CN101215726A - Method for preparing flame-proof viscose fiber - Google Patents

Method for preparing flame-proof viscose fiber Download PDF

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Publication number
CN101215726A
CN101215726A CNA2007101165124A CN200710116512A CN101215726A CN 101215726 A CN101215726 A CN 101215726A CN A2007101165124 A CNA2007101165124 A CN A2007101165124A CN 200710116512 A CN200710116512 A CN 200710116512A CN 101215726 A CN101215726 A CN 101215726A
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CN
China
Prior art keywords
flame retardant
spinning
fire
fire retardant
fiber
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Pending
Application number
CNA2007101165124A
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Chinese (zh)
Inventor
逄奉建
王乐军
刘建华
马君志
马峰刚
王东
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CHTC Helon Co Ltd
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Shandong Helon Co Ltd
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Publication date
Application filed by Shandong Helon Co Ltd filed Critical Shandong Helon Co Ltd
Priority to CNA2007101165124A priority Critical patent/CN101215726A/en
Publication of CN101215726A publication Critical patent/CN101215726A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a process for preparing flame retarding cellulose viscose, which adopts pyrophosphate exchange reaction flame retardant particle whose mean particle diameter is <= 1.0um, non-ionic surface active agent, dispersing agent and solvent water to mix and obtain flame retardant emulsion, each percentage by weight is pyrophosphate exchange reaction flame retardant 20-45 wt%, non-ionic surface active agent 5-10 wt% and dispersing agent 0.5-1.0 wt%, and residue is solvent water. The process for preparation comprises adding pyrophosphate exchange reaction flame retardant of flame retardant emulsion which is corresponded to alpha cellulose 15-30 % into spinning original liquid which is filtered to mix, shaping spinning by adopting spinning bath which is low acid, low salt, low temperature and high zinc. The spinning original liquid of the invention has simple and convenient preparation, fiber does not contain halogen elements, which avoids environmental pollution, when in burning, the invention is not melted, while charring only happens to keep the original shape of fiber, the invention prevents dripping which is melted in high temperature from scalding human body, and flame retardant is distributed evenly in adhesive, which can not smolder after leaving fire and easy to be self-extinguished.

