CN1118592C - Process for refining solvent used in solution spinning method of polyurethane fibre industry - Google Patents
Process for refining solvent used in solution spinning method of polyurethane fibre industry Download PDFInfo
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- CN1118592C CN1118592C CN00132105A CN00132105A CN1118592C CN 1118592 C CN1118592 C CN 1118592C CN 00132105 A CN00132105 A CN 00132105A CN 00132105 A CN00132105 A CN 00132105A CN 1118592 C CN1118592 C CN 1118592C
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- solvent
- spinning method
- solution spinning
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- isocyanate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The present invention discloses a method for refining a solvent for a solution spinning method in spandex industry, which comprises: a compound containing one or a plurality of isocyanate groups is added into a solvent for a solution spinning method in spandex industry and then reacts with the solvent to obtain a reaction product, and finally, the reaction product is treated by fractionation by distillation. The method of the present invention has the advantages of simple technology, low cost and suitability for large-scale industrial production.
Description
The primary solvent system that is widely used in polyurethane fibre industry at present is dimethyl formamide (DMF), and a kind of water white transparency is neutral organic solvent substantially.The dicyandiamide solution that DMF produces as spandex, its consumption accounts for 67% of stoste weight.The quality good or not of solvent has fundamental influence to the quality synthetic and the spandex silk of spandex.In order to improve the quality of polymerization stoste, improve the quality of spandex silk, further raising DMF Study on Quality is necessary.
Usually in the laboratory, the process for purification of DMF solvent is that the molecular sieve by 4A dewaters.If moisture when higher, can stir and place 24 hours, branch vibration layer by adding an amount of potassium hydroxide.Remove impurity such as methyl alcohol simultaneously.In order to slough residual moisture; add a large amount of SILVER REAGENT benzene; under normal pressure, distill; adding P2O5 in the cut more than 130C stirred after 4 hours; tell supernatant liquor; add KOH and stir separation in 2 hours, liquid is decompression distillation under nitrogen protection again, collects midbarrel and is pure dimethyl formamide.This shows that this process for purification can't directly be incorporated in the industrial production owing to its complexity.
In the industrial production, the refining method that normally adopts physics rectifying of DMF.But owing to during spandex produces, use raw material type many, sneak into impurity component complexity among the DMF (as contain moisture ,-OH ,-NH
2,-some active groups such as COOH), the existence of these active groups is difficult to thoroughly remove in serialization rectifying, and is bigger to the polymerisation influence.
The object of the present invention is to provide a kind of technology simply, the process for purification of solvent used in solution spinning method of polyurethane fibre industry cheaply.
The process for purification of solvent used in solution spinning method of polyurethane fibre industry of the present invention is to add the compound that contains one or more isocyanate groups in described solvent used in solution spinning method of polyurethane fibre industry, reacts, and carries out separated then.
The solvent used in solution spinning method of polyurethane fibre industry that the present invention is used to make with extra care comprises dimethyl formamide, dimethylacetylamide, toluene, MEK.
In the present invention, boiling point is higher than 160 ℃ under the employed isocyanate compound normal pressure, comprise phenyl isocyanate (163 ℃ of boiling points (55 ℃/13 * 133.32Pa)), isocyanic acid 11 esters (103 ℃ of boiling points (3 * 133.32Pa)), toluene di-isocyanate(TDI) (246 ℃ of boiling points), diphenyl methane-4,4 '-vulcabond (196 ℃ of boiling points (5 * 133.32Pa)), 1, hexamethylene-diisocyanate (130 ℃ of boiling points (14 * 133.32Pa)), XDI (151 ℃ of boiling points (6 * 133.32Pa)), naphthalene 1,5-vulcabond.(167 ℃ of boiling points (5 * 133.32Pa)), Methylcyclohexyl diisocyanate (boiling point 90 ℃ (133.32Pa)), tetramethylxylylene diisocyanate (boiling point 150 ℃ (0.4kPa)), and their high-boiling derivatives.
In the present invention, the computational methods of employed isocyanate compound dosage are: (unit: kilogram)
In the formula in the numeral of denominator (15-45) the expression solvent impurity contained reactive group work as weight range, equivalent 17), amido (NH: equivalent 15), carboxyl (COOH: equivalent 45) and water (pressing hydroxyl calculating) they comprise hydroxyl (OH:.Accurate dosage final in the reality can determine that consider cost simultaneously, its result who surveys should reach the industrial production standard by the chromatogram result.
The present invention adopts chemical method and physical method way of combining, proves effective.Promptly at first utilize in active reaction reagent (containing isocyanate group) and the solvent-OH (comprising water),-NH, the reaction of-COOH active group forms high boiling material (reactional equation is as follows), by distillation high-purity DMF is separated then, and high boiling material is extracted out at the bottom of tower, thereby reaches the purpose of purifying.
