CN100491606C - Method for recovering solvent in preparing acrylic fibers using ion liquid as solvent - Google Patents
Method for recovering solvent in preparing acrylic fibers using ion liquid as solvent Download PDFInfo
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- CN100491606C CN100491606C CNB2005101105800A CN200510110580A CN100491606C CN 100491606 C CN100491606 C CN 100491606C CN B2005101105800 A CNB2005101105800 A CN B2005101105800A CN 200510110580 A CN200510110580 A CN 200510110580A CN 100491606 C CN100491606 C CN 100491606C
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- solvent
- bmim
- ionic liquid
- acrylic fibers
- ion liquid
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Abstract
The invention discloses a solvent recovery method used in acrylic fibers manufacture with solvent ion liquid [BMIM]Cl or [BMIM]BF<SUB>4</SUB>. Its solvent coefficient of recovery can reach 95.0-99.9%. Thus the invention can reduce production cost and economize resources.
Description
Technical field
The present invention relates to a kind of is the recovery method of solvent in the acrylic fibers preparation of solvent with the ionic liquid, relates to a kind of with ionic liquid [BMIM] Cl or [BMIM] BF specifically
4Recovery method for solvent in the acrylic fibers preparation of solvent.
Technical background
Acrylic fibers have the same feel of wool, are widely used in clothing industry.The production of acrylic fibers can be adopted the method for solvent spinning, also can adopt the method for melt spinning by modification, the method of solvent spinning is adopted in actual production mostly, different according to solvent for use and technology path, the solvent spinning of acrylic fibers can be divided into wet spinning, dry spinning and dry-wet spinning, traditional solvent comprises sodium thiocyanate water solution, dimethyl sulfoxide (DMSO), dimethyl formamide and dimethylacetylamide etc., as everyone knows, inorganic solvent in all above-mentioned solvents has strong corrosivity, and organic solvent has volatility, the health that environment is caused serious pollution and jeopardizing operating personnel.In addition, Recovery of Organic Solvent need be carried out the multi-step pressure reduction evaporation, and inorganic solvent needs the multistage crystallization sedimentation, and whole recovery operation not only technological process is loaded down with trivial details, strict to control of process parameters, and can produce a large amount of waste gas and waste water, again environment is polluted.
Ionic liquid at room temperature is compared with conventional solvent, and the boiling point height is non-volatile, exists with liquid state in wider temperature range, and good heat endurance is arranged; Can change its physicochemical properties by the combination of the yin, yang ion selecting to suit, be the good solvent of many organic matters, inorganic matter and macromolecular material.Ionic liquid is as [BMIM] Cl:1-butyl-3-methyl-imidazoles chlorate; [BMIM] BF
4: 1-butyl-3-methyl-tetrafluoroborate, be widely used in electrochemistry, organic synthesis, catalysis and the field such as separate as a kind of green solvent, also be the good solvent of many macromolecular polymerization reactions and processing simultaneously, as gathering to benzene, polybutene, polymethyl methacrylate, polystyrene etc.United States Patent (USP) 20020010291 discloses a kind of method for preparing the high molecular polyisoolefines in ionic liquid, and United States Patent (USP) 20030157351 discloses a kind of cellulose and dissolved and method for processing in ionic liquid.
Summary of the invention
It is the recovery method of solvent in the acrylic fibers preparation of solvent with the ionic liquid that technical problem to be solved by this invention is to provide a kind of, to solve the defective that exists in the prior art.
The invention provides with [BMIM] Cl or [BMIM] BF
4As the recovery method of solvent in the acrylic fibers preparation process of solvent, this method comprises the steps:
A. will contain ionic liquid [BMIM] Cl or [BMIM] BF
4Coagulating bath in add entry and precipitate, dilute, the concentration that makes effects of ion liquid is 18-20%; Wherein ion liquid concentration can be used AgNO
3Titration is determined.
B. be that 0.22 micron miillpore filter filters solution with the aperture;
C. under the pressure condition of 150Pa, carry out decompression distillation with 95 ℃ temperature;
D. carry out air-distillation at 120 ℃.
The invention has the advantages that:
(1) solvent that is adopted is an ionic liquid, and nontoxic, non-volatility helps environmental protection and operator ' s health.
(2) coagulating agent is a water, is green solvent equally, helps environmental protection.
(3) owing to the ionic liquid non-volatility, vapour pressure approaches zero, so recovery process is simple, has reduced production cost, has saved the resource and the energy.
(4) ionic liquid [BMIM] Cl or [BMIM] BF
4The rate of recovery be 95.0～99.9%, can recycle.
Therefore this method for preparing acrylic fibre and used ion liquid recovery method are suitable for industrial extensive use.
The specific embodiment
Example 1
Carry out wet spinning with the polyacrylonitrile-ionic liquid that contains polyacrylonitrile 16% [BMIM] Cl solution, make coagulating agent, after spinning a period of time, take out the 1000g coagulating bath, use AgNO with [BMIM] Cl-water mixed solution of 20%
3Learn after the titration that this 1000g mixed liquor includes the about 278g of ionic liquid [BMIM] Cl.
Add 2000g water in the 1000g mixed liquor, fully stir.
With the miillpore filter of 0.22 μ m, filtration under diminished pressure.
Under the condition of 150Pa, 95 ℃ of decompression distillation 2 hours, 120 ℃ of air-distillations are 2 hours then, finally obtain the about 271g of ionic liquid [BMIM] Cl, and the rate of recovery is 97.48%.
Example 2
With the polyacrylonitrile-ionic liquid that contains polyacrylonitrile 15% [BMIM] BF
4Solution carries out wet spinning, makes coagulating agent with [BMIM] Cl-water mixed solution of 18%, after spinning a period of time, takes out the 1000g coagulating bath, with Pb (NO
3)
2Learn after the titration that this 1000g mixed liquor includes the about 202g of ionic liquid [BMIM] Cl.
Add 2000g water in the 1000g mixed liquor, fully stir.
With the miillpore filter of 0.22 μ m, filtration under diminished pressure.
Under the condition of 150Pa, 95 ℃ of decompression distillation 2 hours, 120 ℃ of air-distillations are 2 hours then, finally obtain the about 197g of ionic liquid [BMIM] Cl, and the rate of recovery is 97.52%.
Claims (1)
1. one kind is the recovery method of solvent in the acrylic fibers preparation of solvent with the ionic liquid, it is characterized in that this method comprises the steps:
A. will contain ionic liquid [BMIM] Cl or [BMIM] BF
4Coagulating bath in add entry and precipitate, dilute, the concentration that makes effects of ion liquid is 18-20%;
B. be that 0.22 micron miillpore filter filters solution with the aperture;
C. under the pressure condition of 150Pa, carry out decompression distillation with 95 ℃ temperature;
D. carry out air-distillation at 120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101105800A CN100491606C (en) | 2005-11-22 | 2005-11-22 | Method for recovering solvent in preparing acrylic fibers using ion liquid as solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101105800A CN100491606C (en) | 2005-11-22 | 2005-11-22 | Method for recovering solvent in preparing acrylic fibers using ion liquid as solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1793443A CN1793443A (en) | 2006-06-28 |
| CN100491606C true CN100491606C (en) | 2009-05-27 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101105800A Expired - Fee Related CN100491606C (en) | 2005-11-22 | 2005-11-22 | Method for recovering solvent in preparing acrylic fibers using ion liquid as solvent |
Country Status (1)
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| CN (1) | CN100491606C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776790B (en) * | 2012-07-10 | 2013-12-11 | 东华大学 | Waterless dyeing method of dispersed dye |
-
2005
- 2005-11-22 CN CNB2005101105800A patent/CN100491606C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 离子液体中的化学反应. 李丹东，高鹏，赵德智，张姝妍，王玉新，王延平.辽宁上油化工大学学报，第24卷第2期. 2004 |
| 离子液体中的化学反应. 李丹东，高鹏，赵德智，张姝妍，王玉新，王延平.辽宁上油化工大学学报，第24卷第2期. 2004 * |
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| Publication number | Publication date |
|---|---|
| CN1793443A (en) | 2006-06-28 |
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