CN102561031B - Flame retardant viscose fiber and preparation method thereof - Google Patents

Flame retardant viscose fiber and preparation method thereof Download PDF

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CN102561031B
CN102561031B CN 201210024526 CN201210024526A CN102561031B CN 102561031 B CN102561031 B CN 102561031B CN 201210024526 CN201210024526 CN 201210024526 CN 201210024526 A CN201210024526 A CN 201210024526A CN 102561031 B CN102561031 B CN 102561031B
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viscose
flame retardant
viscose fiber
emulsion
preparation
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CN102561031A (en
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宋国新
黄毅
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MODERN AVENUE FASHION GROUP CO., LTD.
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Shanghai Taohong Chemical Technology Co Ltd
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Abstract

The invention discloses a flame retardant viscose fiber and a preparation method thereof. The preparation method of the flame retardant viscose fiber comprises the following steps of adding a flame retardant emulsion into a viscose solution, uniformly mixing, carrying out filtration, and carrying out molding by a conventional wet spinning technology to obtain the flame retardant viscose fiber. A mass ratio of the flame retardant emulsion to the viscose solution is in a range of (1: 100) to (5: 100). The flame retardant emulsion comprises: by weight, 20 to 30 parts of N,N'-di(diphenoxythiophosphoryl)dithioethyldiamide, 5 to 10 parts of tris(2-chloropropyl) phosphate, 10 to 15 parts of cocoamidopropyl betaine, 5 to 10 parts of potassium dodecyl phosphate, 20 to 25 parts of Tween-60, and 500to 800 parts of water. The flame retardant viscose fiber has good flame retardant effects and a high water-retaining capacity.

