Phthalonitrile-terminated polyaryletherketone resin and preparation method thereof

A technology of phthalonitrile and polyaryletherketone, applied in the field of phthalonitrile-terminated polyaryletherketone resin and its preparation, polyaryletherketone resin and its preparation field, can solve the problem of glass transition temperature Sufficiently high, increasing difficulty in processing, low glass transition temperature, etc., to achieve the effect of increasing solubility, improving glass transition temperature and mechanical strength, and lowering melting point

Inactive Publication Date: 2017-07-14
深圳市源沣石油化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Traditional polyaryletherketone is a kind of semi-crystalline linear polymer, although it has good processability, it has a high melting point, so the energy consumption in its processing is relatively large
In addition, the glass transition temperature (Tg) of polyaryletherketone is not high enough, and the modulus drops significantly when it is applied above the glass transition temperature. At high temperatures, the fluidity has little dependence on temperature, resulting in a lower use temperature.
[0004] In order to further increase the use temperature of polyaryletherketone materials, people introduce a rigid structure into the polyaryletherketone main chain to increase the rigidity of polyaryletherketone to increase the glass transition temperature (T g ), and ultimately to increase the use temperature of the material, but the increase in the glass transition temperature will inevitably lead to a continuous increase in its melting point, which brings more and more difficulties to processing
[0005] The Chinese patent application with the application number 201510869420.8 discloses an industrial synthesis method of end-capping modified polyaryletherketone resin. The end-capping agent is 3,4'-difluorobenzophenone, 3-chloro-4-fluorodi A mixture of one or more of benzophenone, 3-fluoro-4-chlorobenzophenone and 3,4'-dichlorobenzophenone can maintain the melting point at a low level, but its vitrification The transition temperature is still low, resulting in a lower service temperature, and its mechanical strength is also low

Method used

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  • Phthalonitrile-terminated polyaryletherketone resin and preparation method thereof

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preparation example Construction

[0043] The preparation method of the phthalonitrile-terminated polyaryl ether ketone resin of the present invention includes the following steps:

[0044] (1) Synthesis of hydroxyl terminated polyaryl ether ketone

[0045] a1. Mix sulfolane and dehydrating agent with a molar ratio of 5-6:1 to 1.29, pass in inert gas protection, mix well, and heat to 80-120℃;

[0046] a2. After the sulfolane is dissolved, add the dihydric phenol. After the dihydric phenol monomer is dissolved, add the catalyst. The temperature is raised to 150-180°C and refluxed for 1.5-2.5h, and then the dihalobenzophenone is added. Hydroquinone and bisphenol S;

[0047] a3. After refluxing at 180~220℃ for 1.5~2.5h, the dehydrating agent and the generated water will be released, and the temperature will be raised to 220~280℃ for 2~4h, then the polymerization reaction will be finished, and the volume of the hydroxyl-terminated polyaryletherketone solution will be V 1 ;

[0048] Among them, the solid content of the react...

Embodiment 1

[0067] Using 4,4-difluorobenzophenone, biphenol and bisphenol S as raw materials, anhydrous potassium carbonate as a catalyst, and xylene as a dehydrating agent. According to the molar ratio: 4,4-difluorobenzophenone: biphenol: bisphenol S: catalyst=1: 0.75: 0.3: 1.4 to weigh the above raw materials;

[0068] After weighing, add sulfolane and dehydrating agent to the reactor, pass in inert gas protection, turn on the screw-belt screw stirring paddle, stir at 80r / min, heat the reactor to 100℃, and wait until the sulfolane is completely dissolved. Add biphenol and bisphenol S, add the catalyst after the monomer is dissolved, raise the temperature to 160℃ and reflux for 2.5h to make the dihydric phenol form a phenol form, and then add 4,4-difluorobenzophenone to the reaction In the container, the solid content of the reaction system is made 20%; after refluxing reaction at 200°C for 2.5 hours, dehydrating agent and water are released, and then the temperature of the reactor is raise...

Embodiment 2

[0071] Refer to Example 1 for the specific method, and the difference from Example 1 is only: according to the molar ratio: 4,4-difluorobenzophenone: dihydroxybenzene: bisphenol S: catalyst=1:0.55:0.5:1.4; The solid content of the reaction system is 25%. The performance parameters of the obtained phthalonitrile-terminated polyaryl ether ketone resin are shown in Table 1, and the infrared spectrum is shown in figure 1 .

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Abstract

The invention relates to a polyaryletherketone resin and a preparation method thereof, particularly a phthalonitrile-terminated polyaryletherketone resin and a preparation method thereof, belonging to the technical field of high-molecular materials. The invention provides a polyaryletherketone resin of which the structure is disclosed in the specification. In the structural formula of the phthalonitrile terminated polyaryletherketone resin, m+n=1, 0<m<1, and 0<n<1. The invention also provides a preparation method of the phthalonitrile-terminated polyaryletherketone resin. The method comprises the steps of (1) synthesis of hydroxyl-terminated polyaryletherketone and (2) synthesis of phthalonitrile-terminated polyaryletherketone. Bisphenol S is introduced to the main chain of the polyaryletherketones, and a crosslinking group bis-phthalonitrile is introduced to the chain end, thereby obtaining the crosslinking function on the premise of facilitating the processing due to the decrease of the melting point of the polyaryletherketones; and thus, the crosslinked polyaryletherketones can obtain the application temperature of a thermosetting engineering material by a thermoplastic engineering material processing technique, thereby opening up a new way for application of polyaryletherketones in the field of high temperature resistance.

Description

Technical field [0001] The invention relates to a polyaryletherketone resin and a preparation method thereof, in particular to a phthalonitrile-terminated polyaryletherketone resin and a preparation method thereof, and belongs to the technical field of polymer materials. Background technique [0002] As a new type of semi-crystalline aromatic special engineering plastic, polyaryl ether ketone has excellent high temperature resistance, corrosion resistance, radiation resistance, flame retardancy, high mechanical properties, excellent dimensional stability and excellent electrical properties. In many special fields, it can replace traditional materials such as metals and ceramics, and has made outstanding contributions in reducing quality and improving performance. It has become one of the most popular high-performance special engineering plastics today. [0003] Traditional polyaryl ether ketone is a kind of semi-crystalline linear polymer. Although it has good processing properties...

Claims

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Application Information

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IPC IPC(8): C08G65/40
CPCC08G75/23
Inventor 钟家春
Owner 深圳市源沣石油化工有限公司
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