CN85100134A - The synthesis technique of PPTA - Google Patents
The synthesis technique of PPTA Download PDFInfo
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- CN85100134A CN85100134A CN 85100134 CN85100134A CN85100134A CN 85100134 A CN85100134 A CN 85100134A CN 85100134 CN85100134 CN 85100134 CN 85100134 A CN85100134 A CN 85100134A CN 85100134 A CN85100134 A CN 85100134A
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- add
- ursol
- pyridine
- ppta
- methyl pyrrolidone
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- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The synthesis technique of PPTA, it belongs to macromolecular compound synthetic technical field.In the polymeric kettle of N-Methyl pyrrolidone is housed, add lithium chloride (be charging capacity 1.2～1.8%) and pyridine (pyridine/Ursol D=0.6～1.20 mole ratio), add Ursol D then, (PPD concentration is 0.20～0.45mol/l to add the p-phthaloyl chloride powder after the dissolving in two steps, TCl excessive 0.30～2.5%), be reflected at N
2Carry out under gas shiled, stirring, the normal pressure, temperature of reaction maintains-5 ℃～80 ℃.The polymer viscosity that generates by this technology stabilizes to 5.5～6.0.
Description
The technical field of the invention is that macromolecular compound is synthetic.
The fiber that is spun into by PPTA (PPTA) resin has high strength, high-modulus, excellent properties such as high temperature resistant, has been the most noticeable specialty synthetic fibre since the seventies.The PPTA resin can be formed by Ursol D (PPD) and p-phthaloyl chloride (TCl) polycondensation, and its primitive reaction formula is as follows:
The common method that realizes this reaction is a low-temperature solution polycondensation.Be about to Ursol D and be dissolved in organic solvent-salts solution, generate PPTA with the p-phthaloyl chloride polycondensation being lower than under 100 ℃ the temperature.Employed organic solvent-salts solution has many kinds, and the Soviet Union has the people to use N-Methyl pyrrolidone-lithium chloride (LiCl) solution.Its technological process is: Ursol D is packed into to be had in the agitator flask, add the N-Methyl pyrrolidone that contains LiCl, dissolved 15 minutes down at 18 ℃～20 ℃, in gained solution, add the TCl(0.025 mol) and α-Jia Jibiding (0.01 mol), continue to stir 60 minutes, take out block from flask, mix with water, polymer precipitation comes out.The logarithmic specific concentration viscosity of surveying polymkeric substance is η
Inh=3.51(day disclosure special permission 53-11994).PPTA resin with this viscosity number can not be spun into high strength fibre.The logarithmic specific concentration viscosity of the PPTA resin of preparation high strength fibre generally should be greater than 5.
The objective of the invention is the technology of carrying out Ursol D and p-phthaloyl chloride polycondensation in N-Methyl pyrrolidone-LiCl solution system is improved the synthetic PPTA resin that is suitable for preparing high strength fibre, viscosity higher (being that molecular weight is higher).
Main points of the present invention are in the polymeric kettle of N-Methyl pyrrolidone is housed, add lithium chloride (be charging capacity weight 1.2～1.8%) and pyridine (pyridine/Ursol D=0.60～1.20, mole ratio), add Ursol D then, add p-phthaloyl chloride powder (PPD concentration is 0.20～0.45mol/l, and TCl excessive 0.30～2.5%) after the dissolving in two steps and be reflected at stirring, normal pressure, N
2Carry out under the gas shiled, temperature of reaction maintains-5 ℃～80 ℃.The amount that adds for the first time p-phthaloyl chloride is preferably 40～60%, is preferably 60～40% for the second time.
In the present invention, before polyreaction begins, join in N-Methyl pyrrolidone-LiCl solution, can increase the solvability of LiCl in N-Methyl pyrrolidone, thereby help improving the molecular weight of PPTA as the pyridine of acid absorber.LiCl add-on, PPD concentration, the excessive number of TCl are conscientiously controlled the molecular weight that also helps improving resin.Add TCl at twice and help deriving heat, polyreaction is carried out more reposefully, also favourable to improving polymericular weight.Therefore according to synthetic PPTA resin of the present invention, molecular weight is higher, and its logarithmic specific concentration viscosity can be stabilized in 5.5～6.0, is fit to make the PPTA resin fibre of high strength and modulus.
