CN1061106C - Method for producing cellulose fiber by dissolvant method - Google Patents
Method for producing cellulose fiber by dissolvant method Download PDFInfo
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- CN1061106C CN1061106C CN97107819A CN97107819A CN1061106C CN 1061106 C CN1061106 C CN 1061106C CN 97107819 A CN97107819 A CN 97107819A CN 97107819 A CN97107819 A CN 97107819A CN 1061106 C CN1061106 C CN 1061106C
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- dissolvant
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- spinning solution
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Abstract
The present invention relates to a method for preparing a spinning solution from directly dissolving cellulose pulp by using N-methyl morpholine oxides, water is used as a coagulator to prepare the spinning solution, and water is also used as a coagulator to prepare artificial fibers. The present invention is a preparation technology with nontoxic solvents, no pollution, recoverable solutions to use, high efficiency in fiber production, no toxicity and environmental protection; cellulose fibers prepared from the present invention have smooth surface, good luster, integral circular sections for fibers, higher dry and wet fracture strength, higher dry and wet strength ratio, proper elongation rate, excellent hydroscopic property and good chromaticity, and the fabrics have favorable size stability, tear resistance and wrinkle resistance; additionally, the present invention has a wide application in the clothing field.
Description
The present invention relates to a kind of material manufacturing method of textile industry.The manufacture method of cellulose fiber by solvent method particularly.
The cellulose fiber fiber products is merrily and lightheartedly soft, and gloss is quiet and tastefully laid out, good hygroscopicity, comfortable and easy to wear, be subjected to domestic and international consumer's welcome deeply, but because the natural material-cotton shortage of produce cellulose fibers goods, can not satisfy the needs of people life, people then seek a kind of raw material that replaces cotton.All once developed common viscose fiber both at home and abroad, comprise staple fibre and long filament, it is a kind of regenerated celulose fibre preferably, but poisonous and hazardous industrial chemicals carbon disulfide, sulfuric acid and caustic soda have been used on the common viscose fiber raw material, carbon disulfide that gives off in process of production and hydrogen sulfide not only have more serious damaging effect to health, and atmosphere, water source and environment are had huge contamination.In addition, serious etching apparatus, the pipeline of strong acid and strong base meeting that uses in the production process.So the viscose manufacturing enterprise of various countries is progressively closing or stopping production, world's viscose output is reducing year by year.
The inventor's novelty assessment report is as follows:
Put forward characteristics according to this class, select to have determined term and range of search, external part has been retrieved world patent Suo Li, U.S. chemical abstract, engineering index, four databases of United States Government report by light disk retrieval, finds 30 pieces of pertinent literatures altogether.From the document result who retrieves, the external document of N-methyl morpholine oxide solvent method artificial fibre spinning that adopts is more, wherein a part of documents the influence of solvent spinning to physical property and mechanical performance, a part has been studied this novel solvent spinning technique in addition.The content of all bibliographical informations all is that the particular content that relates to textile technology does not appear in the newspapers around N-methyl morpholine oxide solution development method and its physical property or the like; Domestic part is by Chinese technical journal piece of writing name database CD and other abstract journal, find altogether with this class and carry 10 pieces in relevant document, from the document result who retrieves, except the introduction with N-methyl morpholine oxide solvent method artificial fibre, other all is summary and imagination property article.
The object of the present invention is to provide a kind of employing N-methyl morpholine oxide and cellulose pulp co-blended spinning, make the manufacture method of regenerated celulose fibre.
Main raw material of the present invention is N-methyl morpholine oxide, pulp, water.
