CN1323197C - Method for preparing viscose filament yarm from electron radiation pulp sheet - Google Patents

Method for preparing viscose filament yarm from electron radiation pulp sheet Download PDF

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CN1323197C
CN1323197C CNB2004100203303A CN200410020330A CN1323197C CN 1323197 C CN1323197 C CN 1323197C CN B2004100203303 A CNB2004100203303 A CN B2004100203303A CN 200410020330 A CN200410020330 A CN 200410020330A CN 1323197 C CN1323197 C CN 1323197C
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pulp
spinning
viscose
radiation
filament yarn
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CN1600909A (en
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王三元
鹿红岩
田文智
孙立
许凤文
李静
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Baoding Swan Fiber Co Ltd
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Baoding Swan Co Ltd
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Abstract

The present invention relates to a method for preparing viscose filament yarn by radiating pulp with electrons, which belongs to the technical field of textile technology. The present invention solves is used for solving the problems of long production period and large consumption of chemical solvent in the producing process of viscose filament yarn. The present invention has the technical scheme that The present invention adopts pulp treated by electronic radiation modification, the radiation level is from 7 to 15KGY, and the weight of a homogeneous reactor is from 8 to 10kg. The present invention adopts the pulp treated by electronic radiation modification as raw material for production, the cellulose hydroxy groups are easy to bond with the molecules of solvent, and simultaneously, cellulose molecules are activated, which is favourable for forming cellulose xanthic acid with lower content of NaOH and CS2. With the invented method, the aging time can be omitted or shortened according to the degree of radiation, the dosage of the CS2 in etiolation reaction is reduced by 14 to 38%, the dosage of the NaOH in the process of alkalizing the pulp is reduced by about 8%, and thereby, the production period is shortened, the production efficiency is increased, few toxic materials are discharged, the prepared viscose is uniform and stable, and the spun viscose filament yarn has good quality.