Description

Fire resistant viscose fiber and preparation method thereof
Technical field
The present invention relates to a kind of viscose and preparation method thereof, relate in particular to a kind of Fire resistant viscose fiber and preparation method thereof.
Background technology
Viscose (viscose fibre) is sticking fine full name.It is divided into viscose filament yarn and short rayon fiber again.Sticking fibre is to be the cellulose fibre of raw material production with cotton or other natural fabric.In 12 kinds of main textile fabrics, sticking fine moisture percentage meets the physiological requirement of human body skin most, have smooth nice and cool, ventilative, antistatic, characteristic such as gorgeous dyes.
Viscose belongs to regenerated celulose fibre.It is to be raw material with the native cellulose, makes the soluble cellulose sulphonic acid ester through operations such as alkalization, aging, sulfonation, is dissolved in sig water again to make viscose glue, makes through wet spinning.Adopt different raw material and spinning technique, can obtain common viscose fiber respectively, koplon and high tenacity staple fibre etc.Common viscose fiber has general physical mechanical performance and chemical property, divides cotton type, wool type and long filament type again, is commonly called as artificial cotton, artificial wool and artificial silk.
Sticking fibre is one of ancient fiber species.In 1891, Kroes (Cross), Buddhist script written on pattra leaves (Bevan) and at first be that raw material has been made sodium cellulose xanghate solution with the cotton than Dare (Beadle) etc., because the viscosity of this solution is very big, thereby called after " viscose glue ".After viscose glue was met acid, cellulose was separated out again.According to this principle, developed into a kind of method of making cellulose fibre in 1893, this fiber just is called " viscose ".By 1905, Miller you (Muller) etc. was invented the coagulating bath of a kind of dilute sulfuric acid and sulfate composition, had realized the suitability for industrialized production of viscose.
The basic composition of viscose is cellulose.The cross section indention skin-core structure of common viscose fiber, vertical straight ditch horizontal stroke that has.And rich fine no skin-core structure, the cross section is rounded.
Viscose has good hygroscopicity, and under the general atmosphere condition, regain is about 13%.Significantly expand after the moisture absorption, the diameter increase can reach 50%, thus under the fabric behind the water feel harden, shrinkage factor is big.The fracture strength of common viscose fiber is littler than cotton, is about 1.6~2.7cN/dtex; Elongation at break is 16%~22% greater than cotton; Wet strong descend manyly, be about and do by force by 50%, the hygrometric state elongation increases about 50%.Its modular ratio cotton is low, easy deformation under little load, and elastic recovery is poor, so fabric extends poor dimensional stability easily.
The chemical composition of viscose is similar to cotton, thus more alkaline-resisting and not acidproof, but alkaline-resisting acid resistance is all poor than cotton.The thermal property of viscose is also similar to cotton in addition, and density is 1.50~1.52g/cm near cotton 3Cellulosic macromolecular hydroxyl is easy to take place the number of chemical reaction, therefore, can carry out modification to viscose by methods such as grafting, improves the viscose performance, and produces the fiber of various specific uses.
Yet existing viscose is not more and more approved by market owing to function singleness.Therefore, urgent expectation can be developed high performance industry function viscose fiber, promotes the surcharge of viscose, to satisfy the needs of the more and more polynary change of people.
Summary of the invention
In order to solve the prior art above shortcomings, one of technical problem to be solved by this invention provides a kind of preparation method of Fire resistant viscose fiber.
Two of technical problem to be solved by this invention provides above-mentioned Fire resistant viscose fiber, has good flame retardation effect, the high outstanding advantage of water-retaining property.
Technical scheme of the present invention is achieved in that
The preparation method of Fire resistant viscose fiber, be made up of following step:
The anti-flammability emulsion is joined in the viscose solution, mix, filter, wet spinning spray silk technological forming obtains Fire resistant viscose fiber of the present invention routinely, and the mass ratio of described anti-flammability emulsion and viscose solution is 1: 100~5: 100;
Wherein, described anti-flammability emulsion, formed by weight by following component:
N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide 20-30 part; Tricresyl phosphate (2-chloropropyl) ester 5-10 part; Cocamidopropyl propyl amide dimethyl betaine 10-15 part; 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite 5-10 part; Tween-60 20-25 part; Water 500-800 part.
With N; N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide, tricresyl phosphate (2-chloropropyl) ester, cocamidopropyl propyl amide dimethyl betaine, 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite and Tween-60 mix; with the ball mill ball milling after 3-5 hour; add water; mix again, can make this anti-flammability emulsion.
In the present invention, described viscose solution refers to the sodium hydrate aqueous solution of cellulose sulfonate, and it is the general intermediate raw material of the industry.
Preferably, in the described viscose solution, the weight percent content of first fibre is 8-9%, and the weight percent content of alkali is 4-6%, falling ball viscosity 45-65 second, degree of ripeness 8-16%.
Preferably, adopt filter to filter, its filtering accuracy is≤4 μ m.
The present invention also provides a kind of Fire resistant viscose fiber, adopts method for preparing to form.
With respect to prior art, beneficial effect of the present invention is embodied as:
Fire resistant viscose fiber of the present invention has good flame retardation effect, the high outstanding advantage of water-retaining property.
The specific embodiment
Embodiment 1
(1) preparation of anti-flammability emulsion
N, 20 kilograms of N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide; 10 kilograms of tricresyl phosphate (2-chloropropyl) esters; 10 kilograms of cocamidopropyl propyl amide dimethyl betaines; 10 kilograms of 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite; 20 kilograms of Tween-60s; 800 kilograms in water.
With N; N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide, tricresyl phosphate (2-chloropropyl) ester, cocamidopropyl propyl amide dimethyl betaine, 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite and Tween-60 mix; with the ball mill ball milling after 3 hours; add water; mix again, can make this anti-flammability emulsion.
(2) preparation of Fire resistant viscose fiber
The anti-flammability emulsion is joined in the viscose solution, mix, filter, wherein filtering accuracy is≤4 μ m, and wet spinning spray silk technological forming obtains Fire resistant viscose fiber of the present invention routinely, and the mass ratio of described anti-flammability emulsion and viscose solution is 5: 100.
In the described viscose solution, the weight percent content of first fibre is 8%, and the weight percent content of alkali is 6%, falling ball viscosity 45 seconds, degree of ripeness 16%.
Comparative Examples 1:
Viscose solution is filtered, and wet spinning spray silk technological forming obtains viscose routinely.
In the described viscose solution, the weight percent content of first fibre is 8%, and the weight percent content of alkali is 6%, falling ball viscosity 45 seconds, degree of ripeness 16%.
Embodiment 2
(1) preparation of anti-flammability emulsion
N, 30 kilograms of N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide; 5 kilograms of tricresyl phosphate (2-chloropropyl) esters; 15 kilograms of cocamidopropyl propyl amide dimethyl betaines; 5 kilograms of 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite; 25 kilograms of Tween-60s; 500 kilograms in water.
With N; N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide, tricresyl phosphate (2-chloropropyl) ester, cocamidopropyl propyl amide dimethyl betaine, 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite and Tween-60 mix; with the ball mill ball milling after 5 hours; add water; mix again, can make this anti-flammability emulsion.
(2) preparation of Fire resistant viscose fiber
The anti-flammability emulsion is joined in the viscose solution, mix, filter, wherein filtering accuracy is≤3 μ m, and wet spinning spray silk technological forming obtains Fire resistant viscose fiber of the present invention routinely, and the mass ratio of described anti-flammability emulsion and viscose solution is 1: 100.
In the described viscose solution, the weight percent content of first fibre is 9%, and the weight percent content of alkali is 4%, falling ball viscosity 65 seconds, degree of ripeness 8%.
Comparative Examples 2:
Viscose solution is filtered, and wet spinning spray silk technological forming obtains viscose routinely.
In the described viscose solution, the weight percent content of first fibre is 9%, and the weight percent content of alkali is 4%, falling ball viscosity 65 seconds, degree of ripeness 8%.
Test case
Project Embodiment 1 Comparative Examples 1 Embodiment 2 Comparative Examples 2
Water-retaining property (%) 77 82 79 84
The LOI value 29 18.5 28 18.5
After flame time (second) 0.2 0.3
Glow the time (second) 0.4 0.4
Press GB/T5455-1997 " textile combustion performance test normal beam technique " standard test, the fiber combustion characteristic is charing, does not have dropping during the sample burning, tests after flame time and glows the time.
By last table as seen, fire resistance excellence of the present invention, more crucial is that water-retaining property of the present invention only descends about 5% with respect to the more conventional viscose decline of existing fire resistance fibre water-retaining property 10-15%, fully can with directly, reduction and reactive dyeing.

