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Semi-continuous preparation process for block PEKK (polyetherketoneketone)

A polyetherketoneketone, semi-continuous technology, applied in the field of polymer synthesis, can solve the problems of destroying the feeding ratio, difficult collision of active end groups, difficult handling, etc. Effect

Inactive Publication Date: 2018-04-06
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) It is difficult for the reactor to handle the high-viscosity material system, so that the material in the gel state cannot be stirred in the late stage of the reaction, resulting in a reduced polymerization time and because the active end group is difficult to collide, it is difficult to prepare higher molecular weight polyether ketone ketone Polymer (general intrinsic viscosity is less than 1.0dL / g), and this has just limited the application of prepared polyether ketone ketone polymer;
[0007] (2) The production cycle is long, and the equipment efficiency is low. When adopting the reactor semi-continuous process to produce polyether ketone ketone, because the material in the gel state is difficult to handle, it takes a long time to process the reaction material after the reaction ends. As a result, its production cycle is as long as 6-20h;
[0008] (3) The polymerization reactor needs to be cleaned frequently. Every time the reactor synthesizes a batch of polyether ketone ketone, a layer of sticky material will be covered on the surface of the polymerization reactor. After two or three times, the thickness can reach 1cm. On the one hand, it seriously affects the reactor. On the other hand, because the existence of residual materials destroys the feeding ratio of the next batch of materials, it is necessary to frequently clean the polymerization reactor during the industrial production of polyether ketone ketone, which seriously affects the production efficiency;
[0009] (4) The current industrial production is a batch production process, and its production automation is low

Method used

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  • Semi-continuous preparation process for block PEKK (polyetherketoneketone)
  • Semi-continuous preparation process for block PEKK (polyetherketoneketone)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Semi-continuous method prepares the technique of block polyether ketone ketone, and the steps are as follows:

[0050] (1) Add 350kg of dichloromethane to the prepolymerization kettle A, cool down to -15°C, then add 147kg of anhydrous aluminum chloride and 35kg of dimethylformamide to the prepolymerization kettle in batches for reaction to obtain a reaction solution A;

[0051] (2) Add 150kg of dichloromethane to the prepolymerization kettle B, cool down to -15°C, then add 63kg of anhydrous aluminum chloride and 15kg of dimethylformamide to the prepolymerization kettle in batches for reaction to obtain a reaction solution B;

[0052] (3) 42.63kg of terephthaloyl chloride and 35.74kg of diphenyl ether are added to the mixing kettle A, then 42kg of dichloromethane is added for dissolving, and mixed solution A is obtained after mixing;

[0053] (4) 18.27kg of isophthaloyl chloride, 15.32kg of diphenyl ether are added in the mixing kettle B, then 18kg of dichloromethane i...

Embodiment 2

[0057] Semi-continuous method prepares the technique of block polyether ketone ketone, and the steps are as follows:

[0058] (1) Add 300kg of dichloromethane to the prepolymerization kettle A, cool down to -15°C, then add 126kg of anhydrous aluminum chloride and 30kg of dimethylformamide to the prepolymerization kettle in batches for reaction to obtain a reaction solution A;

[0059] (2) Add 200kg of dichloromethane to the prepolymerization kettle B, cool down to -15°C, then add 84kg of anhydrous aluminum chloride and 20kg of dimethylformamide to the prepolymerization kettle in batches for reaction to obtain a reaction solution B;

[0060] (3) 36.54kg of terephthaloyl chloride and 30.62kg of diphenyl ether are added to the mixing kettle A, then 36kg of dichloromethane is added for dissolving, and mixed solution A is obtained after mixing;

[0061] (4) 26.36kg of isophthaloyl chloride, 20.42kg of diphenyl ether are added in the mixing kettle B, then 24kg of dichloromethane i...

Embodiment 3

[0065] Semi-continuous method prepares the technique of block polyether ketone ketone, and the steps are as follows:

[0066] (1) Add 250kg of dichloromethane to the prepolymerization kettle A, lower the temperature to -15°C, then add 105kg of anhydrous aluminum chloride and 25kg of dimethylformamide to the prepolymerization kettle in batches for reaction to obtain a reaction solution A;

[0067] (2) Add 250kg of dichloromethane to the prepolymerization kettle B, lower the temperature to -15°C, then add 105kg of anhydrous aluminum chloride and 25kg of dimethylformamide to the prepolymerization kettle in batches for reaction to obtain a reaction solution B;

[0068] (3) 30.45kg of terephthaloyl chloride and 25.53kg of diphenyl ether are added to the mixing kettle A, then 30kg of dichloromethane is added for dissolving, and mixed solution A is obtained after mixing;

[0069] (4) 30.45kg of isophthaloyl chloride, 25.53kg of diphenyl ether are added in the mixing kettle B, then ...

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Abstract

The invention belongs to the technical field of polymer synthesis and particularly relates to a semi-continuous preparation process for block PEKK (polyetherketoneketone). A solvent, a Lewis acid anda Lewis base are added to two prepolymerization reactors respectively; diphenyl ether and isophthaloyl dichloride or terephthaloyl chloride are added in equal molar ratio for reactions, and a prepolymer A and a prepolymer B which have better flowability are formed; then the prepolymer A and the prepolymer B which have better flowability as well as residual diphenyl ether are quantitatively added to a twin-screw reactor by a feeder, the materials are mixed under the strong shear action of the twin-screw reactor, the probability of collision of active end groups is increased, the polymerizationreaction rate is increased, and PEKK with high intrinsic viscosity is prepared within short time.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a process for preparing block polyether ketone ketone by a semi-continuous method. Background technique [0002] Polyether ketone ketone (PEKK) resin is a special engineering plastic with excellent performance, which belongs to a kind of polyarylether ketone. The chemical bond characteristics make it have excellent mechanical properties, radiation resistance, high temperature resistance, chemical corrosion resistance, good electrical insulation and flame retardancy, and can be processed by extrusion, injection molding, molding and other processing methods. It has extremely high application requirements in aerospace, electrical and electronic, automotive and petroleum. [0003] [0004] The synthesis method of polyether ketone ketone reported in the literature is different from the synthesis method of polyether ether ketone by nucleophilic substitution, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40
CPCC08G65/405C08G2650/40
Inventor 孙庆民李光辉马团芝贾远超黄桂青韩楠楠
Owner SHANDONG KAISHENG NEW MATERIALS
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