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A kind of method for preparing poly(aryl ether ketone) polymer

A technology of polyaryletherketone and polymer, which is applied in the field of synthesis of aryl etherketone polymer materials, and can solve problems such as shedding, different entrainment output, and increased production costs

Active Publication Date: 2018-07-13
汤原县海瑞特工程塑料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in the production of polyaryletherketone, the nucleophilic substitution method is mainly used to prepare polyaryletherketone polymers. Such polymers are prepared by high-temperature solvent (diphenyl sulfone, sulfolane) polymerization under nitrogen protection. Jilin University (application number: 97101168.0, publication number: CN1162602A), Changchun Jida High-tech Co., Ltd. (application number: 200610016723.6, publication number: CN1844197A application number: 200810050567.4, publication number: CN101245139A), Changchun Jida Special Plastic Engineering Research Co., Ltd. (Application No. 200610016929.9, Publication No.: CN1884331A), Jilin Zhongyan High Performance Engineering Plastics Co., Ltd. (Application No.: 200810000647.9, Publication No.: CN101215365A), Victrex (formerly British ICI Technology), Degussa (formerly Jilin University Technology ), Solvay (India Gada Technology) and other companies have carried out research and production of such products. There is a common problem in the above-mentioned technologies. The reactants (4,4'-difluorobenzophenone, p- Hydroquinone and biphenol) and solvent (diphenyl sulfone) will sublimate, and will deposit on the upper space of the reactor (reactor wall, reactor top, stirring shaft), and will scale on it for a long time. If it is not cleaned up in time, it will fall off into the reaction solution during the next production process, thus affecting the polymerization reaction
[0004] In this regard, Victrex adopts the entrainment method of nitrogen air flow, and at the same time adopts a high-temperature return device to make the material entrained by the air flow return to the reactor to solve this problem. Other companies use small air flow nitrogen protection, and then clean up every 1-3 reactors Reactor is used to solve this problem, but the quality and color of polyaryletherketone materials produced cannot reach the performance of similar foreign products. The main reason is that the molecular weight control point of polymers produced by such nucleophilic substitution reactions lies in The proportioning ratio of the reactants must be strictly controlled. Different nitrogen flow rates will cause different entrained quantities of different reactants, which will cause changes in molecular weight and molecular weight distribution. Although Victrex’s method is carried out by the air flow, it is returned to the high-temperature reflux device. Into the reactor, the proportioning ratio between the reactants is not actually changed, and the method of cleaning the reactor is time-consuming and energy-consuming, which increases the total production cost

Method used

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  • A kind of method for preparing poly(aryl ether ketone) polymer
  • A kind of method for preparing poly(aryl ether ketone) polymer
  • A kind of method for preparing poly(aryl ether ketone) polymer

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Embodiment 1

[0020] First put in 250 kg of diphenyl sulfone, then add 440.6 kg of 4,4'-difluorobenzophenone, 220 kg of hydroquinone, 300 kg of sodium carbonate, and then add 950 kg of diphenyl sulfone to start the membrane temperature machine to start slow heating. When most of the material in the polymerization tank is liquid (the temperature is generally around 140°C), start the stirring governor and adjust the speed at 10 Hz. Open the nitrogen valve of the polymerizer, feed high-purity nitrogen, adjust the nitrogen flow rate to 1.9m3 / h, turn on the induced draft fan, repeat 3 times, remove the oxygen in the polymerizer, and make the slight negative pressure of nitrogen in the system be -0.01 After Mpa, the heating reaction starts, the exhausted nitrogen is cooled by the reflux condenser, and the sublimable diphenyl sulfone entrained in the gas is recovered in liquid form to the heat-conducting oil heat-tracing buffer tank, and each batch is measured to adjust the batching ratio for recyc...

Embodiment 2

[0023] First put in 250 kg of diphenyl sulfone, then add 440.6 kg of 4,4'-difluorobenzophenone, 220 kg of hydroquinone, 300 kg of sodium carbonate, and then add 950 kg of diphenyl sulfone to start the membrane temperature machine to start slow heating. When most of the material in the polymerization tank is liquid (the temperature is generally around 140°C), start the stirring governor and adjust the speed at 10 Hz. Open the nitrogen valve of the polymerizer, feed high-purity nitrogen, adjust the nitrogen flow rate to 1.9m3 / h, turn on the induced draft fan, repeat 3 times, remove the oxygen in the polymerizer, and make the slight negative pressure of nitrogen in the system be -0.02 After Mpa, the heating reaction starts, the exhausted nitrogen is cooled by the reflux condenser, and the sublimable diphenyl sulfone entrained in the gas is recovered in liquid form to the heat-conducting oil heat-tracing buffer tank, and each batch is measured to adjust the batching ratio for recyc...

Embodiment 3

[0026]First put in 250 kg of diphenyl sulfone, then add 440.6 kg of 4,4'-difluorobenzophenone, 220 kg of hydroquinone, 300 kg of sodium carbonate, and then add 950 kg of diphenyl sulfone to start the membrane temperature machine to start slow heating. When most of the material in the polymerization tank is liquid (the temperature is generally around 140°C), start the stirring governor and adjust the speed at 10 Hz. Open the nitrogen valve of the polymerization kettle, feed high-purity nitrogen, adjust the nitrogen flow rate to 1.9m3 / h, turn on the induced draft fan, repeat 3 times, remove the oxygen in the polymerization kettle, and make the slight negative pressure of nitrogen in the system be -0.03 After Mpa, the heating reaction starts, the exhausted nitrogen is cooled by the reflux condenser, and the sublimable diphenyl sulfone entrained in the gas is recovered in liquid form to the heat-conducting oil heat-tracing buffer tank, and each batch is measured to adjust the batch...

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Abstract

The invention provides a method for preparing a polyaryletherketone polymer. The novel method is used for synthesizing polyether-ether-ketone under the condition of high temperature and micro-negative pressure, and the problem that production difficulty is caused by sublimation of reactant and a solvent, and therefore the requirement for producing a high-quality polyaryletherketone polymer can not be met is solved. By adjusting the negative pressure range and gas displacement of a reaction still, increasing the amount of volatile reactant, stabilizing production conditions and strictly controlling production process, polymer molecular weight is controlled. The method can also be used for preparing copolymerization polymers.

Description

Technical field: [0001] The invention discloses a new method for preparing polyaryl ether ketone polymers, which is an improvement to the existing preparation method of polyarylether ketone polymers, and belongs to the field of synthesis of aryl ether ketone polymer materials. Background technique: [0002] With the development of science and technology, people have higher and higher requirements on the heat resistance level of materials, and general engineering plastics can no longer meet the requirements in some high-tech fields. In order to adapt to the development of cutting-edge technology, since the 1960s, the development of high-performance engineering plastics has been very rapid. Polyaryletherketone (PEEK), which was first successfully developed by the British ICI company, is a fully aromatic semi-crystalline polymer with excellent heat resistance, radiation resistance, insulation and aging resistance. The excellent physical and mechanical properties, thermal prope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/40
CPCC08G65/4012
Inventor 姜忠喜谭冠男
Owner 汤原县海瑞特工程塑料有限公司
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