Claims (3)

1. the preparation method of Fire resistant viscose fiber, be made up of following step:
The anti-flammability emulsion is joined in the viscose solution, mix, filter, wet spinning spray silk technological forming obtains described Fire resistant viscose fiber routinely, and the mass ratio of described anti-flammability emulsion and viscose solution is 1:100~5:100;
It is characterized in that described anti-flammability emulsion is made of by weight following component:
N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide 20-30 part; Tricresyl phosphate (2-chloropropyl) ester 5-10 part; Cocamidopropyl propyl amide dimethyl betaine 10-15 part; 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite 5-10 part; Tween-60 20-25 part; Water 500-800 part.
2. the preparation method of Fire resistant viscose fiber as claimed in claim 1, it is characterized in that: in the described viscose solution, the weight percent content of first fibre is 8-9%, and the weight percent content of alkali is 4-6%, falling ball viscosity 45-65 second, degree of ripeness 8-16%.
3. Fire resistant viscose fiber is characterized in that: adopt claim 1 or 2 described methods to be prepared from.
CN 201210024526 2012-02-03 2012-02-03 Flame retardant viscose fiber and preparation method thereof Active CN102561031B (en)

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CN103284368A (en) * 2013-05-13 2013-09-11 上海特安纶纤维有限公司 Blended flame-retardant fabric and flame-retardant protecting clothes
CN103306030A (en) * 2013-05-13 2013-09-18 上海特安纶纤维有限公司 Blended fabric of polysulfonamide and viscose fiber
CN103388224B (en) * 2013-08-05 2015-07-15 宁波格兰家居用品有限公司 Blended fabric of antiflaming vinylon and antiflaming viscose
CN103397534B (en) * 2013-08-05 2016-05-04 上海婉静纺织科技有限公司 The blend fabric of Fanglun l414 and anti-flaming viscose
CN103361870B (en) * 2013-08-05 2015-07-29 上海婉静纺织科技有限公司 The BLENDED FABRIC of Ju Fang oxadiazole and anti-flaming viscose
CN103361996B (en) * 2013-08-05 2015-11-18 上海婉静纺织科技有限公司 The BLENDED FABRIC of Vinyon N and anti-flaming viscose
CN103361832B (en) * 2013-08-05 2015-08-12 上海婉静纺织科技有限公司 The BLENDED FABRIC of PEI and anti-flaming viscose
CN103361833B (en) * 2013-08-05 2015-07-29 上海婉静纺织科技有限公司 The BLENDED FABRIC of meta-aramid and anti-flaming viscose
CN103361994B (en) * 2013-08-05 2016-08-03 上海婉静纺织科技有限公司 Thermal resistant fire resistant fibric
CN103388267B (en) * 2013-08-05 2015-11-18 上海婉静纺织科技有限公司 The BLENDED FABRIC of polyphenylene sulfide and anti-flaming viscose
CN103361995B (en) * 2013-08-05 2015-11-18 上海婉静纺织科技有限公司 The BLENDED FABRIC of basalt fibre and anti-flaming viscose
CN103361856B (en) * 2013-08-05 2015-08-26 上海婉静纺织科技有限公司 The BLENDED FABRIC of PSA fiber and anti-flaming viscose

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CN101387013A (en) * 2008-05-14 2009-03-18 中原工学院 Environment friendly flame-retardant viscose fiber manufacturing technology
CN101701423A (en) * 2009-10-28 2010-05-05 长春工业大学 Phosphorus flame retardant for viscose fibers and production method and application thereof
CN101851804A (en) * 2010-05-24 2010-10-06 杭州奥通科技有限公司 Method for producing fire-retardant anti-melt viscose fibers

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CN101387013A (en) * 2008-05-14 2009-03-18 中原工学院 Environment friendly flame-retardant viscose fiber manufacturing technology
CN101701423A (en) * 2009-10-28 2010-05-05 长春工业大学 Phosphorus flame retardant for viscose fibers and production method and application thereof
CN101851804A (en) * 2010-05-24 2010-10-06 杭州奥通科技有限公司 Method for producing fire-retardant anti-melt viscose fibers

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