Description

A kind of electron radiation pulp prepares the method for viscose filament yarn
Technical field
The present invention relates to a kind of manufacture method of textile raw material, particularly utilize the physical modification pulp to prepare the method for viscose filament yarn, belong to textile technology field.
Background technology
Viscose filament yarn is a kind of colory textile raw material, have good moisture absorption, ventilative, gentle performance such as feel well, dangle with its textiles that is made into, and good dyeability, antistatic behaviour and beautiful pleasant gloss, these characteristics be many synthetic fiber can not compare.But traditional cellulose viscose manufacturing technique of continuing to use so far exists that process cycle is long, production efficiency is low, a large amount of CS that use in the production process 2Deng problems such as harmful chemical pollute, these problems have restricted the development of viscose.Along with the increase of viscose output, the low and problem of environmental pollution of production efficiency is on the rise, and the waste gas that produces in the production process, waste water treatment fail to obtain obvious effects so far, and the sustainable development of viscose has been subjected to acid test.For this reason, the insider is in the research that steps up the regenerated cellulose production process, its research emphasis is to adopt novel innoxious solvent contaminated solution problem on the one hand, be to utilize correlation technique that cellulose is carried out modification to handle on the other hand, improve its respond, thereby improve traditional viscose production method, shorten the production cycle, and can reduce the use amount of noxious material, pollution is dropped to than low degree.Described cellulosic modification comprises chemical modification and physical modification, and the chemical reagent that the former uses has toxicity more, and reaction is comparatively complicated, so the researcher is more prone to mechanical lapping, microwave ultrasonic wave processing, electron radiation, CO 2First supercritical processing, steam dodge the physical modification aspect of methods such as quick-fried processing and explore.
Summary of the invention
The purpose of this invention is to provide a kind of with short production cycle, method that electron radiation pulp that the chemical solvent consumption is few prepares viscose filament yarn.
The alleged problem of the present invention is solved by following technical scheme:
A kind of electron radiation pulp prepares the method for viscose filament yarn, and its master operation comprises: a. dipping and pulverizing: after pulp is flooded in aqueous slkali, through squeezing, pulverizing, make alkali cellulose; B. experienced, yellow: experienced degraded of alkali cellulose and CS 2Reaction obtains cellulose xanthate; C. cellulose xanthate dissolving: adding dissolving alkali and water are made viscose glue in cellulose xanthate; D. maturation: viscose filtration, maturation, deaeration form spinning glue; E. spinning: spinning glue is decomposed under the acid bath effect, regenerates, be spun into spinning cake through spinning machine; F. post processing, processing: spinning cake is processed into the tube silk after drip washing, oven dry are handled, its special feature is: described pulp carries out the electron radiation modification to be handled, and radiation level is 7~15KGY, and homogeneous reactor weight is 8~10Kg.
Above-mentioned electron radiation pulp prepares the method for viscose filament yarn, and in described experienced operation, ageing time was 8~3 hours when radiation level was 7~10 KGY levels, and ageing time was zero when radiation level was 11~15KGY level.
Above-mentioned electron radiation pulp prepares the method for viscose filament yarn, and in described yellow operation, alkali cellulose is the wet method yellow, initial temperature: 18~23 ℃, warm eventually: 28~31 ℃, and time: 90~140min, CS 2Addition to α-cell: 22%~30.5%, viscose glue is formed: α-cell:7.60~8.60%, NaOH:5.60~6.00%, S:1.60%~2.20%.
Above-mentioned electron radiation pulp prepares the method for viscose filament yarn, in described dipping operation, impregnation concentration: 190.0~240.0g/L, temperature: 17~20 ℃, time: 60~120min, alkali cellulose is formed: α-cell:28.00~33.00 ± 0.50%, NaOH:14.00~18.00 ± 0.50%.
Above-mentioned electron radiation pulp prepares the method for viscose filament yarn, in described maturation operation, and spinning glue degree of ripeness: 7.6~9.5ml, viscosity: 28~50 seconds.