Be embodiments of the invention below.
Example 1:
The 50mlN-methyl-2-pyrrolidone is put into polymeric kettle, add 0.60 gram LiCl and 2ml pyridine, at N
2Protection adds 1.3513 gram Ursol D down, adds 1.2814 gram p-phthaloyl chlorides while stirring, stirs to add remaining 1.2814 gram p-phthaloyl chlorides after 5～20 minutes, and reaction remains on to be carried out under 20～40 ℃ 10～20 minutes, obtained η at last
InhIt is 5.02 pale yellow powder shaped polymer.
Example 2:
The 50ml N-Methyl pyrrolidone is put into polymeric kettle, add 0.62 gram LiCl and 1.5ml pyridine, at N
2Gas shiled adds 1.946 gram Ursol D down, adds 1.8455 gram p-phthaloyl chlorides while stirring, stirs 5～10 minutes, adds remaining 1.8455 gram p-phthaloyl chlorides again, reacts under water quench 10～15 minutes, finally obtains η
InhIt is 5.75 pale yellow powder shaped polymer.
Claims (2)
1, a kind of in N-Methyl pyrrolidone-lithium chloride solution, technology by Ursol D and the synthetic PPTA of p-phthaloyl chloride, it is characterized in that in the polymeric kettle of N-Methyl pyrrolidone is housed, add lithium chloride (be charging capacity weight 12～18%) and pyridine (pyridine/Ursol D=0.60～120 mole ratio), add Ursol D then, (PPD concentration is 0.20～0.45mol/l to add the p-phthaloyl chloride powder after the dissolving in two steps, TCl excessive 0.30～2.5%), be reflected at stirring, normal pressure, N
2Carry out under the gas shiled, temperature of reaction maintains-5 ℃～80 ℃.
2,, it is characterized in that the said p-phthaloyl chloride powder that adds in two steps for once adding 40～60%, adds 60～40% for the second time according to the technology of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85100134A CN85100134B (en) | 1985-04-01 | 1985-04-01 | Synthesis technology of p-diacetyl-benzene p-diaminobenzene polymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85100134A CN85100134B (en) | 1985-04-01 | 1985-04-01 | Synthesis technology of p-diacetyl-benzene p-diaminobenzene polymer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85100134A true CN85100134A (en) | 1986-07-09 |
| CN85100134B CN85100134B (en) | 1987-06-17 |
Family
ID=4790914
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85100134A Expired CN85100134B (en) | 1985-04-01 | 1985-04-01 | Synthesis technology of p-diacetyl-benzene p-diaminobenzene polymer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85100134B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265326B (en) * | 2008-04-21 | 2010-12-15 | 中国石化仪征化纤股份有限公司 | Method and device for preparing polypara-phthaloyl para-phenylene diamine resin |
| CN102190795A (en) * | 2010-03-03 | 2011-09-21 | 北京国能新兴化工科技发展有限公司 | Method for preparing poly(p-phenylene terephthalamide) |
| CN110144636A (en) * | 2019-06-10 | 2019-08-20 | 黄河三角洲京博化工研究院有限公司 | A kind of p-aramid fiber fibrid and preparation method thereof |
-
1985
- 1985-04-01 CN CN85100134A patent/CN85100134B/en not_active Expired
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265326B (en) * | 2008-04-21 | 2010-12-15 | 中国石化仪征化纤股份有限公司 | Method and device for preparing polypara-phthaloyl para-phenylene diamine resin |
| CN102190795A (en) * | 2010-03-03 | 2011-09-21 | 北京国能新兴化工科技发展有限公司 | Method for preparing poly(p-phenylene terephthalamide) |
| CN102190795B (en) * | 2010-03-03 | 2014-05-07 | 北京国能新兴化工科技发展有限公司 | Method for preparing poly(p-phenylene terephthalamide) |
| CN110144636A (en) * | 2019-06-10 | 2019-08-20 | 黄河三角洲京博化工研究院有限公司 | A kind of p-aramid fiber fibrid and preparation method thereof |
| CN110144636B (en) * | 2019-06-10 | 2021-09-24 | 黄河三角洲京博化工研究院有限公司 | Para-aramid fibrid and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN85100134B (en) | 1987-06-17 |
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