CN85102664B - Process for synthesis of linear polyphenylthioether of high molecular weight - Google Patents
Process for synthesis of linear polyphenylthioether of high molecular weightInfo
- Publication number
- CN85102664B CN85102664B CN198585102664A CN85102664A CN85102664B CN 85102664 B CN85102664 B CN 85102664B CN 198585102664 A CN198585102664 A CN 198585102664A CN 85102664 A CN85102664 A CN 85102664A CN 85102664 B CN85102664 B CN 85102664B
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- China
- Prior art keywords
- molecular weight
- high molecular
- reaction
- present
- synthesis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for synthesizing high molecular weight linear polyphenylene sulfide by using p-dichlorobenzene and sodium sulfide as raw materials. A normal-pressure reaction instead of a pressurized reaction in the existing art is adopted to cancel the application of 1, 2, 4,-trichlorobenzene in the system in the existing art. Hexaphosphoamine is used as a solvent, and anhydrous sodium phosphate is used as an auxiliary agent. The present invention has the advantages of reaction equipment simplification, reaction period shortening, product yield and product quality improvement, and cost reduction. The present invention is favorable to the popularization of the method and the industrialization of the production.
Description
The invention belongs to the improvement of synthesis method of high molecular weight pps.
Synthesis method of high molecular weight pps, as United States Patent (USP) 4,303, described in 781, with santochlor, moisture sodium sulphite or with the mixture of water, 1,2,4-trichlorobenzene is raw material, adds sodium phosphate containing crystal water (or water-bearing phosphate potassium, or other carboxylate salt) to make catalyzer, N-methyl-2-pyrrolidone alkane is solvent, adds to depress carry out polycondensation at 190～275 ℃.Wherein catalyzer and sodium sulphite mol amount ratio are 1: 0.1～1.5, before polymerization from room temperature to 202 ℃ thermal dehydration polyreaction, can obtain the polyphenylene sulfide of side chain, limiting viscosity is not higher than 0.35 (206 ℃, α-chloronaphthalene), this method is synthesized polyphenylene sulfide, owing to having adopted many halobenzenes to make raw material, therefore can not obtain linear polyphenylthioether; Because adopt higher temperature and pressure, thus equipment complexity, condition harshness; Add material in reaction with water, must before reaction, remove, cause the reaction times to increase, solvent loss is larger, simultaneously because there being aqueous systems heating to cause the decomposition of part material and solvent, ratio of components in system is restive and make molecular weight of product poor reproducibility like this, and produces the etching problem to equipment; Reaction system component is more, aftertreatment difficulty.Various reasons, makes production cost higher.Object of the present invention is just to find a kind of method that can overcome above-mentioned shortcoming and can synthesize desirable linear polyphenylthioether.
Main points of the present invention are with santochlor, Sodium sulphate anhydrous, 99min is raw material, adding anhydrous sodium phosphate is catalyzer, its mol amount ratio is santochlor: Sodium sulphate anhydrous, 99min: anhydrous sodium phosphate=1: 1: 0.75, make solvent with hempa, carry out normal pressure polycondensation at 210～228 ℃, obtain the high molecular weight polyphenylene sulfide of line style, limiting viscosity reaches 0.437.
In the present invention, Sodium sulphate anhydrous, 99min used is to adopt industrial sodium sulfide through the dissolving crystallized pure nine water cure sodium (Na that make of tap water
2s9H
2o), then nine water cure sodium reduced pressure to (overbottom pressure < 15 mmhg) temperature-gradient method (normal temperature to 160 ℃) dehydration and obtain.
The mensuration of limiting viscosity of the present invention, take α-chloronaphthalene as solvent, 0.4 gram of polyphenylene sulfide/100 milliliter α-chloronaphthalene is measured at 206 ℃, and result is calculated by following formula:
〔η〕＝1nη
r/C
η
r=t/t
0: ... relative viscosity
T
0: the solvent elution time; T: solution elution time
C: strength of solution, grams per milliliter
Compared with the prior art the present invention, has equipment simple, and temperature of reaction reduces, and synthesis cycle shortens, and solvent is beneficial to and reclaims output and quality compared with advantages of higher.
Embodiment adds respectively hempa 100ml in reactor, 24.6 grams of anhydrous sodium phosphates, and 17.0 grams of the Sodium sulphate anhydrous, 99mins that content is 92%, 29.4 grams of santochlor, 210-228 ℃ of reaction 5 hours, obtain white (or near-white) mixture.By hot deionized water and washing with alcohol reaction product, dry, obtain 19.8 grams of polyphenylene sulfides, yield 91.4%, its limiting viscosity (η) 0.437, its melt viscosity 25949 is moored.
Claims (2)
1. be the method for the synthetic high molecular weight polyphenylene sulfide of raw material with santochlor, sodium sulphite, it is characterized in that anhydrous sodium phosphate is catalyzer take Sodium sulphate anhydrous, 99min as sulphur source, hempa is made solvent, carries out normal pressure polycondensation at 210-228 ℃.
2. according to the said method of claim 1, it is characterized in that the mol amount ratio of anhydrous sodium phosphate and Sodium sulphate anhydrous, 99min is 0.75: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585102664A CN85102664B (en) | 1985-04-01 | 1985-04-01 | Process for synthesis of linear polyphenylthioether of high molecular weight |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585102664A CN85102664B (en) | 1985-04-01 | 1985-04-01 | Process for synthesis of linear polyphenylthioether of high molecular weight |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85102664A CN85102664A (en) | 1986-09-24 |
| CN85102664B true CN85102664B (en) | 1987-08-26 |
Family
ID=4792665
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN198585102664A Expired CN85102664B (en) | 1985-04-01 | 1985-04-01 | Process for synthesis of linear polyphenylthioether of high molecular weight |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85102664B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095481C (en) * | 2000-12-27 | 2002-12-04 | 古旗高 | Process for preparing high-density high-molecular linear polyphenyl thioether |
| CN103951825B (en) * | 2014-04-29 | 2016-03-30 | 四川中科兴业高新材料有限公司 | A kind of high strength polyphenylene sulfide and preparation method thereof |
| CN108479730A (en) * | 2018-04-16 | 2018-09-04 | 江苏欣诺科催化剂有限公司 | A kind of adsorbent of catalyst and application thereof |
| CN108976421A (en) * | 2018-07-26 | 2018-12-11 | 四川中科兴业高新材料有限公司 | A kind of preparation method of film-grade PPS resin |
-
1985
- 1985-04-01 CN CN198585102664A patent/CN85102664B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85102664A (en) | 1986-09-24 |
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| C06 | Publication | ||
| C13 | Decision | ||
| GR02 | Examined patent application | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |