CN104674356A - Preparation method of spinning solution - Google Patents
Preparation method of spinning solution Download PDFInfo
- Publication number
- CN104674356A CN104674356A CN201510122252.6A CN201510122252A CN104674356A CN 104674356 A CN104674356 A CN 104674356A CN 201510122252 A CN201510122252 A CN 201510122252A CN 104674356 A CN104674356 A CN 104674356A
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- CN
- China
- Prior art keywords
- preparation
- spinning solution
- solvent
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-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of a spinning solution, relating to the technical field of production of viscose staple fibers. According to the method, the spinning solution is prepared by in-situ chemical modification and low-temperature continuous dissolution; raw materials used in the method are low in cost, simple to prepare, safe, non-toxic and free of waste water and waste gas emission, and thus the preparation method is an environment-friendly spinning solution preparation method; the prepared spinning solution completely achieves the demands of cellulose fiber production. The preparation method disclosed by the invention can substitute for a common preparation method for a viscose staple fiber spinning solution, the preparation flow is greatly shortened, and the production efficiency is improved. The preparation method disclosed by the invention can substitute for common preparation methods for regenerated cellulose fibers, such as viscose staple fiber, and a spinning solution for regenerated cellulose membranes.
Description
Technical field
The present invention relates to the production method of the production technical field of viscose staple fibre, particularly regenerated celulose fibre and regenerated cellulose film.
Technical background
At present, in the suitability for industrialized production of global regenerated celulose fibre and regenerated cellulose film, CS is only had
2the several methods such as dissolution method, cuprammonium process and NMMO dissolution method prepare spinning solution.CS
2dissolution method and cuprammonium process be serious environment pollution because discharging a large amount of waste gas waste water in production, and also there is more inflammable and explosive potential safety hazard in producing, therefore, the developed countries such as America and Europe stopped this two kinds of methods in a large number and produce regenerated celulose fibres and regenerated cellulose film, and only Japan also retains the cuprammonium process production of only a few at present.China is also by CS
2method produces regenerated celulose fibre and regenerated cellulose film is classified as Key Environmental Protection regulation object.And NMMO method because of its solvent expensive, and there is the problems such as difficult solvent recovery, inflammable and explosive, technology barriers in producing and slower development.In addition, China is populous nation, and comfortable and easy to wear, bright, the regenerated celulose fibre meeting human body needs and regenerated cellulose film demand is huge.So regenerated celulose fibre and the regenerated cellulose film of developing environmental protection are the task of top priority.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of spinning solution, to solve huge etc. the problem of the pollution problem in the process of producing at present regenerated celulose fibre and regenerated cellulose film, inflammable and explosive problem, cost.
Technical solution of the present invention comprises the following steps:
1) prepare solvent: first by after demineralized water and alkali stirring and dissolving, more successively dissolve in thiocarbamide, urea and dispersant;
2) pulp is dropped into carry out swelling in solvent, obtain slurry;
3) discharging after slurry being cooled to 10 ~ 50 DEG C, then enter screw machine and dissolve, obtain spinning stoste.
The method that the present invention adopts in-situ chemical modification, low temperature continuous-dissolution prepares spinning solution, raw materials used cheap, prepare simple, safe, nontoxic, discharge without waste water and gas, be a kind of spinning solution preparation method of environmental protection, the spinning solution of preparation reaches the requirement of produce cellulose fibers completely.By the preparation method of alternative common viscose staple fibre spinning solution, and shorten preparation flow widely, improve production efficiency.To be the preparation method of spinning solution of the regenerated celulose fibres such as alternative common viscose staple fibre and regenerated cellulose film.
In addition, in solvent of the present invention, the input amount of alkali accounts for 7 ~ 9% of solvent gross mass, the input amount of thiocarbamide accounts for 7 ~ 9% of solvent gross mass, the input amount of urea accounts for 7 ~ 9% of solvent gross mass, and the input amount of dispersant accounts for 0.5 ~ 5% of solvent gross mass, and all the other are demineralized water.
The input amount of alkali accounts for 7 ~ 9% of solvent gross mass, and the cellulose in pulp can be made fully swelling, and the alkali cellulose of generation is conducive to dissolving at low temperatures.The input amount of urea accounts for 7 ~ 9% of solvent gross mass, is to make urea molecule have enough amounts, completely and alkali cellulose molecular combinations, can cut off the hydrogen bond in cellulosic molecule, thus cellulose is dissolved.The input amount of thiocarbamide accounts for 7 ~ 9% of solvent gross mass, be to the solvability of urea supplement and perfect, can play the effect of the hydrogen bond polymerization stoped in cellulosic molecule further, the stability of the spinning solution of dissolving is improved, and the resting period was more than more than 24 hours.The input amount of dispersant accounts for 0.5 ~ 5% of solvent gross mass, is in order to cellulose fibre disperses fully, is convenient to alkali, urea, zinc oxide etc. and mixes with cellulose fibre.
The degree of polymerization of described pulp is 200 ~ 800, be on the one hand be conducive to solvent can abundant dissolving cellulos, on the other hand, the spinning solution of preparation is through wet spinning, and the regenerated celulose fibre intensity obtained is the highest, can reach 2.0 ~ 3.0CN/dtex.
In order to the stability of the spinning solution making preparation is best, be conducive to later process process, be conducive to spinning technique, described pulp is 7 ~ 9:100 with the mixing quality ratio of solvent.
Described swelling be carry out 10 ~ 180 minutes under the temperature of mixed system is the condition of 10 ~ 70 DEG C.The cellulose in pulp can being made fully swelling, be easy to the alkali cellulose generated, creating condition for dissolving.
The temperature of described screw machine is-12 ~-6 DEG C, rotating speed is 60 ~ 500 revs/min.At this temperature and rotating speed, cellulose can be dissolved completely, and spinning solution is stablized.
In addition, the alkali of use is NaOH, can be solid or liquid; The preferred polyethyleneglycol derivative of dispersant, trade name V388; The preferred thio urea of thiocarbamide, chemical formula: CN
2h
4s.
Detailed description of the invention
1, each raw material weighing preparing 100kg solvent is:
Alkali: 7 ~ 9kg;
Thiocarbamide: 7 ~ 9kg;
Urea: 7 ~ 9kg;
Dispersant: 0.5 ~ 5kg;
Demineralized water: surplus.
Wherein, operable alkali is NaOH, can be solid or liquid.
Dispersant is polyethyleneglycol derivative, trade name V388.
Thiocarbamide is thio urea, chemical formula: CN
2h
4s.
2,100kg solvent process is prepared: first added by demineralized water in the swelling still of band stirring and chuck, again solid caustic soda (or liquid caustic soda) is added in swelling still and carry out stirring and dissolving, exist side by side and add stirring and dissolving in swelling still by thiocarbamide, finally urea and dispersant are added stirring and dissolving in swelling still, obtained solvent.
The stirring and dissolving time of raw material in swelling still of above-mentioned solvent is; 10 ~ 60 minutes, jacket temperature controlled at 10 ~ 70 DEG C.
3, by 7 ~ 9kg, the degree of polymerization be 200 ~ 800 pulp drop in have and carry out swelling in the swelling still of 100kg solvent, under the condition of jacket temperature 10 ~ 70 DEG C, swelling 10 ~ 180 minutes, obtain slurry.
4, slurry is lowered the temperature in advance 10 ~ 180 minutes, start discharging to material temperature 10 ~ 50 DEG C time.
5, feed liquid enters dual-screw-stem machine (or single-screw machine) and dissolves, the temperature of screw machine control-12 ~-6 DEG C, rotating speed controls just pulp to be dissolved as at 60 ~ 500 revs/min the stoste of applicable spinning.
6, the indices testing result of spinning solution:
Falling ball viscosity 30 ~ 70 seconds; Containing first fibre 7 ~ 9%; Containing alkali 7 ~ 9%; Filter value 210 milliliters.
By above-mentioned stoste more after filtration, deaeration, wet spinning just can produce the regenerated celulose fibre and regenerated cellulose film that meet national standard.
