CN101104959A - Method for preparing viscose fiber - Google Patents

Method for preparing viscose fiber Download PDF

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Publication number
CN101104959A
CN101104959A CNA2007100150352A CN200710015035A CN101104959A CN 101104959 A CN101104959 A CN 101104959A CN A2007100150352 A CNA2007100150352 A CN A2007100150352A CN 200710015035 A CN200710015035 A CN 200710015035A CN 101104959 A CN101104959 A CN 101104959A
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China
Prior art keywords
viscose
cellulose
yawn
spinning
preparation
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Pending
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CNA2007100150352A
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Chinese (zh)
Inventor
王乐军
刘海洋
姜明亮
卢海蛟
吕翠莲
葛洪
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CHTC Helon Co Ltd
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Shandong Helon Co Ltd
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Priority to CNA2007100150352A priority Critical patent/CN101104959A/en
Publication of CN101104959A publication Critical patent/CN101104959A/en
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Abstract

The invention discloses a preparation method of viscose fibers, which is characterized in that the cellulose pulp is used in the viscous glue preparation procedure; the cellulose pulp together with an additional modifier are processed to cellulose xanthate with high esterification degree and ripeness degree; the spinning procedure is performed under such conditions as low coagulation bath temperature, low acidity and high sodium sulfate concentration, without using zinc sulfate which results in serious environmental pollution; the thickness of fiber skin is increased by drafting; and the produced viscose fiber has high strength and high wet modulus. The invention solves the problem of zinc pollution in the prior art, produces viscose fibers with high strength, high wet modulus, and good tension, and overcomes the disadvantages that the fabric is easy to deform, instable in size and nonresistant against base when the viscose fiber is in wet state. Compared with the prior viscose staple fibers, the fabric made of the inventive fibers is superior in high strength and good resistance against deformation and alkali.

