CN1693548A - Method of producing poly(terephthaloyl-p-phenylene diamine) fibre - Google Patents
Method of producing poly(terephthaloyl-p-phenylene diamine) fibre Download PDFInfo
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- CN1693548A CN1693548A CN 200410018151 CN200410018151A CN1693548A CN 1693548 A CN1693548 A CN 1693548A CN 200410018151 CN200410018151 CN 200410018151 CN 200410018151 A CN200410018151 A CN 200410018151A CN 1693548 A CN1693548 A CN 1693548A
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- methyl pyrrolidone
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Abstract
The invention discloses a method for producing p-phenylene terephthalamide (PPTA) fiber, in turn performs spinning molding, filature beam washing with water, drying and thermal treatment on PPTA solution, where the spinning molding is meant to be a wet spinning molding, which uses dimethyl acetamide and/or N-methyl pyrrolidone, and water to make solidifying bath. The advantages of the invention are simplifying equipment, and the compositions of the solidifying bath have no corrosion to the equipment, easy to recover, and the waste water is easy to process.
Description
Technical field
The invention belongs to field of high polymer material processing, the method that relates to a kind of Fanglun 1414 of production, this Fanglun 1414 is mainly used in high-tech areas such as Aero-Space, national defence, telecommunications, environmental protection, oil, ocean, as the basic material of electrically insulating material, high-temperature-resistant filtering material, protective clothes material, cellular structural material.
Background technology
At present, Fanglun 1414's industrial process is the dry-wet spinning method, see domestic publication 90100861.3, this method is to pass through the washing processing of the dry-wet spinning moulding of aromatic polyamide condensate concentrated sulfuric acid solution, tow, the oven dry processing of tow, heat treatment successively.
The first step, the polymeric concentrated sulfuric acid solution of certain density PPTA earlier through one section air gap section, and then utilize dilute sulfuric acid to make the tow coagulation forming as coagulating bath after spinneret orifice flows out.
In second step, the tow water is washed, and neutralization contains the washings of sulfuric acid.
The 3rd step is with the tow oven dry after cleaning.
In the 4th step, the tow tension force heat treatment that circulates after the oven dry is obtained required long filament.
The shortcoming of said method is: 1, because the solvent and the coagulating bath of spinning solution is sulfuric acid solution, equipment material required high, causes the equipment investment cost height, and coagulating bath recovery, difficult treatment; 2, owing to will use the solvent of the concentrated sulfuric acid as the preparation spinning solution, it is big dangerous that producers are had when operation; 3, owing to when washing is handled, use in the soda ash water and dilute sulfuric acid, cause the wastewater treatment difficulty, bigger to environmental hazard.
Summary of the invention
Technical problem to be solved by this invention is to overcome the above-mentioned shortcoming that exists in the prior art, provides that a kind of equipment investment cost is low, coagulating bath is handled easily, the production Fanglun 1414's of handling safety method.
The technical scheme that the present invention solves its technical problem is: a kind of Fanglun 1414's of production method, divided for four steps carried out, the first step is polymeric dimethylacetylamide of PPTA or the spinning moulding of N-Methyl pyrrolidone solution in the coagulating bath of dimethylacetylamide or N-Methyl pyrrolidone and water composition, second step was that the washing of tow is handled, the 3rd step was that the oven dry of tow is handled, and the 4th step was the heat treatment of tow.
The concentration of dimethylacetylamide or N-Methyl pyrrolidone is 60-80% in the coagulating bath of the present invention, and temperature is 5-30 ℃.
The solvent of PPTA solution of the present invention is dimethylacetylamide or N-Methyl pyrrolidone, the concentration range of this PPTA solution is that 9-13%, temperature range are that 40-80 ℃, the polymeric inherent viscosity of PPTA are no more than 4.7, is not less than 1.6.
The washing of tow of the present invention is handled and is to use desalted water that tow is washed, and its temperature range is 30-80 ℃.
The heat treatment of tow of the present invention can contain the heat treatment process in an above stage.
Can contain lithium chloride or calcium chloride in the PPTA solution of the present invention.
The present invention compared with prior art, its advantage is: 1, owing to adopt the wet spinning moulding, simplified technological process and corresponding apparatus, thereby reduced equipment cost; 2, since the mixture that uses dimethylacetylamide-water or N-Methyl pyrrolidone-water as coagulating bath, and dimethylacetylamide or N-Methyl pyrrolidone are less to equipment corrosion, dangerous low to operating personnel; 3, can reclaim by rectifying because of dimethylacetylamide or N-Methyl pyrrolidone, its rate of recovery generally can reach 93-96%, has reduced production cost; 4, only use desalted water to wash because washing is handled, so wastewater treatment is easy.