A kind of method for producing cellulose fiber by dissolvant method: it is 0.1～0.5cm that pulp is ground into area
2, the chip about thickness 1mm; The stirring of N-methyl morpholine oxide is dissolved, temperature is controlled at 75～90 ℃, get pulp in the solid weight ratio then: the N-methyl morpholine oxide is that 1: 20～1: 24 ratio drops into stirring and dissolving in the N-methyl morpholine oxide solution with pulp, its temperature is controlled at 75～90 ℃, dissolution time was controlled at 6～12 hours, made spinning solution; Above-mentioned spinning solution is extruded through dual-screw-stem machine, enters casing through fondant filter again, and spinning solution measures through measuring pump in casing, from the spinnerets ejection, enters and solidifies the formation strand in solvent-water-bath; Wherein, the temperature of each district of dual-screw-stem machine, filter, spinning manifold is controlled at 110 ℃; The spinnerets specification: bore dia 0.10-0.23mm, hole count is 400-650 hole/plate, the distance between spinning plate and coagulating bath liquid level is air gap, is controlled at 7-400mm; Spinning solution removes bubble at dual-screw-stem machine through the mouth of finding time, and further dissolving, above-mentioned strand carries out spinneret draft through winding apparatus, its extensibility is controlled at-20%-250%, stretch through filling with in the traction grooved that temperature is controlled at 75-95 ℃ of water, its extensibility is controlled at 15%-100% again again; Strand is the remaining solvent of flush away in the drawing process again; Strand send cutting machine to cut into the staple fibre that length is 32.6～299.4mm after squeezing again; Staple fibre temperature after the cut-out is that 35-90 ℃ soft water washing was dewatered, oils, dewaters, dried in 30-60 minute, promptly makes finished fiber.
Described a kind of method for producing cellulose fiber by dissolvant method is characterized in that: by weight, and finished fiber fiber content 87%-89%, water content 11%-13%.
Described a kind of method for producing cellulose fiber by dissolvant method is characterized in that: with dissolving spinning equipment spinning fibre cellulose fiber.
Described a kind of method for producing cellulose fiber by dissolvant method is characterized in that: dewater at staple fibre, oil, in the dehydration, drying course, oil bath concentration is 0.15-0.80g/l, and bake out temperature is a normal temperature-105 ℃, and drying time is 6-20 hour.
By the cellulose fiber by solvent method that said method makes, its fiber is 1.5d, and dried fracture strength is 4g/d, and wet breaking strength is 3.2g/d, and dried elongation at break is 14%, and regain is 13%.Fiber is white in color, and bright in color is soft, and is smooth.
The cellulose fibre that the present invention makes, smooth surface, good luster, fiber has complete circular section, have higher do, wet breaking strength and do, wet strong ratio, and suitable percentage elongation, hygroscopicity and dyeability are good, and its fabric has good DIMENSIONAL STABILITY, tear resistance, anti-crease property.Be with a wide range of applications at garment industry.
The technical process that the present invention makes cellulose fibre than traditional cellulose viscose manufacturing technique process decreased number 2/3rds, thereby production process equipment, floor space, energy consumption are reduced significantly, the production cycle shortens, production efficiency significantly improves; Simultaneously, traditional viscose production is better overcome because of a large amount of problems such as carbon disulfide, sulfuric acid, the caused toxicity of caustic soda are big, seriously corroded, contaminated environment of using.
Below by embodiment the present invention is further described:
It is 0.1-0.5cm that pulp is ground into area
2, the chip about thickness 1mm; The 86.94kgN-methyl morpholine oxide is put into the dissolution kettle stirring dissolve, temperature is controlled at 82 ℃; Weighing 4.17kg drops into stirring and dissolving in the N-methyl morpholine oxide solution then, and its temperature is controlled at 82 ℃, and dissolution time was controlled at 9 hours, made spinning solution; Above-mentioned spinning solution is extruded through dual-screw-stem machine, enters casing through fondant filter again, and spinning solution measures through measuring pump in casing, from the spinnerets ejection, enters and solidifies the formation strand in solvent-water-bath; Wherein, the temperature of each district of dual-screw-stem machine, filter, spinning manifold is controlled at 110 ℃; The spinnerets specification: bore dia 0.10mm, hole count is 600 holes/plate, the distance between spinning plate and coagulating bath liquid level is air gap, is controlled at 25mm; Above-mentioned strand carries out spinneret draft through winding apparatus, and its extensibility is controlled at 20%, stretches through filling with in the traction grooved that temperature is controlled at 85 ℃ of water more again, and its extensibility is controlled at 35%.Strand is the remaining solvent of flush away in the drawing process again; Strand send cutting machine to cut into the staple fibre that length is 32.6-299.4mm after squeezing again; Staple fibre temperature after the cut-out is that 35-90 ℃ soft water washing was dewatered, oils, dewaters, dried in 30-60 minute, promptly makes finished fiber.Bake out temperature is a normal temperature-105 ℃, and drying time is 10 hours.The finished fiber that makes: fiber number 1.5d does fracture strength 4g/d, wet breaking strength 3.2g/d, and percentage elongation 14%, regain 13%, fiber is white in color, light, feel is smooth.
