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Method for preparing polyphenylene sulfide by taking N-methyl-imidazole derivative as solvent

A technology of methyl imidazole and polyphenylene sulfide, which is applied in the preparation of polyphenylene sulfide (PPS) materials and the field of PPS preparation, can solve the problems of inconvenient use, low solvent recovery rate, high price and the like, and achieve improved heat resistance. , good appearance, the effect of improving the solvent recovery rate

Active Publication Date: 2012-09-12
CHANGZHOU XIAOGUO INFORMATION SERVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many advantages in this process, raw materials are easily available, the yield is over 90%, and the product quality is good, etc., but this process route also has serious disadvantages: ①The solvent N-methylpyrrolidone (NMP) is expensive and consumes a lot ; ②NMP itself has reactivity, which will form PPS with pyrrolidone end groups, thus affecting the solvent resistance of PPS (this is the most important performance of PPS); ③High temperature and pressure reaction promotes the decomposition of solvent NMP, and the solvent recovery rate is low
Although the boiling point of sulfolane is above 280°C, it is easy to decompose above 220°C, producing sulfur dioxide and polymers, inhibiting the synthesis reaction of PPS and seriously affecting product quality
In addition, the melting point of sulfolane is 27~28°C, which is inconvenient to use
Therefore, there is no practical value in synthesizing PPS with sulfolane as a solvent.

Method used

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  • Method for preparing polyphenylene sulfide by taking N-methyl-imidazole derivative as solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 . Add 34 g Na to a 500 mL autoclave 2 S·xH 2 O (containing 62% sodium sulfide and 36% water), 1.9 g LiCl, and 120 g 1-methyl-3-(3-carbonyl) butyryl imidazolium hydrogen sulfide were used as solvents. Seal the autoclave, feed nitrogen gas, and dehydrate 7.5g at a temperature not higher than 190°C. After dehydration, cool down to 50°C, add 45 g p-DCB (0.3mol) [p-DCB:Na 2 S=1:0.95 (molar ratio)] and 0.95 g DMA, and add 60 g of solvent. With mechanical stirring, keep the reaction at 170°C for 5 h and 240°C for 3 h. After the reaction is completed, the temperature is lowered to take the feed solution for post-processing. Feed liquid is suction filtered. The filter cake is washed with water, pickled and then washed with water. The solid material is dried to constant weight. The reaction results are listed in Table 1.

Embodiment 2

[0029] Example 2 . Add 73 g Na to a 500 mL autoclave 2 S·9H 2 O (32% sodium sulfide, 68% water), 1.3 g Li 3 PO 3 , 100 g of 1-methyl-3-(2-cyano) propyl imidazolium bromide as solvent. Close the autoclave, feed nitrogen gas, and dehydrate 43.5g under the condition of not higher than 190°C. After dehydration, cool down to 50°C, add 45 g p-DCB (0.3mol) [p-DCB:Na 2 S=1:1 (molar ratio)] and 0.8 g PNP, and 35 g of solvent was added. Stir mechanically, keep at 200°C for 3 h and 220°C for 4 h. After the reaction is completed, the temperature is lowered to take the feed solution for post-processing. Feed liquid is suction filtered. The filter cake is washed with water, pickled and then washed with water. The solid material is dried to constant weight. The reaction results are listed in Table 1.

Embodiment 3

[0030] Example 3 . Add 45.5 g Na to a 500 mL autoclave 2 S·xH 2 O (containing 62% sodium sulfide and 36% water), 2.5 g sodium acetate, and 120 g 1-methyl-3-(3-hydroxy) butylimidazolium chloride were used as solvents. Seal the autoclave, feed nitrogen gas, and dehydrate 10g at a temperature not higher than 190°C. After dehydration, cool down to 50°C, add 45 g p-DCB (0.3mol) [p-DCB:Na 2 S=1:1.2 (molar ratio)] and 0.8 g PH, and add 60 g of solvent. With mechanical stirring, the reaction was maintained at 140°C for 8 h and at 260°C for 2 h. After the reaction is completed, the temperature is lowered to take the feed solution for post-processing. Feed liquid is suction filtered. The filter cake is washed with water, pickled and then washed with water. The solid material is dried to constant weight. The reaction results are listed in Table 1.

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Abstract

The invention discloses a method for preparing polyphenylene sulfide by taking N-methyl-imidazole derivative as a solvent, and belongs to the field of polymeric chemical industry. The method comprises the following steps: adding industrial sodium sulfide (Na2S.xH2O), a catalyst and the solvent into an autoclave in a certain ratio; dehydrating the mixture at a temperature of not above 190 DEG C; cooling after dehydration; adding p-dichlorobenzene (p-DCB) and an auxiliary agent, and supplementing the solvent; mechanically stirring the mixture, and performing temperature-programmed reaction; after the reaction, cooling and taking material liquid for post-processing; filtering and separating the material liquid; washing a filter cake; and drying the filter cake to obtain PPS (polyphenylene sulfide) resin crude powder. The N-methyl-imidazole compound which is more stable than NMP (N-methyl pyrrolidone) and is high in polarity is taken as the solvent, so that the smooth progression of the reaction is facilitated, the heat resistance of the reaction product PPS is improved, the appearance of the reaction product PPS is better, and the solvent recycling rate is improved.

Description

technical field [0001] The invention belongs to the field of polymer chemical industry, and relates to a preparation method of polyphenylene sulfide (PPS) material. More specifically, it is a method for preparing PPS by using N-methylimidazole derivatives as solvents. [0002] Background technique [0003] PPS is the sixth largest engineering plastic. It has excellent properties such as high temperature resistance, solvent resistance, corrosion resistance, and flame retardancy. It is widely used in machinery, electronics, chemical industry, national defense, and cutting-edge technology fields. Worldwide, the annual output of PPS is close to 200,000 tons, and most of the manufacturers are located in the United States, Japan, Germany and Belgium. The main method of industrial production of PPS is the synthesis of PPS by sodium sulfide method, that is, the Phillips route. Its synthesis method is as follows: [0004] [0005] This process is proposed by US Patent 3,354,12...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0254
Inventor 单玉华储海霞常斌斌毛翠霞侯蓉
Owner CHANGZHOU XIAOGUO INFORMATION SERVICES