Note：R″＝HO，RO，R-NH，R-COO
Method technology of the present invention is simple, with low cost, and the purity of refining back solvent can reach 99.99%.
Further describe the present invention below in conjunction with drawings and Examples.
Fig. 1 is a gas chromatographic analysis collection of illustrative plates before embodiment 1 solvent refining
Fig. 2 is a gas chromatographic analysis collection of illustrative plates after embodiment 1 solvent refining
Fig. 3 is a ultraviolet absorpting spectrum before embodiment 1 solvent refining
Fig. 4 is a ultraviolet absorpting spectrum after embodiment 1 solvent refining
Embodiment 1:
(in the laboratory) gets solvent purity is that 99.5% refining DMF (being dimethyl formamide) 1000ml puts into the there-necked flask that is equipped with distilling apparatus, there-necked flask places heating pot, set 170 ℃ of heating-up temperatures, open heater switch and condensed water, calculate the amount that adds isocyanates according to formula, with MDI (diphenyl methane-4,4 '-vulcabond) is example, its equivalent is 125, and calculating addition is 13～39 grams, adds 30 grams, add bottle stopper on the bonnet from feeding mouth, finish until distillation, get 152 ℃ of fractions, be refining DMF.Solvent before and after refining is carried out gas-chromatography, determination of uv absorption, and collection of illustrative plates is shown in Fig. 1-4.
Gas chromatographic analysis result (Fig. 1～2) shows that refining preceding solvent samples has assorted peak, and the solvent samples after refining does not have this assorted peak.Ultraviolet absorption spectroscopy can determine also by ultra-violet absorption spectrum whether foreign substance is arranged in the sample, UV absorption to this solvent samples the analysis showed that (Fig. 3～4): the solvent samples before refining has a fairly obvious absorption near 400nm, and the solvent samples after making with extra care does not have this absorption.Illustrate that solvent samples impurity absorbing wavelength is 400nm, can be by the refining impurity of removing.
Embodiment 2:
(in industry) connects the feeding-in solid body container of a special processing, when the solvent DMF feed cycle on the intake pipeline before the solvent distillation tower, adding the isocyanates of amount of calculation, is example with MDI, pumps into rectifying column with solvent, and distillation, get 152 ℃ of fractions and enter reactor.Because of industrial cost consideration, in the computer capacity of addition, can adjust dosage to best.
Claims (3)
1. the process for purification of a solvent used in solution spinning method of polyurethane fibre industry, it is characterized in that providing a kind of solvent used in solution spinning method of polyurethane fibre industry dimethyl formamide, in described solvent, add the compound that contains one or more isocyanate groups then, react, carry out separated then.
2. according to the process of claim 1 wherein that the described compound that contains one or more isocyanate groups comprises that boiling point is higher than 160 ℃ phenyl isocyanate under the normal pressure, isocyanic acid 11 esters, toluene di-isocyanate(TDI), diphenyl methane-4,4 '-vulcabond, 1, hexamethylene-diisocyanate, XDI, naphthalene 1, the 5-vulcabond, Methylcyclohexyl diisocyanate, tetramethylxylylene diisocyanate, and their high-boiling derivatives.
3. according to the process of claim 1 wherein that the described adding weight range that contains one or more isocyanate groups compounds is: weight * isocyanate equivalent/(15～45) of (the described solvent purity % of 1-) * described solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00132105A CN1118592C (en) | 2000-12-13 | 2000-12-13 | Process for refining solvent used in solution spinning method of polyurethane fibre industry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00132105A CN1118592C (en) | 2000-12-13 | 2000-12-13 | Process for refining solvent used in solution spinning method of polyurethane fibre industry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1358887A CN1358887A (en) | 2002-07-17 |
| CN1118592C true CN1118592C (en) | 2003-08-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00132105A Expired - Fee Related CN1118592C (en) | 2000-12-13 | 2000-12-13 | Process for refining solvent used in solution spinning method of polyurethane fibre industry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1118592C (en) |
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2000
- 2000-12-13 CN CN00132105A patent/CN1118592C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1358887A (en) | 2002-07-17 |
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| Date | Code | Title | Description |
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Zhejiang Huafeng Spandex Co., Ltd. Assignor: Institute of Chemistry, Chinese Academy of Sciences Contract fulfillment period: 2005.10.20 to 2015.10.19 contract change Contract record no.: 2009330000213 Denomination of invention: Process for refining solvent used in solution spinning method of polyurethane fibre industry Granted publication date: 20030820 License type: Exclusive license Record date: 2009.2.9 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2005.10.20 TO 2015.10.19; CHANGE OF CONTRACT Name of requester: ZHEJIANG PROVINCE HUAFENG SPANDEX CO., LTD. Effective date: 20090209 |
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| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20030820 Termination date: 20131213 |