Claims (4)
1, a kind of method for producing cellulose fiber by dissolvant method: it is 0.1～0.5cm that pulp is ground into area
2, the chip about thickness 1mm; The stirring of N-methyl morpholine oxide is dissolved, temperature is controlled at 75～90 ℃, get pulp in the solid weight ratio then: the N-methyl morpholine oxide is that 1: 20～1: 24 ratio drops into stirring and dissolving in the N-methyl morpholine oxide solution with pulp, its temperature is controlled at 75～90 ℃, dissolution time was controlled at 6-12 hour, made spinning solution; Above-mentioned spinning solution is extruded through dual-screw-stem machine, enters casing through fondant filter again, and spinning solution measures through measuring pump in casing, from the spinnerets ejection, enters and solidifies the formation strand in solvent-water-bath; Wherein, the temperature of each district of dual-screw-stem machine, filter, spinning manifold is controlled at 110 ℃; The spinnerets specification: bore dia 0.10-0.23mm, hole count is 400-650 hole/plate, the distance between spinning plate and coagulating bath liquid level is air gap, is controlled at 7-400mm; Spinning solution removes bubble at dual-screw-stem machine through the mouth of finding time, and further dissolving, above-mentioned strand carries out spinneret draft through winding apparatus, its extensibility is controlled at-20%-250%, stretch through filling with in the traction grooved that temperature is controlled at 75-95 ℃ of water, its extensibility is controlled at 15%-100% again again; Strand is the remaining solvent of flush away in the drawing process again; Strand send cutting machine to cut into the staple fibre that length is 32.6～299.4mm after squeezing again; Staple fibre temperature after the cut-out is that 35-90 ℃ soft water washing was dewatered, oils, dewaters, dried in 30-60 minute, promptly makes finished fiber.
2, a kind of method for producing cellulose fiber by dissolvant method as claimed in claim 1 is characterized in that: by weight, and the fiber content 87%-89% in the finished fiber, water content 11%-13%.
3, a kind of method for producing cellulose fiber by dissolvant method as claimed in claim 1 is characterized in that: spin this cellulose fibre with dissolving spinning equipment.
4, a kind of method for producing cellulose fiber by dissolvant method as claimed in claim 1, it is characterized in that: dewater at staple fibre, oil, in the dehydration, drying course, oil bath concentration is 0.15-0.80g/1, and bake out temperature is a normal temperature-105 ℃, and drying time is 6-20 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97107819A CN1061106C (en) | 1997-12-09 | 1997-12-09 | Method for producing cellulose fiber by dissolvant method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97107819A CN1061106C (en) | 1997-12-09 | 1997-12-09 | Method for producing cellulose fiber by dissolvant method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1209473A CN1209473A (en) | 1999-03-03 |
| CN1061106C true CN1061106C (en) | 2001-01-24 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97107819A Expired - Lifetime CN1061106C (en) | 1997-12-09 | 1997-12-09 | Method for producing cellulose fiber by dissolvant method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1061106C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100500413C (en) * | 2003-07-11 | 2009-06-17 | 株式会社神户制钢所 | Metering feeder, kneading and extruding equipment |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100630267B1 (en) * | 2005-03-18 | 2006-09-29 | 주식회사 효성 | Dipped cord using hybrid cord and radial tire using the same |
| JP4849075B2 (en) * | 2007-02-08 | 2011-12-28 | コニカミノルタオプト株式会社 | Cellulose ester film, production method thereof, polarizing plate using cellulose ester film, and display device |