Description

Method for preparing flame-proof viscose fiber
Technical field
The present invention relates to a kind of artificial fibre, especially relate to a kind of preparation method of Fire resistant viscose fiber.
Background technology
Along with the progress of development of science and technology and textile industry, the weaving kind be on the increase, its range of application and quantity increase substantially, from daily life to industry, communications and transportation, to numerous areas such as military affairs.But following, because of ignite this difficult problem of causing disaster of textiles also seems more and more important.The result that the death by accident that is caused by fire is investigated shows that the fire that is caused by upholstery and textiles accounts for important proportion.Therefore for preventing fire, produce fire resistance fibre and more and more be subject to people's attention.In order to reduce the harm of fabric fire, people have adopted various methods.As limiting non-flame-retardant textile with fabric types and field of employment, the fire-retardant production of viscose is mainly adopted at fiber and is made back or (when fiber is in gel state) in process of production, antimonous oxide is coated on the surface of fiber with the latex state with halogen-containing fire retardant, also there is the fire retardant of employing to prepare the rayon spinning stoste that contains the fire retardant particle, since the preparation have anti-flammability viscose, typical fire retardant has the polyvinyl chloride latex, the polyvinyl bromide latex, the adhesive that chlorinated paraffin wax or bromination aromatic hydrocarbons and antimony oxide are combined into etc., but the halogen-containing fire retardant of the many employings of these fire retardants, exist non-degradable, has certain pollution after discarded, and this kind fire retardant non-refractory, not wash resistant and Exposure to Sunlight, and the molten drop drip phenomenon takes place in fire resistance fibre easily, the high-temperature fusant that fusion drippage produces not only can skin ambustion, and the combustible material on every side that can ignite, cause more conflagration, easily glow after leaving burning things which may cause a fire disaster, not from putting out, bring certain difficulty to fire prevention, the rayon spinning stoste that adopts fire retardant and spinning viscose glue to be mixed with simultaneously is inhomogeneous, the uniformity of its flame retardant effect is relatively poor, and the adding of fire retardant particulate has influenced the viscose filtration performance and powerful index reduces, and has increased the difficulty of spinning.
Summary of the invention
Technical problem to be solved by this invention has provided a kind of method for preparing flame-proof viscose fiber, adopt this method to prepare Fire resistant viscose fiber, spinning solution prepares simple and convenient, do not contain halogenic ingredient in the fiber that makes, avoided environmental pollution, thereby and in the not fusion of when burning charing only takes place and avoid the high-temperature fusion dropping that the people is scalded to keep the fiber original form, fire retardant is uniformly dispersed in viscose glue simultaneously, after leaving burning things which may cause a fire disaster, do not glow, easily from putting out.
Technical scheme of the present invention is: method for preparing flame-proof viscose fiber, its preparation section is with high quality cotton, cellulose pulps such as wood pulps are raw material, employing comprises dipping, squeezing, pulverize, experienced, yellow, dissolving, mix, deaeration, filter, spinning, stretch oneself and yawn, concise, the viscose production stage that oven dry etc. are conventional, mix in the spinning solution and adopt the fire retardant emulsion that contains pyrophosphate based flame retardant particulate that after filtration, will prepare before the spinning to join, be mixing after the raising adding, can add in the spinning glue containing the fire retardant emulsion by sound attitude blender, adopt sulfuric acid 50~90g/l then, sodium sulphate 230~290g/l, zinc sulfate 15~45g/l, the low acid that temperature is 30~45 ℃, less salt, low temperature, high zinc spinning bath spinning moulding.In order to make flame retardant particle can be evenly distributed in the surperficial and inner of viscose, just must handle the emulsification of flame retardant particle well, dispersed, being complementary between grinding, also to make the blend of fire retardant emulsion and viscose glue compatible simultaneously, layering does not appear, precipitation, therefore select the emulsification of suitable fire retardant particulate, dispersant, the configuration of fire retardant emulsion is as follows: the pyrophosphate based flame retardant particulate that adopts average grain diameter≤1.0 μ m, non-ionic surface active agent, dispersant and aqueous solvent mix and make the fire retardant emulsion, its each composition percentage by weight is respectively pyrophosphate based flame retardant 20-45wt%, non-ionic surface active agent 5-10wt%, dispersant 0.5-1.0wt%, surplus is an aqueous solvent; Mix in the spinning solution after with the relative first fibre 15~30% of effective fire retardant pyrophosphate based flame retardant amount the adding of fire retardant emulsion being filtered then; And the pyrophosphate based flame retardant can grind to obtain the fire retardant particulate of small particle diameter, and the powder particulate of control pyrophosphate based flame retardant diameter of particle>2 μ m is less than 5%, to improve fire retardant emulsion uniformity; Wherein non-ionic surface active agent is one or more mixtures in aliphatic alcohol polyethenoxy, fatty alcohol-polyoxyethylene ether phosphoric acid fat, the polyoxypropylene-polyoxyethylene; Dispersant is one or both mixtures in calgon, the sodium phosphate trimer, and aqueous solvent adopts the soft water after softening.After the fire retardant emulsion preparation,, improve emulsification, dispersant uniformity simultaneously, the fire retardant emulsion that makes can be stirred, grinds, with further raising spinning filtrability of viscose in order to reduce the particle diameter of fire retardant particulate.Spinning adopts the fire retardant quality of the emulsion of said method configuration stable, and is good with the compatible property of the blend of viscose glue, can satisfy explained hereafter fully.
