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A kind of post-processing method of soluble nitrogen-containing polyarylene ether resin

A polyarylene ether, soluble technology, applied in the field of polymer post-processing, can solve the problems of poor transparency and low modulus

Active Publication Date: 2020-04-21
芜湖万隆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the existing post-processing method for preparing nitrogen-containing polyarylether resins. There are still a certain amount of low-molecular-weight polymers and cyclic oligomers in the products, resulting in poor transparency and modulus of products. low problem, and provide a post-treatment method for soluble nitrogen-containing polyarylether resin

Method used

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  • A kind of post-processing method of soluble nitrogen-containing polyarylene ether resin
  • A kind of post-processing method of soluble nitrogen-containing polyarylene ether resin
  • A kind of post-processing method of soluble nitrogen-containing polyarylene ether resin

Examples

Experimental program
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Effect test

Embodiment 1

[0066]

[0067] Among them, n=0.7, m=0.3.

[0068] The phenolphthalein polyarylether nitrile ketone solution (theoretical output 36g) prepared by polycondensation reaction need not carry out desalting step, add 700g DMF and dilute to solid content 4.9%, mechanical stirring obtains homogeneous solution, slowly drips the mixed solution of water, methanol (water The mass ratio to methanol is 1:4) 100g, the solution gradually turns white until a small amount of precipitate precipitates out, after solid-liquid separation, the jelly is heated to 40°C, re-dissolved with 10g DMF, again in 50g water and acetic acid Precipitate in the precipitant (mass ratio of water and acetic acid 1:1), boil 5-7 times, and dry to obtain 2.9g of polymer. The number average molecular weight is 74kDa and the molecular weight distribution is 2.50.

[0069] Experimental results show that: the polymer obtained by the above post-treatment is a cross-linked component, which has poor solubility in DMF, DMAc, ...

Embodiment 2

[0072] The solution after the solid-liquid separation of Example 1 continues to slowly drip water, the mixed solution of ethanol (the mass ratio of water and ethanol is 1:4) 10g, a large amount of precipitation occurs in the solution, after the solid-liquid separation, dissolve with 270g DMF again, will The solution was heated to 40°C, precipitated again in a precipitant of 1000g water and acetic acid (the mass ratio of water and acetic acid was 1:1), boiled in water for 5-7 times, and dried to obtain 30.2g of polymer.

[0073] Experimental results show that: the above post-treatment has obtained a linear high molecular weight polymer, which has better solubility in DMF, DMAc, and DMSO after vacuum drying (at room temperature, the solubility in DMF solvent is greater than 0.5g / ml). The number average molecular weight of the polymkeric substance obtained is 196.9kDa, molecular weight distribution 1.36; GPC curve such as figure 2 shown. The appearance of the film prepared by t...

Embodiment 3

[0075]

[0076] Accurately weigh 3.0 g of carbazole-type polyaryletherketone resin, dissolve it in 71 g of chloroform solution with a solid content of 4.05%, stir it mechanically, and after the dissolution is complete, add 18 ml of methanol into it in 3 times (6 mL each time) , the solution gradually turns white until a large amount of precipitates are separated out. After the solid-liquid separation, the jelly is heated to 80°C, dissolved with 20g DMAc again, and precipitated in 50g water again. After drying, the obtained polymer 2.6g , with a number average molecular weight of 65kDa and a molecular weight distribution of 2.15.

[0077] Experimental results show that: the above post-treatment has obtained a linear high molecular weight polymer, which has good solubility in chloroform and tetrahydrofuran after vacuum drying (at room temperature, the solubility in chloroform solvent is greater than 0.5g / ml). The appearance of the film prepared by solution casting method is c...

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Abstract

The invention provides an aftertreatment method for soluble nitrogen-containing polyarylether resin and belongs to the technical field of polymer aftertreatment methods. The aftertreatment method comprises the following steps: diluting soluble nitrogen-containing polyarylether resin powder or polymer solution obtained through polymerization reaction by adopting a good solvent, uniformly stirring to obtain nitrogen-containing polyarylether dilute solution, then adding a poor solvent, carrying out one-step or two-step separation to obtain a product after solid-liquid separation, dissolving solidin the product into the good solvent, then adding a precipitating agent, and carrying out precipitation, so that the treated soluble nitrogen-containing polyarylether resin is obtained. The aftertreatment method provided by the invention has the advantages that the treated polymer has better solubility, molecular weight distribution becomes narrow, the treated polymer is applicable to preparationof thin film materials, the obtained polymer can be used as a special injection, mould pressing and extrusion material for preparing plates and the thin film materials, tensile property and transparency of a thin film are improved, and elongation at break can be improved to 150% from 4-8% of the original resin.

Description

technical field [0001] The invention belongs to the technical field of post-treatment methods for polymers, and in particular relates to a post-treatment method for soluble nitrogen-containing polyarylether resins. Background technique [0002] Polyarylether resin is a high temperature resistant polymer with good heat resistance, high strength and high modulus, but its Tg is often relatively low. For this reason, those skilled in the art will consider modifying the polymer by introducing monomers containing nitrogen atoms to increase the rigidity of the main chain and improve the heat resistance. Because the elongation at break of nitrogen-containing polyarylether resin is lower, its application is affected. The topological structure, molecular weight and molecular weight distribution of nitrogen-containing polyarylether resins are important parameters of polymer structure, and it is an important factor affecting the physical properties of polymers. Polyarylether resin mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/46
CPCC08G65/46
Inventor 周光远王志鹏王红华张兴迪
Owner 芜湖万隆新材料有限公司