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Polyphenylene sulfide without lithium chloride and additives, and preparation method and applications thereof

A technology of polyphenylene sulfide resin and catalyst, which is applied in the field of polyphenylene sulfide and its preparation, can solve the problems of high recovery rate of lithium chloride, cumbersome recovery process, long reaction route, etc., and achieve excellent thermal stability, High yield, good fluidity and thermal stability

Pending Publication Date: 2019-05-03
重庆晟淦新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In response to the above-mentioned status quo, people have carried out many explorations, such as using multiple filtration and washing methods to remove by-product salts, but the recovery process of this method is cumbersome and the energy consumption is high; or the precipitation method is used to separate lithium salts, but the precipitation recovered Lithium salt needs to consume other chemical substances, and the precipitate is separated and dehydrated and then reacted with hydrochloric acid to produce lithium chloride. The reaction route is long and the high recovery rate of lithium chloride cannot be guaranteed.

Method used

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  • Polyphenylene sulfide without lithium chloride and additives, and preparation method and applications thereof
  • Polyphenylene sulfide without lithium chloride and additives, and preparation method and applications thereof
  • Polyphenylene sulfide without lithium chloride and additives, and preparation method and applications thereof

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preparation example Construction

[0025] The invention provides a kind of synthetic method of polyphenylene sulfide resin, comprises the following steps:

[0026] S101: Under an inert gas argon atmosphere, add sulfur powder and catalyst into the reactor, then add N-methylpyrrolidone, heat and stir evenly until a uniform suspension is formed in the reactor. Among them, the catalyst includes butyl myristate, La(NO 3 ) 3 and MCM-41 mesoporous molecular sieve; and butyl myristate, La(NO 3 ) 3 The molar ratio of MCM-41 mesoporous molecular sieve is (0.5~2.5):(0.01~0.05):10; the molar ratio of sulfur powder, catalyst, N-methylpyrrolidone and dichlorobenzene is 1:(0.005~ 0.05): (3~8): (1.05~1.30).

[0027] S102: Add dichlorobenzene to the suspension obtained in S101, raise the temperature to 120-150° C. at a rate of 1-5° C. / min, and stir at constant temperature for 1-3 hours.

[0028] S103: Cool the product obtained in S102 to room temperature, then separate the solid from the liquid and collect the solid phase....

Embodiment 1

[0034] The present embodiment provides a kind of synthetic method of polyphenylene sulfide resin, comprises the following steps:

[0035] S101: First, introduce argon gas to replace the gas in the reaction system, and keep the gas flow rate at 90mL / min, add sulfur powder and catalyst into the reaction kettle, then add N-methylpyrrolidone, heat and stir until a uniform suspension. Among them, the molar ratio of sulfur powder, catalyst, N-methylpyrrolidone and dichlorobenzene is 1:0.05:3:1.30 in sequence.

[0036] The catalyst includes butyl myristate, La(NO 3 ) 3 and MCM-41 mesoporous molecular sieve; its preparation method comprises the following steps: S201: butyl myristate, La(NO 3 ) 3 Mix with the carrier and stir until clear, then dry; S202: Place the product obtained in S201 in a nitrogen flow with a gas flow rate of 100mL / min, heat it to 220°C at a heating rate of 1°C / min, then keep the temperature for 5h, and then The temperature was lowered to 50° C. at a cooling ...

Embodiment 2

[0041] The present embodiment provides a kind of synthetic method of polyphenylene sulfide resin, comprises the following steps:

[0042] S101: First, introduce argon gas to replace the gas in the reaction system, and keep the gas flow rate at 60mL / min, add sulfur powder and catalyst into the reaction kettle, then add N-methylpyrrolidone, heat and stir until a uniform suspension. Among them, the molar ratio of sulfur powder, catalyst, N-methylpyrrolidone and dichlorobenzene is 1:0.005:8:1.02 in sequence.

[0043] The catalyst includes butyl myristate, La(NO 3 ) 3 and MCM-41 mesoporous molecular sieve; its preparation method comprises the following steps: S201: butyl myristate, La(NO 3 ) 3 Mix with the carrier and stir until clear, then dry; S202: Place the product obtained in S201 in a nitrogen stream with a gas flow rate of 20mL / min, heat it to 280°C at a heating rate of 3°C / min, then keep the temperature for 2h, and then The temperature was lowered to 80° C. at a coolin...

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Abstract

The invention relates to polyphenylene sulfide without lithium chloride and additives, and a preparation method and applications thereof. The preparation method comprises following steps: S101, at inert gas atmosphere, sulphur powder and a catalyst are introduced into a reaction kettle, a solvent is added, heating and uniform stirring are carried out until a uniform suspension liquid is obtained;S102, dichlorobenzene is added into the uniform suspension liquid, the temperature is increased to 120 to 150 DEG C at a temperature increasing speed of 1 to 5 DEG C / min, and an obtained mixture is stirred for 1 to 3h at a constant temperature; S103, a product obtained in S102 is cooled to room temperature, and is subjected to solid liquid separation so as to obtain a solid phase; and S104, the solid phase is washed with deionized water, and is dried so as to obtain polyphenylene sulfide. According to the preparation method, using of lithium chloride and additives in conventional methods is avoided, the prepared polyphenylene sulfide is excellent in performance, extremely low in chlorine content, and excellent in fluidity and heat stability; synthesis cost is reduced further; and the economic benefit and social benefit in production process are improved effectively.

Description

technical field [0001] The invention relates to the field of polymer resin synthesis, in particular to a polyphenylene sulfide free of lithium chloride and additives, a preparation method and application thereof. Background technique [0002] As a special engineering plastic with outstanding performance, polyphenylene sulfide (PPS) is known as "plastic gold" and is the most cost-effective special engineering plastic so far. . Although the polyphenylene sulfide material has only been used for about 40 years, it has developed rapidly and has become the first brand of special engineering plastics. Polyphenylene sulfide has excellent physical and chemical properties and good compatibility with other materials. It is widely used in high-tech fields such as chemical industry, automobile, electronic appliances, military, environmental protection and aerospace. [0003] At present, the industrial production of PPS mainly adopts the sodium sulfide method, with N-methylpyrrolidone (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0213C08G75/0263
Inventor 陈培龙王园淦姜春阳胡松华胡唯一余拥黄锋胡泽王强
Owner 重庆晟淦新材料科技有限公司
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