Multistage big multiplying power stretching plasticizing is carried out in the fibre spinning moulding: one-level effectively stretches 10~40%; Secondary effectively stretches 20~70%; Three grades effectively stretch 5~15%, as between can the employing dish, three bathe, the mode of three grades of stretchings of plasticizing.Adopt such mode of stretching oneself and yawn, make the even structure of fiber, increase fibrocortex thickness and outer rim roundness.
Adopt the inventive method to prepare Fire resistant viscose fiber, the fire retardant quality of the emulsion of configuration is stable, good with the compatible property of the blend of viscose glue, fire-retardant spinning solution prepares simple and convenient, the spinning viscose filtration is difficult for stopping up, and has avoided the adding of fire retardant particulate to influence viscose filtration performance and the reduction of powerful index.Adopt low acid, less salt, low temperature, high zinc spinning bath and multistage big multiplying power plasticization drawing, make the even structure of fiber, increase fibrocortex thickness and outer rim roundness.Do not contain halogenic ingredient in the fiber that makes, nontoxic, degradable, discarded back non-environmental-pollution, have the gas permeability similar, dyeability, hygroscopicity to cotton, make its wearability good, thereby and the Fire resistant viscose fiber that adopts the preparation of this method not fusion and charing only takes place avoid the high-temperature fusion dropping that the people is scalded when burning to keep the fiber original form, fire retardant is uniformly dispersed in viscose glue, leave burning things which may cause a fire disaster after, do not glow, easily from putting out.
The specific embodiment
Embodiment one
Produce the 1.67dtex Fire resistant viscose fiber
Will be after grinding average grain diameter be 0.8 ± 0.1 μ m and particle diameter greater than the powder particulate of 2 μ m less than the liquid mixing of 3% fire retardant sulfo-pyrophosphate 40Kg, fatty alcohol-polyoxyethylene ether phosphoric acid fat 6Kg, 0.8Kg calgon and soft water 53L preparation, stir again and grind, make the fire retardant emulsion.And adopt the high quality cotton pulp to make first fibre 8.0%, contain alkali 5.2%, viscosity 52s through conventional viscose manufacturing process, the spinning glue of degree of ripeness 18ml (10%NH4Cl), after filtering, spinning glue the fire retardant emulsion is evenly joined in the spinning glue first fibre 18% with effective fire retardant sulfo-pyrophosphate addition through sound attitude blender, then through sulfuric acid 75g/l, zinc sulfate 35g/l, sodium sulphate 240g/l, coagulation forming in the spinning bath that temperature is 35 ℃, one-level 15% stretches through between dish then; Three bathe secondary 29% stretches; Three grades of plasticizings 12% stretch, and produce qualified fire resistance fibre through concise, oven dry again.Make the fibrous finished product leading indicator: do fracture strength: 〉=2.40cN/dtex; Wet breaking strength: 〉=1.32cN/dtex; Dried elongation at break: 15.2%; Fiber number 1.69dtex; Whiteness: 78%; Oil content: 2.24%; Regain: 10.6%; Limited oxygen index (LOI) 28.4%.
Embodiment two
Produce the 3.33dtex Fire resistant viscose fiber
To grind the back average grain diameter is 0.9 ± 0.1 μ m, and particle diameter greater than 2 μ m powder particulates less than 4.5% fire retardant pyrophosphate 16Kg, polyoxypropylene-polyoxyethylene 4Kg, 0.5Kg calgon mixes with soft water 30L, stir again and grind, make the fire retardant emulsion, adopt the high-quality wood pulps to make first fibre 8.5% through conventional viscose manufacturing process, contain alkali 5.1%, viscosity 41s, the spinning glue of degree of ripeness 20ml (10%NH4Cl), after spinning glue filters operation, the fire retardant emulsion is evenly joined in the spinning glue first fibre 24% with effective fire retardant pyrophosphate addition, then through sulfuric acid 85g/l, zinc sulfate 25g/l, sodium sulphate 280g/l, the coagulating bath moulding that temperature is 42 ℃ stretches through one-level 12%; Secondary 24% stretches; 3 7% stretch, and produce qualified fire resistance fibre through concise, oven dry again.The fibrous finished product leading indicator that makes: do fracture strength: 〉=2.21cN/dtex; Wet breaking strength: 〉=1.14cN/dtex; Dried elongation at break: 19.4%; Fiber number 3.33dtex; Whiteness: 68%; Oil content: 2.28%; Regain: 9.6%; Limited oxygen index (LOI) 32.4%.
Embodiment three
Produce 1.67dtex Fire resistant viscose fiber Fire resistant viscose fiber
To after grinding, average grain diameter be the fire retardant sulfo-pyrophosphate 30Kg of 0.8 ± 0.1 μ m, with polyoxypropylene-polyoxyethylene 5Kg, 0.6Kg sodium phosphate trimer mixes with soft water 45L, stir again and grind, make the fire retardant emulsion, adopt the high-quality wood pulps to make first fibre 8.2% through conventional viscose manufacturing process, contain alkali 5.1%, viscosity 45s, the spinning glue of degree of ripeness 19ml (10%NH4Cl), after spinning glue filters operation, the fire retardant emulsion is evenly joined in the spinning glue first fibre 28% with effective fire retardant sulfo-pyrophosphate addition, then through sulfuric acid 60g/l, zinc sulfate 40g/l, sodium sulphate 260g/l, the coagulating bath moulding that temperature is 32 ℃ stretches through one-level 25%; Secondary 35% stretches; Three grade of 5% stretching produced qualified fire resistance fibre through concise, oven dry again.The fibrous finished product leading indicator that makes: do fracture strength: 〉=2.15cN/dtex; Wet breaking strength: 〉=1.12cN/dtex; Dried elongation at break: 18.6%; Fiber number 1.67dtex; Whiteness: 71%; Oil content: 2.26%; Regain: 9.8%; Limited oxygen index (LOI) 37.3%.