The specific embodiment
Below in conjunction with specific embodiment method of the present invention is described.
Embodiment 1:
The end product of present embodiment is that filament number is the Fanglun 1414 of 5.55dtex.
The first step, 9% PPTA polymer solution in N-Methyl pyrrolidone flows out through spinneret orifice earlier, enters coagulation forming in the coagulating bath again.Wherein, the polymeric inherent viscosity of this PPTA is 4.7, contains the lithium chloride with respect to condensate weight 50% in the solution, and the temperature of PPTA polymer solution is 60 ℃; Coagulating bath is 60% the N-Methyl pyrrolidone aqueous solution, and coagulation bath temperature is 5 ℃, and the tow speed in the coagulating bath is 15m/min, and draw ratio is 1.05, and setting time is 15 seconds.
Second step is with the N-Methyl pyrrolidone of tow with remnants in 60 ℃ the desalted water flush away tow.Wherein, the tow speed in the rinsing machine is 15.1m/min.
In the 3rd step, the moisture that the tow after cleaning is dried to the tow is no more than 4%.Wherein, bake out temperature is 120 ℃, and the tow speed in the dryer is 15.2m/min.
In the 4th step, the tow after the oven dry is carried out the heat treatment in two stages.The heat treatment in two stages can improve the crystalline orientation structure of fibrous inside better than the heat treatment in a stage, makes it have better serviceability.Wherein, the temperature of heat treated process control tow of phase I is that 402 ℃, draw ratio are 1.3, heat treatment time is 30 seconds; The temperature of the heat treated process control tow of second stage is that 443 ℃, draw ratio are 1.0, heat treatment time is 30 seconds.
At last, will carry out post processing through heat treated tow and obtain required product.This postprocessing working procedures is according to carrying out different processing to the requirement of final products is different, for example: being used for weaving needs through curling, cut into certain-length with staple fibre; The staple fibre that is used for papermaking or composite needs through cutting into certain-length; The direct package of long filament becomes tube.
Embodiment 2:
The end product of present embodiment is that filament number is the Fanglun 1414 of 7.77dtex.
The first step, 13% PPTA polymer solution in N-Methyl pyrrolidone flows out through spinneret orifice earlier, enters coagulation forming in the coagulating bath again.Wherein, the polymeric inherent viscosity of this PPTA is 1.6, and the temperature of PPTA polymer solution is 80 ℃; Coagulating bath is 80% the N-Methyl pyrrolidone aqueous solution, and coagulation bath temperature is 30 ℃, and the tow speed in the coagulating bath is 16m/min, and draw ratio is 1.05, and setting time is 15 seconds.
Second step is with the N-Methyl pyrrolidone of tow with remnants in 80 ℃ the desalted water flush away tow.Wherein, the tow speed in the rinsing machine is 16.1m/min.
In the 3rd step, the moisture that the tow after cleaning is dried to the tow is no more than 4%.Wherein, bake out temperature is 120 ℃, and the tow speed in the dryer is 16.2m/min.
In the 4th step, the tow after the oven dry is carried out the heat treatment in a stage.Wherein, the temperature of control tow is that 432 ℃, draw ratio are 1.3, heat treatment time is 30 seconds.
At last, heat treated tow is carried out post processing and obtain required product.This postprocessing working procedures is carried out different processing according to the requirement difference of final products, and for example: being used for weaving needs through curling, cut into certain-length with staple fibre; The staple fibre that is used for papermaking or composite needs through cutting into certain-length; The direct package of long filament becomes tube.
Embodiment 3:
The end product of present embodiment is that filament number is the Fanglun 1414 of 7.77dtex.
The first step, 11% PPTA polymer solution in dimethylacetylamide flows out through spinneret orifice earlier, enters coagulation forming in the coagulating bath again.Wherein, the polymeric inherent viscosity of this PPTA is 2.8, and the temperature of PPTA polymer solution is 40 ℃; Coagulating bath is 67% the dimethylacetylamide aqueous solution, and coagulation bath temperature is 15 ℃, and the tow speed in the coagulating bath is 17m/min, and draw ratio is 1.05, and setting time is 15 seconds.
Second step is with the dimethylacetylamide of tow with remnants in 30 ℃ the desalted water flush away tow.Wherein, the tow speed in the rinsing machine is 17.1m/min.
