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Preparation method of catalyst and preparation method of chlorine-containing unsaturated polyester

An unsaturated and catalyst technology, applied in the field of preparation of chlorine-containing unsaturated polyester, can solve problems such as no practical use value, and achieve the problem of solving solid waste in production lines, shortening reaction time, and improving flame retardancy and heat resistance. Effect

Active Publication Date: 2022-04-15
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has no practical value and can only be treated as solid waste.

Method used

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  • Preparation method of catalyst and preparation method of chlorine-containing unsaturated polyester
  • