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Polyaryletherketone resin and synthesis method thereof

A polyaryletherketone and compound technology, applied in the field of polymer materials, can solve the problems of inability to obtain high molecular weight polymers, inaccurate polymerization reaction ratio, etc., and achieve the effects of improving mechanical properties, shortening reaction time, and improving crystallinity

Active Publication Date: 2021-09-21
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to reduce the influence of the capping agent, try to increase the molecular weight of the capping agent (ZL201110148146.7), but it is still a small molecule capping agent, even if it is difficult to dissolve in the purified organic solvent, but in more than ten tons of boiling organic solvent Under the action of the solvent, it will still be introduced into the next reaction, and for the binary polycondensation reaction, the material ratio has an important influence on the molecular weight, and the capped monomer entering the recovery solvent will cause the polymerization ratio to be inaccurate and cannot be obtained. High-molecular-weight polymers ["Polymer Chemistry", Pan Zuren, Chemical Industry Press; CN200980142463.9], so suitable reactive end-capping agents have always been a technical difficulty in this field

Method used

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  • Polyaryletherketone resin and synthesis method thereof
  • Polyaryletherketone resin and synthesis method thereof
  • Polyaryletherketone resin and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Embodiment 1: Utilize the specific embodiment of polyaryletherketone resin synthesized by end-capping of oligomer

[0056] 1.1 The preparation of the capping agent is as follows:

[0057] Add 4.0 kg of diphenyl sulfone to a reaction kettle protected by inert gas, melt it to 160°C, add 1.3083 kg of 4,4'-difluorobenzophenone, and 0.636 kg of sodium carbonate, heat it to 160°C, add terephthalate 0.5505 kg of phenol. The temperature of the reaction system was raised to 210°C for 2 hours, 250°C for 1 hour, and 305°C for 1 hour.

[0058] According to the binary polycondensation theory and infrared characterization, the synthesized structure is as follows:

[0059]

[0060] 1.2 Synthesis of polyaryletherketone resin

[0061] Diphenylsulfone (672 kg) was added to the kettle. Reduced pressure and evacuated to 0.2 MPa, and fed nitrogen to normal pressure. Under nitrogen protection, heat to 160°C. Then add 127.2 kilograms of sodium carbonate, 218.050 kilograms of 4,4'-dif...

Embodiment 2

[0062] Embodiment 2: Specific examples of synthesis of unblocked polyaryletherketone resin

[0063] Diphenylsulfone (672 kg) was added to the kettle. Reduced pressure and evacuated to 0.2 MPa, and fed nitrogen to normal pressure. Under nitrogen protection, heat to 160°C. Add 127.2 kilograms of sodium carbonate, 219.140 kilograms of 4'-difluorobenzophenone and 110.110 kilograms of hydroquinones again. The reaction kettle was heated to 220°C for 2 hours, 250°C for 1 hour, 290°C for 1 hour, and 310°C for 3 hours. The polymer is cooled, pulverized, extracted with ethanol or acetone to constant weight, extracted with distilled water to constant weight, and dried. The materials were analyzed for intrinsic viscosity, differential thermal scanner (DSC), and thermogravimetric loss (TGA) and tensile properties. Its thermal and mechanical properties compared with the blocked polyaryletherketone resin are as follows: figure 1 , figure 2 and image 3 shown.

Embodiment 3

[0064] Embodiment 3: Utilize the specific embodiment of polyaryletherketone resin synthesized by end-capping of oligomer

[0065] The synthesis of polyaryletherketone resin is the same as in Example 1, except that the end-capping agent is different. The product analysis results are shown in Table 1.

[0066] The preparation method of end-capping agent is:

[0067] Add 4 kg of diphenyl sulfone to a reactor protected by inert gas, melt it to 160°C, add 1.5264 kg of 4,4'-difluorobenzophenone, and 0.636 kg of sodium carbonate, heat it to 160°C, add terephthalate 0.5505 kg of phenol. The temperature of the reaction system was raised to 210°C for 2 hours, 250°C for 1 hour, and 305°C for 1 hour.

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Abstract

The invention discloses a synthesis method of polyaryletherketone resin, which belongs to the technical field of high polymer materials, and particularly relates to a preparation method of special engineering plastic polyaryletherketone resin. The oligomer with the same repeating unit as the polyaryletherketone is used as the end-capping reagent, and the end-capping reagent cannot run off and enter a solvent recovery system, so that the next polymerization reaction cannot be influenced. And the added oligomer does not influence the thermal stability of the material, and the crystallization property of the polymer is slightly improved, so that the mechanical property of the polymer is slightly improved. The addition of the end-capping reagent is easy to control the polymerization reaction, and under the condition of accurate absolute ratio, the polymerization reaction speed is high, the energy consumption is saved, and the method can be widely applied to industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to special engineering plastic polyaryletherketone resin and its preparation method and application. Background technique [0002] In the 1980s, after ICI company announced the preparation method of polyether ether ketone resin, polyarylether ketone series products were successively developed, including polyether ketone, polyether ketone ketone, polyetherether ketone ketone, polyetherether ketone ether ketone A series of products such as ketones. Polyaryletherketone high-performance polymers are widely used in the fields of electronic appliances, mechanical instruments, transportation and aerospace due to their excellent physical and mechanical properties, thermal properties, electrical properties and chemical properties. [0003] Polyaryletherketone resin is generally carried out by nucleophilic polycondensation reaction, and the polymerization temperature ex...

Claims

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Application Information

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IPC IPC(8): C08G65/48
CPCC08G65/48
Inventor 岳喜贵牟建新张海博姜振华庞金辉
Owner JILIN UNIV
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