CN102336907A - Method for washing poly terephthaloyl-p-phenylene diamine polymer - Google Patents
Method for washing poly terephthaloyl-p-phenylene diamine polymer Download PDFInfo
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Abstract
A method for washing a poly terephthaloyl-p-phenylene diamine polymer belongs to the field of chemical engineering and relates to a washing technology of a polymeric material. The method provided by the invention comprises the following washing steps of: taking a polymer mixture, adding desalinized water which accounts for 2-4 times the weight of the polymer mixture, stirring for 5-10 minutes at room temperature, followed by vacuum filtration; repeating one more time; adding 0.01-0.05% of dilute nitric acid which accounts for 2-4 times the weight of the polymer mixture, stirring for 5-10 minutes at room temperature, followed by vacuum filtration; repeating one more time; drying and warehousing for later use; taking ash samples and contrasting: carrying out vacuum drying on the washed polymer for 10 hours at the temperature of 120 DEG C, determining the polymer ash according to A method in the GB-T 12006.3 standard, wherein the calcining time is 5 hours and the calcining temperature is 800 DEG C. It is known from the ash retention after washing that the washing method with the least ahs retention is the optimal method in the several washing methods; by the method provided by the invention, the poly terephthaloyl-p-phenylene diamine polymer is washed clean, the application amount of the desalinized water is reduced and the filtrate treatment cost is decreased.
Description
Technical field
Belong to field of chemical engineering, relate to the washing technology of polymer materials, exactly relate to the polymeric washing methods of a kind of PPTA.
Background technology
The Fanglun 1414 also claims para-aramid fiber; Para-aramid fiber is present the widest, the fiber that has the call of purposes in the high-performance fiber in the world; Be the first-selection of making high-strength light plate armour and special type protection material, be widely used in fields such as space flight, aviation, military project, electromechanics, building, automobile, sports goods.
Low-ash PPTA polymer is preparation high quality Fanglun 1414's a important prerequisite, and the said PPTA polymer of the present invention chemical structure is following:
The main means that reduce ash content are washing polymers, and PPTA polymer washing situation is following at present:
After the PPTA polyreaction finishes; Adopt polymer mixture quality 2-3 de-salted water washing doubly 3-5 time, oven dry makes the PPTA polymer, and the polymer ash content is generally more than 400ppm; This kind method is simple; Water consumption is also little, but the polymer ash content is higher, influences the spinning technique of p-aramid fiber.
Chinese patent CN 101456951A discloses the purging method in a kind of p-aramid fiber production processes of polyalcohol.This method adds in polymer mixture earlier and is equivalent to 20 times of de-salted waters of simple polymerisation body; With sodium hydroxide solution regulation system pH value to 3-5; Add 20 times of de-salted water repetitive scrubbings 5 times again after filtering then; Use 20 times 0.02%EDTA disodium salt solution washing 3 times at last, de-salted water washing 2 times makes the p-aramid fiber polymkeric substance behind the filtering drying.This method can be clean with the solvent cleaning that is adsorbed in the polymerization process in the polymkeric substance, can also the calcium chloride that be added in the polymer process wherein be cleaned up, and wherein calcium ion content can clean to below the 50ppm.But the de-salted water usage quantity is 220 times of simple polymerisation physique amount when adopting this method, is about as much as the de-salted water of 22 times of polymer mixtures, and so the big water loss processing cost that can cause filtrating is very high, is unfavorable for the through engineering approaches of this technology; The affiliation that adds of sodium hydroxide solution causes polymeric part degraded, also can introduce new sodium ion to polymer simultaneously; EDTA disodium salt price is more expensive, has increased the polymeric production cost of p-aramid fiber.
Summary of the invention
The present invention provides and reduces de-salted water usage quantity and filtrating processing cost, and minimum a kind of of the ash content after the washing gathers the paraphenylene terephthalamide to the polymeric washing methods of diamines.