Description

A kind of preparation method of viscose
Technical field
The present invention relates to a kind of cellulose fibre technology, especially relate to a kind of preparation method of viscose.
Background technology
Adopting poisonous and zinc sulfate natural resources shortage is that to produce viscose be a big shortcoming in making at present.The zinc sulfate that filature wastewater in the viscose production contains has brought great pollution to environment, serious harm people's is healthy, and the whole bag of tricks such as the precipitation method, resin treatment method or dilution discharge etc. to the zinc wastewater treatment, its disposal cost is all higher, and the discharging water quality index is also unstable.In order to solve this phenomenon, all adopt low zinc spinning in factory at present, but when the zinc in the coagulating bath dropped to 6g/l, colluding by force of the fiber of preparation will be affected.And adopt no zinc coagulating bath method to produce viscose at present, though its environmental pollution of having avoided zinc salt to bring, the physical and mechanical properties index of prepared viscose is relatively poor.And the common viscose that makes violent swelling when hygrometric state makes wet strength and modulus very low, and it is yielding to have a fabric, and poor dimensional stability is not alkaline-resisting, can not stand to improve the mercerization of appearance of fabrics and handle; Can only adopt loose formula dyeing during dyeing, make shortcomings such as dyeing course is difficult to carry out continuously, and the polynoise fiber of producing, though it is wet strong and wet modulus is higher, but fiber colludes lower by force, and fragility is bigger, easily forms the fibrillation structure, and technology is also complicated, its product is used be subjected to certain restriction.
Summary of the invention
Technical problem to be solved by this invention has provided and has a kind ofly not only overcome in the viscose production environmental pollution that band zinc waste water brings but also the viscose of preparation has the preparation method of the viscose of higher intensity and wet modulus.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of preparation method of viscose, and adopt cellulose pulp to make alkali cellulose, will add 35~55% (to alpha-cellulose weight) CS in the alkali cellulose that make 2React and made cellulose xanthate in 1.5~6 hours, and in cellulose xanthate dissolving just or back course of dissolution, add denaturant V315 and (be used for modified high-strength viscose silk and high-wet-modulus fibre denaturant for what BEROL NOBEL_NOBEL INDUSTRIES SWTDEN produced, solvable in the viscose glue, it in viscose glue nonionic, and be cationic in acid bath, can mix with nonionic and cationic viscose glue and spinning additive.It uses in modified high strength and high-wet-modulus fibre, use amount is about relative cellulose 1~4%, can be added in the course of dissolution of xanthate acid and in the viscose glue after the deaeration) or V318 (a kind of interpolation auxiliary agent that improves processing characteristics of producing for BEROLNOBEL_NOBEL INDUSTRIES SWTDEN, the same V315 of its operating position), make the performance of fiber with raising, addition is 1.5%~2.5% (alpha-cellulose weight relatively), make alpha-cellulose 5.5%~10.0%, NaOH 4.5%~10.0%, it is fine than being 0.9~1.2 to control alkali, viscosity (falling ball method) 60~200s, degree of ripeness (10%NH 4The Cl value) 7.0~39ml, viscose glue esterification degree are the spinning viscose glue of 35~65 high esterification degree, high degree of ripeness; Adopt spinning spray orifice aperture 45~55 μ m, spinning coagulation bath to adopt 25~45 ℃ of sulfuric acid 70~105g/l's, aluminum sulfate 15~80g/l, sodium sulphate 350~400g/l, acid bath temperature, the wet spinning of spinning immersion length 〉=70cm, through stretch oneself and yawn, concise, operation such as bleaching post processing etc. obtains finished fiber, fiber is done by force at 3.5~5.0cN/dtex, the hygrometric state elastic modelling quantity is 0.35~0.58cN/dtex, and wet is by force 2.0~3.5cN/dtex.In the present invention,, reduce the reproduction speed of cellulose xanthate in the spinning, increase the skin thickness of fiber, improve the fibrocortex degree of orientation, thereby reduce the swellbility of fiber, improve the intensity of fiber by adopting the spinning coagulation bath of high-load sodium sulphate.Adopt aluminum sulfate to control the decomposition of yellow acid fat, improve the structural homogeneity of fiber.
Wherein, cellulose pulp can adopt a kind of in cotton pulp, wood pulp, bamboo pulp, the sugarcane slurry, perhaps can adopt more than one combinations.
And when stretching oneself and yawn, then can adopt shower nozzle stretch oneself and yawn between stretching oneself and yawn, coiling, three bathe stretch oneself and yawn, four bathe stretch oneself and yawn, retraction or two or more combination, control is always stretched oneself and yawn than being 50~300%.By rational stretching, improve the degree of orientation of plain molecule in the fiber greatly, thereby improve the intensity of fiber.
The spray orifice in when silk spray can adopt circle, also comprises annular, square, triangle, Y shape, and the material that is provided with the spinnerets of spray orifice can adopt tantalum matter plated film or yellow platinum or glass to make.
When carrying out the post processing refining desulfuration, can adopt caustic soda or sodium sulfite, its concentration 2~25g/l, 50~95 ℃ of temperature.The post processing refining bleaching then can adopt hydrogen peroxide or clorox, its concentration 0.1~5.0g/l, 35~65 ℃ of temperature.
Method technology of the present invention is simple, easy to control, each raw material is easy to get, production cost is low, in the viscose glue preparation, add denaturant, make high esterification degree, the cellulose xanthate ester of high degree of ripeness, improved the strainability of viscose glue, improved in the spinning coagulation bath uniform in shaping, and adopt the serious zinc sulfate of cancellation environmental pollution in spinning coagulation bath, use the sodium of high level and the method for aluminum sulfate, the environmental pollution that the high zinc waste water of having avoided adopting zinc sulfate to bring brings, and by with stretch oneself and yawn cooperating of technology, increased the thickness of fibrocortex, thereby make the viscose that makes have higher intensity and wet modulus, it is good by force to collude, and it is yielding to have overcome under the viscose hygrometric state fabric, poor dimensional stability and not alkaline-resisting shortcoming, the fabric that adopts this fiber to make has the intensity height, anti-repeatedly morphotropism, alkali resistance has the good physical and mechanical properties similar to cotton fiber all above common viscose staple fibre.