In the 3rd step, the moisture that the tow after cleaning is dried to the tow is no more than 4%.Wherein, bake out temperature is 120 ℃, and the tow speed in the dryer is 17.2m/min.
In the 4th step, the tow after the oven dry is carried out three phases heat treatment.The heat treatment of three phases can improve the crystalline orientation structure of fibrous inside better than the heat treatment in two stages, makes it have better serviceability.Wherein, the temperature of phase I control tow is that 442 ℃, draw ratio are 1.0, heat treatment time is 30 seconds; The temperature of second stage control tow is that 400 ℃, draw ratio are 1.1, heat treatment time is 30 seconds; The temperature of phase III control tow is 410 ℃, and draw ratio is 1.15, and heat treatment time is 30 seconds.
At last, heat treated tow is carried out post processing and obtain required product.This postprocessing working procedures is carried out different processing according to the requirement difference of final products, and for example: being used for weaving needs through curling, cut into certain-length with staple fibre; The staple fibre that is used for papermaking or composite needs through cutting into certain-length; The direct package of long filament becomes tube.
Claims (6)
1, a kind of method of producing the Fanglun 1414, divided for four steps carried out, the first step is polymeric dimethylacetylamide of PPTA or the spinning moulding of N-Methyl pyrrolidone solution in the coagulating bath of dimethylacetylamide or N-Methyl pyrrolidone and water composition, second step was that the washing of tow is handled, the 3rd step was that the oven dry of tow is handled, and the 4th step was the heat treatment of tow.
2, production Fanglun 1414's according to claim 1 method, it is characterized in that: the concentration of dimethylacetylamide or N-Methyl pyrrolidone is 60-80% in the described coagulating bath, temperature is 5-30 ℃.
3, production Fanglun 1414's according to claim 1 method, it is characterized in that: the solvent of described PPTA solution is dimethylacetylamide or N-Methyl pyrrolidone, the concentration range of this PPTA solution is that 9-13%, temperature range are that 40-80 ℃, the polymeric inherent viscosity of PPTA are no more than 4.7, is not less than 1.6.
4, production Fanglun 1414's according to claim 1 method is characterized in that: the washing of described tow is handled and is to use desalted water that tow is washed, and its temperature range is 30-80 ℃.
5, production Fanglun 1414's according to claim 1 method, it is characterized in that: the heat treatment of described tow can contain the heat treatment process in an above stage.
6, production Fanglun 1414's according to claim 1 method is characterized in that: can contain lithium chloride or calcium chloride in the described PPTA solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410018151 CN1693548A (en) | 2004-05-09 | 2004-05-09 | Method of producing poly(terephthaloyl-p-phenylene diamine) fibre |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410018151 CN1693548A (en) | 2004-05-09 | 2004-05-09 | Method of producing poly(terephthaloyl-p-phenylene diamine) fibre |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286794A (en) * | 2011-08-09 | 2011-12-21 | 中国石油化工股份有限公司 | High-performance fibers and preparation method thereof |
| CN102336907A (en) * | 2011-06-22 | 2012-02-01 | 上海舟汉纤维材料科技有限公司 | Method for washing poly terephthaloyl-p-phenylene diamine polymer |
| CN102953128A (en) * | 2012-04-16 | 2013-03-06 | 国能飞腾科技有限公司 | Continuous spinning system of poly (p-phenylene terephthalamide) |
| WO2017050220A1 (en) * | 2015-09-25 | 2017-03-30 | 清华大学 | Preparation method for para-aramid fiber |
-
2004
- 2004-05-09 CN CN 200410018151 patent/CN1693548A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336907A (en) * | 2011-06-22 | 2012-02-01 | 上海舟汉纤维材料科技有限公司 | Method for washing poly terephthaloyl-p-phenylene diamine polymer |
| CN102286794A (en) * | 2011-08-09 | 2011-12-21 | 中国石油化工股份有限公司 | High-performance fibers and preparation method thereof |
| CN102286794B (en) * | 2011-08-09 | 2013-06-12 | 中国石油化工股份有限公司 | High-performance fibers and preparation method thereof |
| CN102953128A (en) * | 2012-04-16 | 2013-03-06 | 国能飞腾科技有限公司 | Continuous spinning system of poly (p-phenylene terephthalamide) |
| WO2017050220A1 (en) * | 2015-09-25 | 2017-03-30 | 清华大学 | Preparation method for para-aramid fiber |
| US10781536B2 (en) | 2015-09-25 | 2020-09-22 | Tsinghua University | Preparation method of para-aramid nanofibers |
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