Above-mentioned electron radiation pulp prepares the method for viscose filament yarn, and in described spinning process, spinning coagulation bath is formed: H 2SO 4: 128.0~138.0 ± 1.0 g/L, ZnSO 4: 10.0~12.5 ± 0.5g/L, Na 2SO 4: 260~290g/L, bathe temperature: 48~56 ± 1 ℃.
The present invention has improved the preparation method of existing viscose filament yarn, the pulp that it is handled with the modification of electron radiation technology is raw materials for production, through radiation treatment, this pulp has changed the structure of fibril aggregation attitude, the cellulose hydroxyl is more prone to combining of solvent molecule, cellulosic molecule is activated simultaneously, helps the formation of cellulose xanthate.Adopt the electron radiation pulp to prepare viscose filament yarn, can be shortened by the radiation degree or save experienced operation according to pulp, and make CS in the yellow reaction 2Consumption reduce 14~38%, it is about 8% that the consumption of pulp alkalization NaOH reduces, thereby effectively shorten the production cycle, enhances productivity, and reduces the discharging of noxious material, and make the viscose glue that makes more uniform and stable.After testing, the made viscose glue good spinning property of this method reaches conventional spinning level fully, and finished silk can reach international Grade A level.
Technical essential of the present invention is to adopt pulp through electron radiation as raw materials for production, cooperates the production technology that adapts with it, efficiently prepares the viscose filament yarn identical in quality with the common process method.Its principle is: pulp is under the radiation effects of high-power electron beam, and the strand of crystal region and noncrystalline domain evenly ruptures, and is destroyed with intramolecular hydrogen bond between the molecule, changed fiber collection attitude structure, makes cellulosic hydroxy and alkali and CS 2The combination of molecule is more prone to, and simultaneously in the high-power electron beam processing procedure, electron beam passes to atom in the molecule with energy, and fiber molecule is activated, and has reduced the molecule activation energy, and molecular motion is activated, and helps at lower NaOH and CS 2The formation of cellulose xanthate under the concentration, and side reaction is suppressed.After adopting electron radiation technical finesse cellulose pulp, cellulosic degree of polymerization is evenly degraded, and helps the yellow successful reaction and carries out, and made viscose glue is uniform and stable.
Adopt the electron radiation pulp, should take all factors into consideration various factors such as production efficiency, economic benefit, rationally select required electron radiation dosage of pulp modification and pulp homogeneous reactor weight for use, make pulp performance and technical indicator after the modification be applicable to viscose filament yarn production.Homogeneous reactor be meant if with the pulp between of a certain pulp of pulp parcel and the top after radiation, the molecule aggregation degree and the activation degree that are obtained can reach the relative body of piling uniformly.Through testing the Comprehensive Assessment that reaches experimental index repeatedly, determine that dosage of radiation is 7~15KGY, homogeneous reactor weight 8~10Kg is advisable.Compare with common process, experienced operation shortened to 3~8 hours by original 21 hours when the pulp radiation level was 7~10KGY, and shortening amount is 61.9%~85.7%, can save experienced operation when the pulp radiation level is 11~15KGY.The CS2 consumption reduces with the raising of radiation level in the yellow operation, and common pulp CS2 consumption is 35.5%, and electron radiation pulp CS2 consumption is 30.5~22.0%, and reduction is 14.1%~38%; Sheet steeping liquid concentration NaOH consumption is reduced to 220~190g/l by former 240g/1, reduces about 8%.
Adopt the electron radiation pulp, the production process of viscose filament yarn needs good stability of spinning process of the process combination ability electron gain radiation viscose filament yarn of rational yellow technology, viscose glue physical and chemical indexes, coagulation bath condition and spinning condition and qualified end product quality.Adopt the finished silk kind of the inventive method preparation: the semicontinuous bright yarn of 66.7~666.7dtex/18~120f, dull yarn, finished silk physical and chemical indexes: fiber number deviation :≤± 2.5%, do strong: 〉=1.80CN/dtex, wet strong: 〉=0.80 CN/dtex, dried stretching: 〉=14.5%, monofilament deviation: 〉=3.0 grades of≤2.0% dyeing, residual sulphur :≤10mg/g.
The specific embodiment
The embodiment of several production electron radiation viscose filament yarns is provided below;
One. technical process: 1. radiation modification pulp; 2. dipping, squeezing, pulverizing; 3. alkali cellulose; 4. experienced; 5. yellow, dissolving; 6. viscose glue; 7. back dissolving; 8. filter; 9. deaeration, maturation; 10. spinning glue; 11. spinning; 12. spinning cake; 13. drip washing; 14. oven dry; 15. become tube.
Two. capital equipment:
Pulp is made: high-energy electron accelerator
Alkali cellulose is made: classic steeping press, thickness pulverizer
Viscose glue is made: dissolving machine, blender, flame filter press, deaerator are mediated in yellow
Spinning: semi-continuous centrifugal formula spinning machine
Post processing, processing: leaching machine, Water Extraction Machinery, dryer, bobbin winder
Three. the main technique condition
Embodiment 1. pulp radiation level 7KGY:
1, alkali is fine makes:
Maceration extract: NaOH concentration 240.0 ± 1.0g/L temperature: 18.0 ± 0.5 ℃
Dip time: 120min
Alkali cellulose is formed: α-cell (methylcellulose): 30.00 ± 0.50%
NaOH:17.30±0.30%
Ageing time: 8 hours experienced temperature: 25.5 ± 0.5 ℃
Experienced mode: constant temperature leaves standstill experienced
Alkali cellulose cuprammonium viscosity: 50~60mp
2, viscose glue manufacturing:
Yellow method: wet method yellow method
Temperature: initial temperature: 20.0 ± 0.5 ℃, warm eventually: 29.5~30.5 ℃
The yellow time: 120min
CS 2Addition: 30.5% (to α-cell)
Viscose glue is formed: α-cell:8.00 ± 0.30% NaOH:5.80 ± 0.10%, S:2.10 ± 0.05%
Spinning glue: degree of ripeness: 8.0 ± 0.3ml (10%NH 4Cl)
Viscosity 32~42 seconds (18 ℃ of falling ball viscosities)
3, spinning:
Spinning form: semicontinuous spinning
Kind: 133.3dtex/30f
Spin speed: 81~83m/min
Drawing-off: 25% nervous drawing-off: 2.67%
Acid bath condition: H 2SO 4: 132.0 ± 1.0g/L ZnSO 4: 11.5 ± 0.5g/g
Na 2SO 4: 265.0 ± 5.0 g/L bathe temperature: 52.0 ± 1.0 ℃
4, finished silk physical and chemical indexes:
The fiber number deviation :-0.5%, do strong: 2.05CN/dtex is wet strong: 0.98 CN/dtex, dried stretching: 16.6%, the monofilament deviation: 0, dye 3.5 grades residual sulphur: 6.8mg/g.
Embodiment 2. pulp radiation level 10KGY:
1, alkali is fine makes:
Maceration extract: NaOH concentration 220.0 ± 1.0g/L temperature: 18.0 ± 0.5 ℃
Dip time: 120min
Alkali cellulose is formed: α-cell:30.5 ± 0.50%
NaOH:15.8±0.30%
Ageing time: 3 hours, experienced temperature: 25.5 ± 0.5 ℃
Experienced mode: constant temperature leaves standstill experienced
Alkali cellulose cuprammonium viscosity: 50~60mp
2, viscose glue manufacturing:
The yellow method: wet method yellow method,
Temperature: initial temperature: 22 ± 0.5 ℃, warm eventually: 28.5~30.5 ℃
The yellow time: 120min
CS 2Addition: 29% (to α-cell)
Viscose glue is formed: α-cell:8.30 ± 0.30%, NaOH:5.80 ± 0.10%, S:1.95 ± 0.05%
Spinning glue: degree of ripeness: 8.5 ± 0.3ml (10%NH 4Cl)
Viscosity 32~42 seconds (18 ℃ of falling ball viscosities);
3, spinning:
Spinning form: semicontinuous spinning
Kind: 83.3dtex/18f
Spin speed: 74~76m/min
Drawing-off: 20% nervous drawing-off: 2.67%
Acid bath condition: H 2SO 4: 128.0 ± 1.0g/L ZnSO 4: 11.5 ± 0.5g/LNa 2SO 4: 265.0 ± 5.0g/L bathes temperature: 50.0 ± 1.0 ℃
4, finished silk physical and chemical indexes:
The fiber number deviation :-0.5% does by force: 1.94CN/dtex is wet strong: 0.97 CN/dtex, dried stretching: 16.4%, the monofilament deviation: 0, dye 4.0 grades residual sulphur: 6.1mg/g.
Embodiment 3. pulp radiation level 13KGY:
1, alkali is fine makes:
Maceration extract: NaOH concentration 190g/L temperature: 18.0 ± 0.5 ℃
Dip time: 120min
Alkali cellulose is formed: α-cell:30.00 ± 0.50%
NaOH:14.30±0.30%
Ageing time: 0 hour
Alkali cellulose cuprammonium viscosity: 45~55mp
2, viscose glue manufacturing:
Yellow method: wet method yellow method
Temperature: initial temperature: 20.0 ± 0.5 ℃, warm eventually: 28.5~29.5 ℃
The yellow time: 120min
CS 2Addition: 22% (to α-cell)
Viscose glue is formed: α-cell:8.10 ± 0.30%, NaOH:5.80 ± 0.10%, S:1.70 ± 0.05% spinning glue: degree of ripeness: 8.6 ± 0.3ml (10%NH 4Cl)
Viscosity 32~42 seconds (18 ℃ of falling ball viscosities);
3, spinning:
Spinning form: semicontinuous spinning
Kind: 333.3dtex/60f
Spin speed: 65~70m/min
Drawing-off: 15% nervous drawing-off: 2.67%
Acid bath condition: H 2SO 4: 128.0 ± 1.0g/L ZnSO 4: 11.5 ± 0.5g/LNa 2SO 4: 265.0 ± 5.0g/L bathes temperature: 50.0 ± 1.0 ℃;
4, finished silk physical and chemical indexes:
The fiber number deviation: 0.7%, do strong: 1.92CN/dtex is wet strong: 0.95 CN/dtex, dried stretching: 16.6%, the monofilament deviation: 0, dye 3.5 grades residual sulphur: 5.0mg/g.

