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Manufacturing method of polyphenylene sulfide resin

A technology of polyphenylene sulfide resin and manufacturing method, which is applied in the field of polyphenylene sulfide resin manufacturing, can solve problems such as the sustainable operation of the salt solution concentration process, the impact on the ecological environment, and resource waste, and achieve the realization of waste water and waste resources. The effects of efficient utilization, lower production cost, and reduced waste discharge

Pending Publication Date: 2020-06-09
CHONGQING JUSHI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, in order to improve product quality, reaction aids such as organic acid sodium salt and lithium salt will be added to the reaction system. Compared with the former, lithium salt as a polymerization aid has certain advantages in terms of PPS synthesis control and product quality. Due to its high price and difficulty in recycling, it directly restricts the reduction of PPS production cost
Current PPS production technology mainly contains precipitation method (US5635587A, CN101205298B, CN102276838B and CN106565956B) and organic solvent extraction method (US5262137A, CN102675683B, CN104877167B and CN106565581A) about lithium salt recovery, but these means not only need to add a large amount of precipitation agent or organic solvent In actual production, it is not considered that the accumulation of a large amount of organic matter caused by the closed cycle process will hinder the sustainable operation of the brine concentration process
CN 104877167B removes solid oligomers and salt by-products in the synthetic filtrate by filtration and is directly used in the synthesis reaction, but this method may affect the quality and stability of PPS products for the neglect of organic matter and salts dissolved in the solvent
On the other hand, the salt by-products of the CN 103897187B synthesis reaction cannot be rationally utilized after being incinerated to cause waste of resources, and also have a negative impact on the ecological environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In the 100L reactor, N-methyl-2-pyrrolidone (hereinafter referred to as NMP) 54.52kg (550mol), polyhydrate sodium sulfide (hereinafter referred to as Na 2 S) 16.81kg (100mol), 0.18kg (4.5mol) of sodium hydroxide and 1.91kg (45mol) of lithium chloride are heated to 190°C at room temperature of 0.5°C / min under nitrogen protection until the dehydration rate reaches 70%.

[0027]Then add p-dichlorobenzene (hereinafter referred to as p-DCB) 14.70kg (100mol), NMP 14.87kg (150mol) to the above-mentioned dehydration-completed reaction solution, heat up to 230°C at 0.5°C / min, keep constant temperature for 1h, and then add 0.5°C / min. The temperature was raised to 270°C at a ℃ / min rate, kept at a constant temperature for 2.5 hours, and then cooled to 140°C by 1 hour after completion.

[0028] The above synthetic slurry was centrifugally filtered, the filter cake was washed with 80-90 ℃ hot water until the electrical conductivity was qualified, then centrifugally filtered, and the ...

Embodiment 2

[0032] In the 100L reactor, N-methyl-2-pyrrolidone (hereinafter referred to as NMP) 54.52kg (550mol), polyhydrate sodium sulfide (hereinafter referred to as Na 2 S) 16.81kg (100mol), 0.18kg (4.5mol) of sodium hydroxide and 1.91kg (45mol) of lithium chloride are heated to 135°C at room temperature at 2°C / min under nitrogen protection until the dehydration rate reaches 70%.

[0033] Then add p-dichlorobenzene (hereinafter referred to as p-DCB) 14.70kg (102mol), NMP 14.87kg (150mol) to the above-mentioned dehydration-completed reaction solution, heat up to 230°C at 0.5°C / min, keep constant temperature for 1h, and then add 0.5°C / min. The temperature was raised to 265°C at a ℃ / min rate, kept at a constant temperature for 3 hours, and then cooled to 120°C through 1 hour after completion.

[0034] The above-mentioned synthetic slurry was centrifugally filtered, the filter cake was washed with 80-90 ℃ hot water until the electrical conductivity was qualified, then centrifugally filter...

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PUM

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Abstract

The invention discloses a manufacturing method of polyphenylene sulfide resin. The method is characterized by comprising the steps: taking sodium sulfide polyhydrate and p-dichlorobenzene as raw materials; taking N-methyl-2-pyrrolidone as a solvent, simultaneously adding an alkaline stabilizer and a lithium salt auxiliary agent, carrying out condensation polymerization synthesis, and carrying outsegmented recovery on slurry containing polyphenylene sulfide, so as to obtain polyphenylene sulfide with the melt mass flow rate of 100-1200 g / 10min. Meanwhile, the treatment process that the solventand the auxiliaries can be recycled and salt byproducts can be utilized is achieved, waste discharge is reduced while the production cost is reduced, and resource utilization of waste water and wasteis achieved.

Description

technical field [0001] The present application relates to the technical field of polyphenylene sulfide resin manufacturing, in particular to a method for manufacturing polyphenylene sulfide resin in which solvents and auxiliary agents are recyclable and salt by-products are available. Background technique [0002] Polyphenylene Sulfide (PPS) is a high-performance thermoplastic resin with the advantages of high mechanical strength, high temperature resistance, non-flammability, and good thermal stability. It is widely used in electronics, automobiles, machinery and chemicals. and other fields. At present, the PPS manufacturing method mainly adopts the polycondensation reaction of alkali metal sulfides or hydrosulfides and polyhalogenated aromatic compounds in aprotic organic solvents in the presence of reaction stabilizers and auxiliary agents. [0003] In order to reduce the production cost, the PPS reaction filtrate and the cleaning solution are usually mixed by step-wise ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0268C08G75/0213C08G75/0281
CPCC08G75/0213C08G75/0268C08G75/0281
Inventor 吕天生李乾华王政谢晓鸿陈尚敬胡洪铭杨思瑶
Owner CHONGQING JUSHI NEW MATERIAL TECH CO LTD