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Method for preparing polyphenylene sulfide by using composite catalyst

A technology of composite catalyst and polyphenylene sulfide, which is applied in the field of polymer engineering, can solve problems affecting normal production, poor product quality, and poor catalytic effect, and achieve the effects of improving catalytic effect, reducing dosage, and saving energy

Inactive Publication Date: 2017-05-24
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Sodium acetate, as a catalyst for preparing polyphenylene sulfide, overcomes the shortcoming of high price of lithium chloride as a catalyst, but pure sodium acetate is used as a catalyst for preparing polyphenylene sulfide, and the catalytic effect is poor, and the polymerization time is as long as 4 to 6 hours. The temperature is as high as 265-270°C, the synthesis cycle is long, the energy consumption is high, the product quality is poor, and the melt flow rate is above 400g / min, so it can only be used as a low-end modified filler
At the same time, after the synthesis reaction is completed, a large amount of sodium acetate will be precipitated during the cooling process, and mixed with low molecular weight substances, which will easily scale on the reactor wall and cooling coils, resulting in difficulty in cooling and affecting normal production.

Method used

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  • Method for preparing polyphenylene sulfide by using composite catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take by weighing industrial grade pentahydrate crystalline sodium sulfide 1500Kg (according to the main content, this is the quantitative benchmark), take by weighing industrial grade p-dichlorobenzene, composite catalyst (lithium chloride The molar ratio to sodium acetate is 0.3:1), solvent N-methylpyrrolidone, caustic soda, and polymerize in a reactor. The evaporative dehydration temperature is 195°C, the first stage polymerization temperature is 225±2°C, the time is 45 minutes, the stirring speed is 25rpm, the second stage polymerization temperature is 262±2°C, the time is 150 minutes, the stirring speed is 40rpm. After the polymerization reaction, the reaction material was cooled to 165° C., separated, washed and dried to obtain 850 kg of polyphenylene sulfide product with a yield of 88.17%. After analysis, the melting point of the product is 280°C, the melt flow rate is 185g / min, and the ash content is 0.3%. The product can be used for spinning and injection moldin...

Embodiment 2

[0027] Take by weighing 3 water crystalline sodium sulfide 1350Kg (according to the main content, this is the quantitative benchmark), take by weighing industrial grade p-dichlorobenzene in molar ratio 1:0.995:0.42:6.0:0.025, composite catalyst (lithium chloride and acetic acid The molar ratio of sodium is 0.5:1), the solvent N-methylpyrrolidone and caustic soda are polymerized in the reactor. The evaporative dehydration temperature is 190°C, the first stage polymerization temperature is 224±2°C, the time is 60 minutes, the stirring speed is 20rpm, the second stage polymerization temperature is 265±2°C, the time is 120 minutes, the stirring speed is 35rpm. After the polymerization reaction, the reaction material was cooled to 170° C., separated, washed and dried to obtain 920 kg of polyphenylene sulfide product with a yield of 83.29%. After analysis, the melting point of the product is 280°C, the melt flow rate is 180g / min, and the ash content is 0.25%. The product can be used...

Embodiment 3

[0029] Take by weighing 800Kg of crystalline sodium sulfide pentahydrate, 700Kg of crystalline sodium sulfide trihydrate (according to the main content, this is the quantitative benchmark), take by weighing industrial grade p-dichlorobenzene with a molar ratio of 1:0.990:0.50:6.5:0.025, compound The catalyst (the molar ratio of lithium chloride to sodium acetate is 0.2:1), the solvent N-methylpyrrolidone and caustic soda are polymerized in a reactor. The evaporative dehydration temperature is 192°C, the first stage polymerization temperature is 224±2°C, the time is 50 minutes, the stirring speed is 35rpm, the second stage polymerization temperature is 265±2°C, the time is 130 minutes, the stirring speed is 55rpm. After the polymerization reaction, the reaction material was cooled to 170° C., separated, washed and dried to obtain 935 kg of polyphenylene sulfide product with a yield of 86.02%. After analysis, the melting point of the product is 282°C, the melt flow rate is 220g / ...

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Abstract

The invention relates to the technical field of polymer engineering, in particular to a method for preparing polyphenylene sulfide by using a composite catalyst. The method comprises the steps: adding a sodium sulfide crystal, a solvent and caustic soda into a reaction container, heating under the protection of nitrogen, completely dissolving the added materials, and evaporating part of water and solvent; dissolving paradichlorobenzene and the composite catalyst into the solvent, adding the solution into a reactor, heating and performing polymerization reaction to prepare the polyphenylene sulfide. When the polyphenylene sulfide is prepared by the method, scaling is avoided after the polymerization reaction and in the process of cooling the materials, the reaction byproducts are easy to separate, and the comprehensive performance and the yield of the product are high.

Description

technical field [0001] The invention relates to the technical field of polymer engineering, in particular to a method for preparing polyphenylene sulfide with a composite catalyst. Background technique [0002] PPS is a polymer compound with good heat resistance, chemical corrosion resistance and flame retardancy. It can be widely used in special fields such as electronic appliances, automobile manufacturing, food machinery, petrochemical, military and other industries. It is known as Following polycarbonate (PC), polyoxymethylene (POM), polyester (PET), nylon (PA) and polyphenylene oxide (PPO), it is the sixth largest general-purpose engineering plastic and one of the eight major aerospace materials. [0003] The industrial production of PPS mainly adopts the sodium sulfide method. The sodium sulfide method uses p-dichlorobenzene and crystalline sodium sulfide as raw materials, and uses N-methylpyrrolidone (NMP) as a solvent to perform high-temperature polycondensation unde...

Claims

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Application Information

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IPC IPC(8): C08G75/0254
CPCC08G75/0254
Inventor 杨永彬颜杰杨虎刘建容
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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