| CN101085838B (en) * | 2007-07-03 | 2011-03-30 | 中国科学院化学研究所 | Method for continuously preparing cellulose/ionic liquid solution |
| EP2589689B1 (en) * | 2010-06-30 | 2018-02-28 | Kolon Industries, Inc. | Dope for spinning lyocell, method for preparing lyocell filament fiber , and method for preparing a lyocell staple fiber using same |
| CN103421202B (en) * | 2012-05-22 | 2016-09-21 | 中国科学院化学研究所 | A kind of preparation method of high strength regenerative cellulose material |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1124033A (en) * | 1994-03-01 | 1996-06-05 | 连津格股份公司 | Process for producing cellulose shaped bodies |
| CN1134733A (en) * | 1994-09-05 | 1996-10-30 | 连津格股份公司 | Process for producing cellulose fibres |
| CN1134732A (en) * | 1994-09-05 | 1996-10-30 | 连津格股份公司 | Process for producing a cellulose moulding |
| CN1151194A (en) * | 1994-06-22 | 1997-06-04 | 考脱沃兹纤维(控股)有限公司 | Process for the manufacture of lyocell fibre |
| CN1165545A (en) * | 1995-08-11 | 1997-11-19 | 连津格股份公司 | Cellulose fibre |
| CN1173901A (en) * | 1995-10-13 | 1998-02-18 | 连津格股份公司 | Method for making cellulose fibres |
| CN1181788A (en) * | 1995-12-27 | 1998-05-13 | 连津格股份公司 | Method for the prodn. of cellulose fibres and device for carrying out the method |
| CN1189860A (en) * | 1996-03-04 | 1998-08-05 | 连津格股份公司 | Process for the manufacture of cellulose fibres |
-
1997
- 1997-12-09 CN CN97107819A patent/CN1061106C/en not_active Expired - Lifetime
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1124033A (en) * | 1994-03-01 | 1996-06-05 | 连津格股份公司 | Process for producing cellulose shaped bodies |
| CN1151194A (en) * | 1994-06-22 | 1997-06-04 | 考脱沃兹纤维(控股)有限公司 | Process for the manufacture of lyocell fibre |
| CN1134733A (en) * | 1994-09-05 | 1996-10-30 | 连津格股份公司 | Process for producing cellulose fibres |
| CN1134732A (en) * | 1994-09-05 | 1996-10-30 | 连津格股份公司 | Process for producing a cellulose moulding |
| CN1165545A (en) * | 1995-08-11 | 1997-11-19 | 连津格股份公司 | Cellulose fibre |
| CN1173901A (en) * | 1995-10-13 | 1998-02-18 | 连津格股份公司 | Method for making cellulose fibres |
| CN1181788A (en) * | 1995-12-27 | 1998-05-13 | 连津格股份公司 | Method for the prodn. of cellulose fibres and device for carrying out the method |
| CN1189860A (en) * | 1996-03-04 | 1998-08-05 | 连津格股份公司 | Process for the manufacture of cellulose fibres |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100500413C (en) * | 2003-07-11 | 2009-06-17 | 株式会社神户制钢所 | Metering feeder, kneading and extruding equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1209473A (en) | 1999-03-03 |
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Applicant after: YIBIN GRACE GROUP Co.,Ltd. Applicant before: YIBIN CITY CHEMICAL FIBRE FACT |
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Free format text: CORRECT: APPLICANT; FROM: YIBIN CITY CHEMICAL FIBRE FACTORY TO: YIBIN SILIYA GROUP LTD. |
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Free format text: CORRECT: PATENTEE; FROM: YIBIN SILIYA GROUP LTD. TO: SILIYA CO., LTD,. YIBIN; CO-PATENTEE; FROM: SICHUAN UNIVERSITY TO: SICHUAN UNIVERSITY |
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Address after: 644002 \u3001 Liu Jingzhuan, aerospace Road, Nangang economic and Technological Development Zone, Sichuan, Yibin Co-patentee after: SICHUAN University Patentee after: YIBIN GRACE Co.,Ltd. Address before: The South Bank of Yibin province Sichuan City Cuiping District 644000 Co-patentee before: Sichuan University Patentee before: YIBIN GRACE GROUP Co.,Ltd. |
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Effective date of registration: 20011116 Address after: Sichuan University Patentee after: YIBIN GRACE GROUP Co.,Ltd. Address before: Sichuan Union Univ. Patentee before: YIBIN GRACE GROUP Co.,Ltd. |
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| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20010124 |