Claims (4)

1. an electron radiation pulp prepares the method for viscose filament yarn, and its master operation comprises: a. dipping with pulverize: after pulp flood,, make alkali cellulose through squeezing, pulverizing in aqueous slkali; B. experienced, yellow: experienced degraded of alkali cellulose and CS 2Reaction obtains cellulose xanthate; C. cellulose xanthate dissolving: adding dissolving alkali and water are made viscose glue in cellulose xanthate; D. maturation: viscose filtration, maturation, deaeration form spinning glue; E. spinning: spinning glue is decomposed under the acid bath effect, regenerates, be spun into spinning cake through spinning machine; F. post processing, processing: spinning cake is processed into the tube silk after drip washing, oven dry are handled, it is characterized in that:
Pulp is carried out the electron radiation modification handle radiation level 7~15KGY, homogeneous reactor weight 8~10Kg;
In experienced operation, when radiation level was 7~10KGY level, ageing time was 8~3 hours, and when radiation level was 11~15KGY level, ageing time was zero;
In the yellow operation, alkali cellulose adopts the wet method yellow, and technological parameter is: initial temperature: 18~23 ℃, warm eventually: 28~31 ℃, and time: 90~140min, CS 2To the addition 22%~30.5% of α-cell, viscose glue is formed: α-cell:7.60~8.60%, NaOH:5.60~6.00%, S:1.60%~2.20%.
2. electron radiation pulp according to claim 1 prepares the method for viscose filament yarn, it is characterized in that: in described dipping and pulverizing process, impregnation concentration is 190.0~240.0g/L, 17~20 ℃ of temperature, time 60~120min, alkali cellulose is formed: α-cell:28.00~33.00 ± 0.50%, NaOH:14.00~18.00 ± 0.50%.
3. electron radiation pulp according to claim 2 prepares the method for viscose filament yarn, it is characterized in that: in described maturation operation, and spinning glue degree of ripeness: 7.6~9.5ml, viscosity: 28~50 seconds.
4. electron radiation pulp according to claim 3 prepares the method for viscose filament yarn, it is characterized in that: in described spinning process, spinning coagulation bath is formed: H 2SO 4: 128.0~138.0 ± 1.0g/L, ZnSO 4: 10.0~12.5 ± 0.5g/L, Na 2SO 4: 260~290g/L, bathe temperature: 48~56 ± 1 ℃.
CNB2004100203303A 2004-08-16 2004-08-16 Method for preparing viscose filament yarm from electron radiation pulp sheet Expired - Fee Related CN1323197C (en)

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100402712C (en) * 2005-04-11 2008-07-16 保定天鹅股份有限公司 Viscose filament with abnormal section, preparation method thereof and spinneret assembly
CN108677581A (en) * 2018-04-25 2018-10-19 武汉水木弘新材料有限公司 The method for preparing low polymerization degree low crystallinity cellulose using high-energy electron beam irradiation

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
电子束处理粘胶纤维改性及生产中的应用 程闻博,广西化纤通讯,第2期 2000 *
电子束处理粘胶纤维改性及生产中的应用 程闻博,广西化纤通讯,第2期 2000;电子束辐射技术在粘胶工业中的应用 周瑞敏 唐述祥,辐射研究与辐射工艺学报,第19卷第4期 2001 *
电子束辐射技术在粘胶工业中的应用 周瑞敏 唐述祥,辐射研究与辐射工艺学报,第19卷第4期 2001 *

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Address after: 071055, 1369 West Hing Shing Road, Xinshi District, Hebei, Baoding

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