A kind ofly gather the paraphenylene terephthalamide to the polymeric washing methods of diamines, comprise detection, the contrast of washing back to the polymer ash content, its scheme is: clean according to the following steps obtain gather the paraphenylene terephthalamide to the diamines polymer, the ash content of mensuration is minimum; It comprises that following washing step is:
1) gets a polymer mixture, add polymer mixture weight 2-4 de-salted water doubly, stirred 5-10 minute vacuum filtration under the room temperature;
2) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 1 same amount at room temperature stirs the time identical with step 1, vacuum filtration;
3) adding polymer mixture weight 2-4 mass percent concentration doubly is rare nitric acid of 0.01%～0.05%, stirs 5-10 minute vacuum filtration under the room temperature;
4) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 3 same amount at room temperature stirs the time identical with step 3, vacuum filtration;
5) with the polymer mixture behind the vacuum filtration, add polymer mixture weight 2-4 de-salted water doubly, stirred 5-10 minute vacuum filtration under the room temperature;
6) dry, warehouse-in is for use;
7) get the contrast of ash content appearance: the polymer after the washing is pressed A method mensuration polymer ash content in GB-T 12006.3 standards 120 ℃ of following vacuum-dryings 10 hours, and wherein calcination time is 5 hours, 800 ℃ of calcining temperatures.
Positively effect after the embodiment of the present invention is:
Can know that from cleaning back ash content retention amount this purging method ash content retention amount is minimum, be method best in these several kinds of purging methods; Not only wash totally, and reduced the de-salted water usage quantity, reduced the filtrating processing cost.
Embodiment
In order to further specify the present invention, specifically set forth in conjunction with following examples:
Embodiment 1:
(1) gets the 1000g polymer mixture, add the 2000g de-salted water, stirred 5 minutes vacuum filtration under the room temperature.
(2) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 1 same amount at room temperature stirs the time identical with step 1, vacuum filtration.
(3) adding 2000g mass percent concentration is rare nitric acid of 0.01%, stirs 5 minutes vacuum filtration under the room temperature.
(4) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 3 same amount at room temperature stirs the time identical with step 3, vacuum filtration.
(5) add the 2000g de-salted water, stirred 5 minutes vacuum filtration under the room temperature.
Polymer after the washing is pressed A method mensuration polymer ash content in GB-T 12006.3 standards 120 ℃ of following vacuum-dryings 10 hours, and wherein calcination time is 5 hours, 800 ℃ of calcining temperatures.The polymer ash content that records is 46ppm.
Embodiment 2:
(1) gets the 1000g polymer mixture, add the 3000g de-salted water, stirred 5 minutes vacuum filtration under the room temperature.
(2) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 1 same amount at room temperature stirs the time identical with step 1, vacuum filtration.
(3) adding 3000g mass percent concentration is rare nitric acid of 0.03%, stirs 5 minutes vacuum filtration under the room temperature.
(4) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 3 same amount at room temperature stirs the time identical with step 3, vacuum filtration.
(5) add the 3000g de-salted water, stirred 5 minutes vacuum filtration under the room temperature.
Polymer after the washing is pressed A method mensuration polymer ash content in GB-T 12006.3 standards 120 ℃ of following vacuum-dryings 10 hours, and wherein calcination time is 5 hours, 800 ℃ of calcining temperatures.The polymer ash content that records is 30ppm.
Embodiment 3:
(1) gets the 1000g polymer mixture, add the 3000g de-salted water, stirred 10 minutes vacuum filtration under the room temperature.
(2) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 1 same amount at room temperature stirs the time identical with step 1, vacuum filtration.
(3) adding 3000g mass percent concentration is rare nitric acid of 0.05%, stirs 10 minutes vacuum filtration under the room temperature.
(4) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 3 same amount at room temperature stirs the time identical with step 3, vacuum filtration.
(5) add the 3000g de-salted water, stirred 10 minutes vacuum filtration under the room temperature.
Get ash content sample contrast condition: the polymer after the washing is pressed A method mensuration polymer ash content in GB-T 12006.3 standards 120 ℃ of following vacuum-dryings 10 hours, and wherein calcination time is 5 hours, 800 ℃ of calcining temperatures.The polymer ash content that records is 26ppm.
Contrast other purging methods, clean back ash content retention amount result:
Comparative Examples 1:
(1) gets the 1000g polymer mixture, add the 3000g de-salted water, stirred 10 minutes vacuum filtration under the room temperature.
(2) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 1 same amount at room temperature stirs the time identical with step 1, vacuum filtration.
(3) repeating step (2) washes polymkeric substance 3 times with de-salted water.
(4) polymer after the washing is pressed A method mensuration polymer ash content in the GB-T12006.3 standard 120 ℃ of following vacuum-dryings 10 hours, and wherein calcination time is 5 hours, 800 ℃ of calcining temperatures.The polymer ash content that records is 448ppm.
Comparative Examples 2:
(1) gets the 1000g polymer mixture, add the 2000g de-salted water.
(2) continuing to add NaOH solution adjusting pH value is 4, stirs 20 minutes.