The specific embodiment
Embodiment 1
Add 55% (to alpha-cellulose weight) CS in the alkali cellulose that adopts high polymerization degree cotton to make 2Reacted 1.5 hours, course of dissolution adds 1.5% (alpha-cellulose weight relatively) denaturant V315 behind cellulose xanthate, obtains viscose glue and consists of: alpha-cellulose 8.20%, NaOH 5.8%, viscosity (falling ball method) 100s, degree of ripeness (10%NH 4The Cl value) 30.0ml, viscose glue esterification degree are the spinning viscose glue of 50 high esterification degree, high degree of ripeness;
Adopt wet moulding, adopt the aperture at the circular tantalum matter of 55 μ m plated film spinning head, the coagulating bath technology that spinning moulding is used: 29 ℃ of sulfuric acid 75g/l, aluminum sulfate 15g/l, sodium sulphate 390g/l, acid bath temperature, spinning immersion length 75cm, cellulose xanthate solidifies and is regenerated as cellulose fibre after the spinning;
Between shower nozzle is stretched oneself and yawn, coiled, stretch oneself and yawn, three bathe and to stretch oneself and yawn, four to bathe and stretch oneself and yawn, always stretch oneself and yawn than being 280%;
Refining desulfuration adopts caustic soda, its concentration 10g/l, 89 ℃ of temperature; Refining bleaching adopts hydrogen peroxide, its concentration 0.25g/l, 55 ℃ of temperature.After super-dry, promptly obtain finished fiber again.Prepared fiber is done by force at 4.5cN/dtex, and the hygrometric state elastic modelling quantity is 0.52cN/dtex, and wet is 2.8cN/dtex by force.
Embodiment 2
Adopt common wood pulp pulp, add 48% (alpha-cellulose weight) CS in the alkali cellulose that makes 2Reacted 1.6 hours, and behind cellulose xanthate, added 2.5% (alpha-cellulose weight relatively) denaturant V318 in the course of dissolution, obtain viscose glue and consist of: alpha-cellulose 8.8%, NaOH 4.8%, viscosity (falling ball method) 180s, degree of ripeness (10%NH 4The Cl value) 7.5ml, viscose glue esterification degree are the spinning viscose glue of 55 high esterification degree, high degree of ripeness;
Adopt wet moulding, adopt the Y shape yellow platinum opposite sex spinning head of aperture at 50 μ m,
With above-mentioned spinning solution through material for being pressed in the coagulating bath.The coagulating bath technology that spinning moulding is used: 43 ℃ of sulfuric acid 100g/l, aluminum sulfate 75g/l, sodium sulphate 360g/l, acid bath temperature, spinning immersion length 80cm, cellulose xanthate solidifies and is regenerated as cellulose fibre after spinning;
Above-mentioned fiber stretches oneself and yawn between shower nozzle is stretched oneself and yawn, coiled, two bathe and stretch oneself and yawn, and always stretches oneself and yawn than being 290%.
Refining desulfuration adopts sodium sulfite, its concentration 10g/l, 90 ℃ of temperature; Refining bleaching adopts clorox, its concentration 0.15g/l, and 45 ℃ of temperature promptly obtain finished fiber again after super-dry.Prepared fiber is done by force at 4.1cN/dtex, and the hygrometric state elastic modelling quantity is 0.53cN/dtex, and wet is 2.6cN/dtex by force.
Embodiment 3
Add 35% (to alpha-cellulose weight) CS in the alkali cellulose that adopts high polymerization degree cotton and sugarcane slurry to make 2Reacted 4.5 hours, course of dissolution adds 2.0% (alpha-cellulose weight relatively) denaturant V315 behind cellulose xanthate, obtains viscose glue and consists of: alpha-cellulose 6.40%, NaOH 4.8%, viscosity (falling ball method) 80s, degree of ripeness (10%NH 4The Cl value) 35.0ml, viscose glue esterification degree are the spinning viscose glue of 53 high esterification degree, high degree of ripeness;
Adopt wet moulding, adopt the aperture at 45 μ m triangle tantalum matter plated film spinning heads, the coagulating bath technology that spinning moulding is used: 32 ℃ of sulfuric acid 70g/l, aluminum sulfate 20g/l, sodium sulphate 350g/l, acid bath temperature, spinning immersion length 73cm, cellulose xanthate solidifies and is regenerated as cellulose fibre after the spinning;
Between shower nozzle is stretched oneself and yawn, coiled, stretch oneself and yawn, three bathe and to stretch oneself and yawn, four to bathe and stretch oneself and yawn, always stretch oneself and yawn than being 180%;
Refining desulfuration adopts caustic soda, its concentration 5g/l, 80 ℃ of temperature; Refining bleaching adopts hydrogen peroxide, its concentration 0.18g/l, 55 ℃ of temperature.After super-dry, promptly obtain finished fiber again.Prepared fiber is done by force at 3.8cN/dtex, and the hygrometric state elastic modelling quantity is 0.46cN/dtex, and wet is 2.6cN/dtex by force.
Embodiment 4
Adopt in the mixed alkali cellulose that gets of common cotton pulp, wood pulp and bamboo pulp and add 45% (alpha-cellulose weight) CS 2Reacted 3 hours, and behind cellulose xanthate, added 2.2% (alpha-cellulose weight relatively) denaturant V315 in the course of dissolution, obtain viscose glue and consist of: alpha-cellulose 7.8%, NaOH 6.8%, viscosity (falling ball method) 160s, degree of ripeness (10%NH 4The Cl value) 28ml, viscose glue esterification degree are the spinning viscose glue of 45 high esterification degree, high degree of ripeness;
Adopt wet moulding, adopt the circular yellow platinum opposite sex spinning head of aperture at 50 μ m;
With above-mentioned spinning solution through material for being pressed in the coagulating bath.The coagulating bath technology that spinning moulding is used: 40 ℃ of sulfuric acid 90g/l, aluminum sulfate 70g/l, sodium sulphate 365g/l, acid bath temperature, spinning immersion length 95cm, cellulose xanthate solidifies and is regenerated as cellulose fibre after spinning;
Above-mentioned fiber stretches oneself and yawn between shower nozzle is stretched oneself and yawn, coiled, two bathe and stretch oneself and yawn, and always stretches oneself and yawn than being 250%.
Refining desulfuration adopts sodium sulfite, its concentration 17g/l, 55 ℃ of temperature; Refining bleaching adopts clorox, its concentration 3.5g/l, and 35 ℃ of temperature promptly obtain finished fiber again after super-dry.Prepared fiber is done by force at 3.8cN/dtex, and the hygrometric state elastic modelling quantity is 0.47cN/dtex, and wet is 2.4cN/dtex by force.

Claims (6)

1. the preparation method of a viscose is characterized in that: adopt cellulose pulp to make alkali cellulose, will add 35~55% (to alpha-cellulose weight) CS in the alkali cellulose that make 2React and made cellulose xanthate in 1.5~6 hours, and in cellulose xanthate dissolving just or back course of dissolution, add denaturant 1.5%~2.5% (alpha-cellulose weight relatively), make alpha-cellulose 5.5%~10.0%, NaOH 4.5%~10.0%, viscosity (falling ball method) 60~200s, degree of ripeness (10%NH 4The Cl value) 7.0~39ml, viscose glue esterification degree are the spinning viscose glue of 35~65 high esterification degree, high degree of ripeness; Adopt spinning spray orifice aperture 45~55 μ m, spinning coagulation bath to adopt 25~45 ℃ of sulfuric acid 70~105g/l's, aluminum sulfate 15~80g/l, sodium sulphate 350~400g/l, acid bath temperature, the wet spinning of spinning immersion length 〉=70cm, through stretch oneself and yawn, concise, operation such as bleaching post processing etc. obtains finished fiber.
2. the preparation method of a kind of viscose as claimed in claim 1 is characterized in that: one or more combinations in described cellulose pulp employing cotton pulp, wood pulp, bamboo pulp, the sugarcane slurry.
3. the preparation method of a kind of viscose as claimed in claim 1 is characterized in that: described stretch oneself and yawn comprise shower nozzle stretch oneself and yawn between stretching oneself and yawn, coiling, three bathe stretch oneself and yawn, four bathe stretch oneself and yawn, retraction or two or more combination, always stretch oneself and yawn than being 50~300%.
4. the preparation method of a kind of viscose as claimed in claim 1, it is characterized in that: described spray orifice comprises circle, also comprises annular, square, triangle, Y shape.
5. the preparation method of a kind of viscose as claimed in claim 1 is characterized in that: described refining desulfuration employing caustic soda or sodium sulfite, concentration 2~25g/l, 50~95 ℃ of temperature.
6. the preparation method of a kind of viscose as claimed in claim 1 is characterized in that: post processing refining bleaching employing hydrogen peroxide or clorox, its concentration 0.1~5.0g/l, 35~65 ℃ of temperature.
CNA2007100150352A 2007-06-14 2007-06-14 Method for preparing viscose fiber Pending CN101104959A (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101545150B (en) * 2009-04-30 2011-01-05 郑睿敏 Method for manufacturing modal fiber
CN101591814B (en) * 2009-05-25 2011-03-16 郑睿敏 Method for manufacturing high wet modulus fiber
CN102101890A (en) * 2010-12-28 2011-06-22 成都丽雅纤维股份有限公司 Post dissolution process of viscose
CN102337688A (en) * 2011-03-24 2012-02-01 湖南拓普竹麻产业开发有限公司 Mixed pulp used for producing viscose fiber and its production process
CN103205580A (en) * 2013-04-19 2013-07-17 金川集团股份有限公司 Desulfurization method in noble metal enriching process
CN103233289A (en) * 2013-04-08 2013-08-07 宜宾海丝特纤维有限责任公司 Viscose monofilament production process
CN103668518A (en) * 2012-09-21 2014-03-26 江苏蓝品纤维科技发展有限公司 Aramid fiber and functional fiber prepared therefrom
CN108035004A (en) * 2017-11-20 2018-05-15 河北吉藁化纤有限责任公司 A kind of flame retardant viscose fiber and preparation method thereof
CN109944084A (en) * 2019-03-20 2019-06-28 广州市番禺区港棉制衣厂 A kind of waterproof and breathable shell fabric and preparation method thereof
CN110184665A (en) * 2019-05-29 2019-08-30 新乡化纤股份有限公司 A kind of production technology of the continuous spunbond glue fiber of odd-shaped cross section
CN110644068A (en) * 2019-08-26 2020-01-03 徐州锦业纺织科技有限公司 Production process of rayon yarn
CN114182363A (en) * 2020-10-12 2022-03-15 青岛尼希米生物科技有限公司 Cellulose fiber capable of adsorbing and quickly deeply dyeing and preparation method and application thereof
CN114351271A (en) * 2021-12-24 2022-04-15 唐山三友集团兴达化纤有限公司 Water-transparent viscose fiber and preparation method and application thereof

