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Method for preparing powdered resin

A powder resin and polymer technology, which is applied in the field of high-performance powder resin preparation, can solve the problems of poor processing effect and high energy consumption, and achieve the effects of improving the workshop environment, saving energy, and saving energy

Inactive Publication Date: 2012-12-05
KINGFA SCI & TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The original resin post-treatment process has the disadvantages of large energy consumption and poor treatment effect

Method used

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  • Method for preparing powdered resin
  • Method for preparing powdered resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 (about 15% solid content)

[0024] Polymerization process:

[0025] In a four-port reaction kettle equipped with a thermometer, a nitrogen pipe, a condensing separator, and an anchor stirrer, first add 50Kg of refined sulfolane, then add 6.67Kg of 4,4'-difluorobenzophenone and 3.303Kg Hydroquinone, when it is completely dissolved and the temperature rises to 80°C, add 3.498Kg (over 2%) Na 2 CO 3 , and then add 2Kg of xylene, stir and heat until the temperature rises to 150°C, the system starts to azeotrope, xylene and water condense in the water separator, the upper layer of xylene is refluxed, and the lower layer of water is continuously released, and the water is recovered to the theoretical When measuring, the xylene in the upper layer starts to be clear and transparent, and then continues to reflux for 20 minutes, and then starts to distill the xylene from the system. Continue to increase the viscosity. After 1.5 hours, stop the reaction after the visc...

Embodiment 2

[0029] Embodiment 2 (solid content about 30%)

[0030] Polymerization process:

[0031] In a four-port reaction kettle equipped with a thermometer, a nitrogen pipe, a condensing separator, and a paddle stirrer, first add 20Kg of refined sulfolane, and then add 6.67Kg of 4,4'-difluorobenzophenone and 3.303Kg Hydroquinone (available polymer 8.64Kg, solid content about 30%), when it is completely dissolved and the temperature rises to 80°C, add 3.498g (excess 2%) Na 2 CO 3 , then continue to heat up, add 2Kg of xylene, stir and heat, until the temperature rises to 150 ° C, the system starts to azeotrope, xylene and water condense in the water separator, the upper layer of xylene is refluxed, and the lower layer of water is continuously released. When the water is recovered to the theoretical amount, the xylene in the upper layer becomes clear and transparent, and the reflux continues for 20 minutes, and then the xylene starts to be evaporated from the system. The viscosity inc...

Embodiment 3

[0035] Example 3 (about 15% solid content) Polymerization process:

[0036] In a four-port reaction kettle equipped with a thermometer, a nitrogen pipe, a condensing water separator, and a propeller stirrer, first add 50Kg of refined sulfolane, then add 6.67Kg of 4,4'-difluorobenzophenone and 3.303Kg Hydroquinone (available polymer 8.64Kg, solid content about 15%), when it is completely dissolved and the temperature rises to 80°C, add 3.498Kg (excess 2%) Na 2 CO 3 , then continue to heat up, add 2Kg of xylene, stir and heat, until the temperature rises to 150 ° C, the system starts to azeotrope, xylene and water condense in the water separator, the upper layer of xylene is refluxed, and the lower layer of water is continuously released. When the water is recovered to the theoretical amount, the xylene in the upper layer becomes clear and transparent, and the reflux continues for 20 minutes, and then the xylene starts to be evaporated from the system. The polymerization react...

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Abstract

The invention provides a method for preparing powdered resin, the steps of which include: (1) After the polymerization reaction is completed, the temperature is directly lowered so that the polymer is precipitated from the reaction system and becomes a polymer colloidal liquid; the cooling rate is 2-50°C / min, the cooling time is 1~60min; increase the stirring to prevent agglomeration during the process, and the stirring speed is 10~3000 rpm; (2) When the system cools down to 130~250℃, add a certain amount of bad Solvent, so that the polymerization product system and poor solvent form a suspension liquid mixture; (3) Remove the mother liquor from the suspension polymer by centrifugation, filtration or leaching, and filter and separate to obtain the required crude product of the polymer; (4) Use a solvent Or boiling water to extract and refine the salt and impurities in the polymer several times at high temperature, and dry to obtain the product. The advantages of this treatment method are: the polymer powder with uniform size can be obtained through process control; the rapid discharge can be realized to avoid the change of resin viscosity during the discharge process; the problem of sticky material on the wall of the reactor can be solved, and the production efficiency can be improved.

Description

technical field [0001] The invention relates to a method for preparing powdered resin, in particular to a method for preparing high-performance powdered resin. Background technique [0002] Many resins such as polyaryletherketone resins have the advantages of high temperature resistance, high strength, and radiation resistance. Because the polymerization reaction temperature is often above 300 ° C, high-temperature solvents such as diphenyl sulfone are required, and other solvents cannot adapt. No matter what kind of solvent is used for synthesis, after the polycondensation reaction, the reaction product needs to be washed and separated to remove the reaction solvent, inorganic salts, residual monomers and other compounds. Among them, the most difficult to remove are alkali metal halides and alkaline earth metal halides. High levels of by-products or solvents remaining in the polymer can lead to technical disadvantages in the final product in forming various extrusion mold...

Claims

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Application Information

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IPC IPC(8): C08G65/46C08G75/20
CPCC08J3/14C08F6/06C08G65/46C08J2371/10C08J2381/06
Inventor 饶先花曹民代惊奇苏成晓赵东辉曾祥斌宁凯军蔡彤旻
Owner KINGFA SCI & TECH CO LTD
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