Claims (3)

1. method for preparing flame-proof viscose fiber, it is characterized in that: pyrophosphate based flame retardant particulate, non-ionic surface active agent, dispersant and the aqueous solvent of employing average grain diameter≤1.0 μ m mix and make the fire retardant emulsion, wherein each percentage by weight is respectively pyrophosphate based flame retardant 20-45wt%, non-ionic surface active agent 5-10wt%, dispersant 0.5-1.0wt%, surplus is an aqueous solvent; To mix in the spinning solution that make after the fire retardant emulsion is filtered with relative first fibre 15~30% addings of pyrophosphate based flame retardant; Adopt sulfuric acid 50~90g/l, sodium sulphate 230~290g/l, zinc sulfate 15~45g/l afterwards, the spinning bath spinning moulding that temperature is 30~45 ℃.
2. method for preparing flame-proof viscose fiber according to claim 1, it is characterized in that: the powder particulate of particle diameter in the pyrophosphate based flame retardant particulate>2 μ m is less than 5%.
3. method for preparing flame-proof viscose fiber as claimed in claim 1 or 2, it is characterized in that: stretch after the fibre spinning moulding: one-level effectively stretches 10~40%; Secondary effectively stretches 20~70%; Three grades effectively stretch 5~15%.
CNA2007101165124A 2007-12-27 2007-12-27 Method for preparing flame-proof viscose fiber Pending CN101215726A (en)

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Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011026159A1 (en) 2009-09-01 2011-03-10 Lenzing Ag Fire-retardant cellulose fiber, use thereof, and method for the production thereof
CN102505169A (en) * 2011-10-26 2012-06-20 阜宁澳洋科技有限责任公司 Flame-retardant viscose fiber and preparation method thereof
CN102644125A (en) * 2012-04-10 2012-08-22 山东银鹰化纤有限公司 Method for preparing polychromatic viscose fibers
CN102965751A (en) * 2012-12-20 2013-03-13 唐山三友集团兴达化纤有限公司 High-wet-modulus and flame-retardant regenerated cellulose fibers and preparation method thereof
CN103614795A (en) * 2013-11-25 2014-03-05 常熟市金羽纤维制品厂 Flame-retardant viscose fiber
TWI561693B (en) * 2012-02-24 2016-12-11
CN106400148A (en) * 2016-11-16 2017-02-15 安徽依采妮纤维材料科技有限公司 Viscose fabric good in flame resistance
CN106400149A (en) * 2016-11-16 2017-02-15 安徽依采妮纤维材料科技有限公司 Flame-retardant viscose fabric
CN106591988A (en) * 2016-11-16 2017-04-26 安徽依采妮纤维材料科技有限公司 Viscose fabric
CN106591987A (en) * 2016-11-16 2017-04-26 安徽依采妮纤维材料科技有限公司 High flame retardant viscose fabric
CN106637458A (en) * 2016-11-16 2017-05-10 安徽依采妮纤维材料科技有限公司 High-flame-retardancy viscose fabric
CN106702511A (en) * 2016-11-16 2017-05-24 安徽依采妮纤维材料科技有限公司 Flame-retardant mucilage glue fabric
CN106757457A (en) * 2016-11-16 2017-05-31 安徽依采妮纤维材料科技有限公司 A kind of good viscose fabric of fire resistance
CN106757458A (en) * 2016-11-16 2017-05-31 安徽依采妮纤维材料科技有限公司 A kind of viscose fabric
CN107938010A (en) * 2017-10-30 2018-04-20 宜宾丝丽雅股份有限公司 A kind of high-intensity fine denier flame retardant viscose fiber and its production technology
CN108532015A (en) * 2018-04-20 2018-09-14 唐山三友集团兴达化纤有限公司 A kind of method and flame retardant viscose fiber preparing flame retardant viscose fiber based on self-assembling technique
CN109487362A (en) * 2018-11-30 2019-03-19 山传雷 A kind of inorganic fire-retarded phase-change energy-storage fibre cellulose fiber and preparation method thereof
CN110067034A (en) * 2019-04-22 2019-07-30 东华大学 A kind of fire-retardant regenerated cellulose fiber and preparation method thereof
CN114990718A (en) * 2022-06-24 2022-09-02 江南大学 Halogen-free environment-friendly compound flame-retardant viscose fiber and preparation method thereof

