cooling is dispersed with stirring 45min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 20min, and, cleaning 35min loose in 70 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 160 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 5 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get 1.2 parts of titanate coupling agents by mass fraction, with isopropyl alcohol with titanate coupling agent 1 ﹕ 3 dilution, mixing, then add 15 parts of steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 45min, oven dry under 80 ℃ 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 ℃ of conditions, add again 110 parts of cellulose spinning viscoses, airtight stirring reaction 60min obtains fire-retardant cellulose spinning viscose;
C) with step B) stirring on the viscose equipment of special use 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, replaces arbitrarily in specific embodiment, thereby can obtain numerous embodiment, and this is not exemplified one by one.
Claims (2)
1. the manufacture method of a 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 0.1-1.5um, length are the alkali magnesium sulfate crystal whisker of 5-10um, 6-10 part characterization parameter diameter is that 0.2-1um, length are the basic magnesium chloride whisker of 6-12um, and 8-12 part characterization parameter diameter is that 0.2-0.8um, length are the magnesium salt whisker of 6-10um; After above-mentioned three kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, cooling is dispersed with stirring 30-45min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 10-20min, fall apart, clean again 25-35min the 60-70 that contains calcium stearate dispersion ℃ of deionized water for ultrasonic wavelength-division, getting solution upper strata suspension whisker filters through 160 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
B) get 0.8-1.2 part titanate coupling agent by mass fraction, with isopropyl alcohol with titanate coupling agent 1 ﹕ 3 dilution, mixing; Then add 10-15 part steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30-45min, oven dry under 70-80 ℃ 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 ℃ of condition, add again cellulose spinning viscose 90-110 part, airtight stirring reaction 45-60min obtains fire-retardant cellulose spinning viscose;
C) with step B) stirring on the viscose equipment of special use 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.
2. the manufacture method of fire resistant viscose acetal fibre according to claim 1 is characterized in that in the described step:
Steps A) getting 10 parts of characterization parameter diameters by mass fraction is 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 ℃ of vacuum drying ovens, cooling is dispersed with stirring 38min in containing the absolute ethyl alcohol of calgon afterwards, then atmospheric plasma is processed 15min, loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion again, clean 30min, getting solution upper strata suspension whisker filters through 160 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
Step B) gets 1.0 parts of titanate coupling agents by mass fraction, with isopropyl alcohol with titanate coupling agent 1 ﹕ 3 dilution, mixing, then add 12 parts of A) modified crystal whiskers that obtains, airtight mix and blend reaction 38min, oven dry under 75 ℃ of conditions, 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 ℃ of conditions, add again 100 parts of cellulose spinning viscoses, airtight stirring reaction 52min obtains fire-retardant cellulose spinning viscose.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104562683A (en) * | 2015-02-04 | 2015-04-29 | 湖州厉华妤婕联合纺织有限公司 | Preparation method of novel waterproof fire-resistant textile |
| CN105492464A (en) * | 2013-08-05 | 2016-04-13 | 托尔奇图拉帕达纳股份公司 | Cellulose substrate with anti-flame properties and relative production method |
| CN106381564A (en) * | 2016-09-21 | 2017-02-08 | 东华大学 | Preparation method of functional regeneration cellulose fiber |
| 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 |
| CN110184666A (en) * | 2019-06-20 | 2019-08-30 | 宜宾屏山辉瑞油脂有限公司 | Spinning head used in the manufacturing method and manufacturing process of flame retardant cellulose fiber |
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| 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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2012
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Patent Citations (3)
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| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105492464A (en) * | 2013-08-05 | 2016-04-13 | 托尔奇图拉帕达纳股份公司 | Cellulose substrate with anti-flame properties and relative production method |
| CN104562683A (en) * | 2015-02-04 | 2015-04-29 | 湖州厉华妤婕联合纺织有限公司 | Preparation method of novel waterproof fire-resistant textile |
| CN106381564A (en) * | 2016-09-21 | 2017-02-08 | 东华大学 | Preparation method of functional regeneration cellulose fiber |
| 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 |
| CN110184666A (en) * | 2019-06-20 | 2019-08-30 | 宜宾屏山辉瑞油脂有限公司 | Spinning head used in the manufacturing method and manufacturing process of flame retardant cellulose 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 |
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| CN102965750B (en) | 2014-07-30 |
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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 |
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