(3) coarse filtration polymkeric substance, and then in polymkeric substance, add the 2000g de-salted water, stirred 20 minutes.
(4) repeating step (3) washes polymkeric substance 5 times with de-salted water.
(5) de-salted water is changed into 0.02% EDTA disodium salt solution, repeating step (3) flushing 3 times.
(6) use de-salted water repeating step (3) at last, wash 2 times after-filtration dry the p-aramid fiber polymkeric substance.
Press A method mensuration polymer ash content in GB-T 12006.3 standards, wherein calcination time is 5 hours, 800 ℃ of calcining temperatures.The polymer ash content that records is 40ppm.
Claims (1)
1. one kind is gathered the paraphenylene terephthalamide to the polymeric washing methods of diamines, comprises detection, the contrast of washing back to the polymer ash content, and it is characterized in that: that cleans acquisition according to the following steps gathers the paraphenylene terephthalamide to the diamines polymer, and the ash content of mensuration is minimum; It comprises that following washing step is:
1) gets a polymer mixture, add polymer mixture weight 2-4 de-salted water doubly, stirred 5-10 minute vacuum filtration under the room temperature;
2) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 1 same amount at room temperature stirs the time identical with step 1, vacuum filtration;
3) adding polymer mixture weight 2-4 mass percent concentration doubly is rare nitric acid of 0.01%～0.05%, stirs 5-10 minute vacuum filtration under the room temperature;
4) with the polymer mixture behind the vacuum filtration, the de-salted water of adding and step 3 same amount at room temperature stirs the time identical with step 3, vacuum filtration;
5) with the polymer mixture behind the vacuum filtration, add and be equivalent to polymer mixture weight 2-4 de-salted water doubly, stirred 5-10 minute vacuum filtration under the room temperature;
6) dry, warehouse-in is for use;
7) get ash content sample contrast condition: the polymer after the washing is pressed A method mensuration polymer ash content in GB-T 12006.3 standards 120 ℃ of following vacuum-dryings 10 hours, and wherein calcination time is 5 hours, 800 ℃ of calcining temperatures.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101686912A CN102336907B (en) | 2011-06-22 | 2011-06-22 | Method for washing poly terephthaloyl-p-phenylene diamine polymer |
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| CN2011101686912A CN102336907B (en) | 2011-06-22 | 2011-06-22 | Method for washing poly terephthaloyl-p-phenylene diamine polymer |
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| CN102336907B CN102336907B (en) | 2012-11-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110698669A (en) * | 2019-10-25 | 2020-01-17 | 中芳特纤股份有限公司 | Method for cleaning poly (p-phenylene terephthalamide) resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057602A (en) * | 1989-11-03 | 1991-10-15 | E. I. Dupont De Nemours And Company | Para-phenylene diamine polymer color improvement with sequestering agent |
| CN1693548A (en) * | 2004-05-09 | 2005-11-09 | 邢哲 | Method of producing poly(terephthaloyl-p-phenylene diamine) fibre |
| CN101456951A (en) * | 2008-10-28 | 2009-06-17 | 烟台氨纶股份有限公司 | Cleaning method in production process of para-aramid polymer |
-
2011
- 2011-06-22 CN CN2011101686912A patent/CN102336907B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057602A (en) * | 1989-11-03 | 1991-10-15 | E. I. Dupont De Nemours And Company | Para-phenylene diamine polymer color improvement with sequestering agent |
| CN1693548A (en) * | 2004-05-09 | 2005-11-09 | 邢哲 | Method of producing poly(terephthaloyl-p-phenylene diamine) fibre |
| CN101456951A (en) * | 2008-10-28 | 2009-06-17 | 烟台氨纶股份有限公司 | Cleaning method in production process of para-aramid polymer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110698669A (en) * | 2019-10-25 | 2020-01-17 | 中芳特纤股份有限公司 | Method for cleaning poly (p-phenylene terephthalamide) resin |
| CN110698669B (en) * | 2019-10-25 | 2022-02-11 | 中芳特纤股份有限公司 | Method for cleaning poly (p-phenylene terephthalamide) resin |
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| CN102336907B (en) | 2012-11-28 |
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Address after: 201111 room 212, floor 2, building 6, No. 60, Zhonghui Road, Minhang District, Shanghai Patentee after: Shanghai Zhouhan fiber material technology Co.,Ltd. Address before: No. 1-3, Xingnan Road, Minhang District, Shanghai, 200237 Patentee before: SHANGHAI ZHOUHAN FIBER MATERIAL TECHNOLOGY Co.,Ltd. |
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