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101545150B (en) * 2009-04-30 2011-01-05 郑睿敏 Method for manufacturing modal fiber
CN101591814B (en) * 2009-05-25 2011-03-16 郑睿敏 Method for manufacturing high wet modulus fiber
CN102101890A (en) * 2010-12-28 2011-06-22 成都丽雅纤维股份有限公司 Post dissolution process of viscose
CN102337688A (en) * 2011-03-24 2012-02-01 湖南拓普竹麻产业开发有限公司 Mixed pulp used for producing viscose fiber and its production process
CN103668518A (en) * 2012-09-21 2014-03-26 江苏蓝品纤维科技发展有限公司 Aramid fiber and functional fiber prepared therefrom
CN103233289A (en) * 2013-04-08 2013-08-07 宜宾海丝特纤维有限责任公司 Viscose monofilament production process
CN103205580A (en) * 2013-04-19 2013-07-17 金川集团股份有限公司 Desulfurization method in noble metal enriching process
CN108035004A (en) * 2017-11-20 2018-05-15 河北吉藁化纤有限责任公司 A kind of flame retardant viscose fiber and preparation method thereof
CN109944084A (en) * 2019-03-20 2019-06-28 广州市番禺区港棉制衣厂 A kind of waterproof and breathable shell fabric and preparation method thereof
CN110184665A (en) * 2019-05-29 2019-08-30 新乡化纤股份有限公司 A kind of production technology of the continuous spunbond glue fiber of odd-shaped cross section
CN110644068A (en) * 2019-08-26 2020-01-03 徐州锦业纺织科技有限公司 Production process of rayon yarn
CN114182363A (en) * 2020-10-12 2022-03-15 青岛尼希米生物科技有限公司 Cellulose fiber capable of adsorbing and quickly deeply dyeing and preparation method and application thereof
CN114351271A (en) * 2021-12-24 2022-04-15 唐山三友集团兴达化纤有限公司 Water-transparent viscose fiber and preparation method and application thereof
CN114351271B (en) * 2021-12-24 2023-10-13 唐山三友集团兴达化纤有限公司 Water-meeting transparent viscose fiber and preparation method and application thereof

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