Claims (9)
1. a preparation method for spinning solution, is characterized in that comprising the following steps:
1) prepare solvent: first by after demineralized water and alkali stirring and dissolving, more successively dissolve in thiocarbamide, urea and dispersant;
2) pulp is dropped into carry out swelling in solvent, obtain slurry;
3) discharging after slurry being cooled to 10 ~ 50 DEG C, then enter screw machine and dissolve, obtain spinning stoste.
2. method according to claim 1, it is characterized in that in described solvent, the input amount of alkali accounts for 7 ~ 9% of solvent gross mass, the input amount of thiocarbamide accounts for 7 ~ 9% of solvent gross mass, the input amount of urea accounts for 7 ~ 9% of solvent gross mass, the input amount of dispersant accounts for 0.5 ~ 5% of solvent gross mass, and all the other are demineralized water.
3. method according to claim 1, is characterized in that the degree of polymerization of described pulp is 200 ~ 800.
4. method according to claim 3, is characterized in that described pulp is 7 ~ 9:100 with the mixing quality ratio of solvent.
5. method according to claim 3 or 4, it is characterized in that described swelling be carry out 10 ~ 180 minutes under the temperature of mixed system is the condition of 10 ~ 70 DEG C.
6. method according to claim 1, is characterized in that the temperature of described screw machine is-12 ~-6 DEG C, rotating speed is 60 ~ 500 revs/min.
7. method according to claim 1 or 2 or 3, is characterized in that described alkali is NaOH.
8. method according to claim 1 or 2 or 3, is characterized in that described dispersant is polyethyleneglycol derivative.
9. method according to claim 1 or 2 or 3, is characterized in that described thiocarbamide is thio urea.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510122252.6A CN104674356A (en) | 2015-03-20 | 2015-03-20 | Preparation method of spinning solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510122252.6A CN104674356A (en) | 2015-03-20 | 2015-03-20 | Preparation method of spinning solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104674356A true CN104674356A (en) | 2015-06-03 |
Family
ID=53309917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510122252.6A Pending CN104674356A (en) | 2015-03-20 | 2015-03-20 | Preparation method of spinning solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104674356A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB216475A (en) * | 1923-05-25 | 1924-11-03 | Leon Lilienfeld | Manufacture of cellulose solutions |
| GB818044A (en) * | 1956-07-19 | 1959-08-12 | British Industrial Plastics | Improvements in and relating to thermo-setting aminoplastic moulding compositions |
| RU2114121C1 (en) * | 1995-08-08 | 1998-06-27 | Акционерное общество открытого типа "Усольехимпром" | Method of preparing methyloxypropyl cellulose |
| WO2008114524A1 (en) * | 2007-03-20 | 2008-09-25 | The University Of Tokyo | Cellulose aerogel and method for production thereof |
| CN102432892A (en) * | 2011-08-04 | 2012-05-02 | 中国纺织科学研究院 | Method for dissolving cellulose and method for preparing regenerated fiber |
| CN102964606A (en) * | 2012-11-28 | 2013-03-13 | 东华大学 | Cellulose composite solvent system and application thereof |
-
2015
- 2015-03-20 CN CN201510122252.6A patent/CN104674356A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB216475A (en) * | 1923-05-25 | 1924-11-03 | Leon Lilienfeld | Manufacture of cellulose solutions |
| GB818044A (en) * | 1956-07-19 | 1959-08-12 | British Industrial Plastics | Improvements in and relating to thermo-setting aminoplastic moulding compositions |
| RU2114121C1 (en) * | 1995-08-08 | 1998-06-27 | Акционерное общество открытого типа "Усольехимпром" | Method of preparing methyloxypropyl cellulose |
| WO2008114524A1 (en) * | 2007-03-20 | 2008-09-25 | The University Of Tokyo | Cellulose aerogel and method for production thereof |
| CN102432892A (en) * | 2011-08-04 | 2012-05-02 | 中国纺织科学研究院 | Method for dissolving cellulose and method for preparing regenerated fiber |
| CN102964606A (en) * | 2012-11-28 | 2013-03-13 | 东华大学 | Cellulose composite solvent system and application thereof |
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Application publication date: 20150603 |