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011026159A1 (en) 2009-09-01 2011-03-10 Lenzing Ag Fire-retardant cellulose fiber, use thereof, and method for the production thereof
CN102505169A (en) * 2011-10-26 2012-06-20 阜宁澳洋科技有限责任公司 Flame-retardant viscose fiber and preparation method thereof
TWI561693B (en) * 2012-02-24 2016-12-11
CN102644125A (en) * 2012-04-10 2012-08-22 山东银鹰化纤有限公司 Method for preparing polychromatic viscose fibers
CN102644125B (en) * 2012-04-10 2014-01-08 山东银鹰化纤有限公司 Method for preparing polychromatic viscose fibers
CN102965751A (en) * 2012-12-20 2013-03-13 唐山三友集团兴达化纤有限公司 High-wet-modulus and flame-retardant regenerated cellulose fibers and preparation method thereof
CN102965751B (en) * 2012-12-20 2015-05-20 唐山三友集团兴达化纤有限公司 High-wet-modulus and flame-retardant regenerated cellulose fibers and preparation method thereof
CN103614795A (en) * 2013-11-25 2014-03-05 常熟市金羽纤维制品厂 Flame-retardant viscose fiber
CN106637458A (en) * 2016-11-16 2017-05-10 安徽依采妮纤维材料科技有限公司 High-flame-retardancy viscose fabric
CN106400149A (en) * 2016-11-16 2017-02-15 安徽依采妮纤维材料科技有限公司 Flame-retardant viscose fabric
CN106591988A (en) * 2016-11-16 2017-04-26 安徽依采妮纤维材料科技有限公司 Viscose fabric
CN106591987A (en) * 2016-11-16 2017-04-26 安徽依采妮纤维材料科技有限公司 High flame retardant viscose fabric
CN106400148A (en) * 2016-11-16 2017-02-15 安徽依采妮纤维材料科技有限公司 Viscose fabric good in flame resistance
CN106702511A (en) * 2016-11-16 2017-05-24 安徽依采妮纤维材料科技有限公司 Flame-retardant mucilage glue fabric
CN106757457A (en) * 2016-11-16 2017-05-31 安徽依采妮纤维材料科技有限公司 A kind of good viscose fabric of fire resistance
CN106757458A (en) * 2016-11-16 2017-05-31 安徽依采妮纤维材料科技有限公司 A kind of viscose fabric
CN107938010A (en) * 2017-10-30 2018-04-20 宜宾丝丽雅股份有限公司 A kind of high-intensity fine denier flame retardant viscose fiber and its production technology
CN108532015A (en) * 2018-04-20 2018-09-14 唐山三友集团兴达化纤有限公司 A kind of method and flame retardant viscose fiber preparing flame retardant viscose fiber based on self-assembling technique
CN108532015B (en) * 2018-04-20 2021-03-05 唐山三友集团兴达化纤有限公司 Method for preparing flame-retardant viscose fiber based on self-assembly technology and flame-retardant viscose fiber
CN109487362A (en) * 2018-11-30 2019-03-19 山传雷 A kind of inorganic fire-retarded phase-change energy-storage fibre cellulose fiber and preparation method thereof
CN109487362B (en) * 2018-11-30 2021-06-15 青岛邦特生态纺织科技有限公司 Inorganic flame-retardant phase-change energy-storage cellulose fiber and preparation method thereof
CN110067034A (en) * 2019-04-22 2019-07-30 东华大学 A kind of fire-retardant regenerated cellulose fiber and preparation method thereof
CN110067034B (en) * 2019-04-22 2021-09-21 东华大学 Flame-retardant regenerated cellulose fiber and preparation method thereof
CN114990718A (en) * 2022-06-24 2022-09-02 江南大学 Halogen-free environment-friendly compound flame-retardant viscose fiber and preparation method thereof
CN114990718B (en) * 2022-06-24 2023-11-28 江南大学 Halogen-free environment-friendly compound flame-retardant viscose fiber and preparation method thereof

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