A kind of process for preparing cyano polyaryletherketone resin

A technology of cyanopolyarylether and process method, which is applied in the field of polymer materials, can solve problems such as high requirements for stirring equipment, adverse effects, and wide molecular weight distribution of products, so as to avoid wide molecular weight distribution, reduce the load of stirring motor, Guaranteed purity and performance

Active Publication Date: 2017-06-30
中昊黑元化工研究设计院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patented technology uses flash evaporation technology to recover solvent and promote product powderization, which solves the problem that polymer products need to be pulverized, and reduces the energy consumption of solvent recovery. However, this technology still has the following four shortcomings in the actual operation process: First, The requirements for stirring equipment are very high, and the stirring resistance will increase exponentially during the solvent volatilization process, which is prone to the phenomenon of motor stalling; second, after the flash evaporation is completed, due to the high temperature in the process, the remaining organic impurities in the polymer are difficult to carbonize or oxidize. It is washed away by organic solvents such as acetone; the third is that it is difficult for the polymer to become a uniform powder, and the existence of larger granular products affects the later purification, which in turn affects the purity and molecular weight distribution of the polymer; the fourth is that when N-methylpyrrole is used When alkane is used as a solvent, it will have adverse effects on the reaction: (1) The boiling point of N-methylpyrrolidone is 203 ° C, and the polymerization temperature is low under normal pressure, and part of the crystallization is prone to occur during the polymerization of cyanopolyaryletherketone resin, resulting in the molecular weight of the product. The distribution is wide; (2) As N-methylpyrrolidone will appear in the high temperature environment of potassium carbonate, the color will deepen, resulting in the product color deepening

Method used

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  • A kind of process for preparing cyano polyaryletherketone resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Taking a 100L polymerization kettle as an example, prepare raw materials according to the following quality: 2,6-dichlorocyanobenzene (6.88Kg), 4,4-dihydroxybenzophenone (8.56Kg), potassium carbonate (1.1Kg), Sodium carbonate (3.45Kg), diphenyl sulfone (38.6Kg), trimethylbenzene (7.8Kg).

[0026] Accurately weigh the above formula components respectively, add diphenyl sulfone and trimethylbenzene into a 100L polymerization kettle equipped with a water separator, agitator (frame-type paddle-type two-way stirring) and a heating device, and pass in an inert gas nitrogen protection , start stirring, frame stirring 30r / min, paddle stirring 60r / min, the jacket of the reactor is heated to 140°C, after 40 minutes all diphenyl sulfone is dissolved, and 2,6-dichlorocyanobenzene and 4, For 4-dihydroxybenzophenone, continue to stir for 10 minutes to dissolve the monomer, then add catalyst potassium carbonate and sodium carbonate mixed salt, raise the temperature of the jacket of th...

Embodiment 2

[0032] Refer to Example 1 for the specific method. The only difference from Example 1 is that the reflux reaction time is extended by 30 minutes, and the polymerization reaction is extended by 30 minutes; the properties of the obtained polyether ether ketone resin are shown in Table 1.

Embodiment 3

[0034] Refer to Example 1 for the specific method, and the difference from Example 1 is only that the reflux reaction time is shortened by 30 minutes, and the polymerization reaction is shortened by 30 minutes; the properties of the obtained polyether ether ketone resin are shown in Table 1.

[0035] Table 1 Properties of cyanopolyaryletherketone resin

[0036]

[0037]It can be seen from the above examples that with the appropriate prolongation of the reflux reaction and polymerization reaction time, the molecular weight of the polyaryletherketone resin increases, which increases its mechanical properties and deteriorates its processing fluidity. The purification effect of the same post-treatment method is slightly On the contrary, the reflux reaction time and polymerization reaction time are appropriately shortened. Although the mechanical properties are slightly reduced, the processing fluidity and purification effect are increased.

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Abstract

The invention discloses a process method for preparing cyano polyetherketoneketone resin. According to the process method, dihalogenation benzonitrile and 4, 4-dihydroxy benaophenonel serve as raw materials, diphenyl sulfone serves as solvent, a reaction is conducted for 2-3 hours at the temperature of 295-320 DEG C under the action of the catalysts and a dehydrating agent in inert atmosphere, after the polymerization reaction is ended, the temperature is lowered to 210-230 DEG C, and trimethylbenzene is added, so that all the cyano polyetherketoneketone resin is crystallized uniformly and separated out, a whole material system forms white slurry which can flow easily under the action of trimethylbenzene, then the organic solvent and deionized water are utilized for conducting washing several times, drying is conducted, and finally the cyano polyetherketoneketone resin is obtained. By means of the method, the cyano polyetherketoneketone resin is separated out naturally in the solvent, meanwhile, the materials are changed into the powder slurry form, material conveying and processing of the next step are facilitated, the problem that product purification and solve recovery are difficult to conduct is solved, meanwhile, macromolecular chains are not destroyed, and the product purity and performance are guaranteed.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular to a preparation method of cyano polyaryletherketone resin. Background technique [0002] Polyether ketone is a high molecular polymer whose main chain is alternately formed by ether bonds and ketone groups. It has excellent high temperature resistance, corrosion resistance, radiation resistance, flame retardancy, balanced physical and mechanical properties and excellent dimensional stability. As well as excellent electrical properties, it can be widely used as a special engineering plastic in the fields of electronics, aerospace, and automobile transportation. The typical polymer in polyetherketone is polyaryletherketone, which can be formed by polycondensation of difluorobenzophenone and aromatic dihydric phenol at high temperature, or by aromatic dihalide and 4,4-dihydroxy-diphenyl It is obtained by polycondensation of ketone. [0003] Invention patent of a cyanopolya...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/40C08G65/46
Inventor 钟家春王家贵聂绪建何平林幽静
Owner 中昊黑元化工研究设计院有限公司
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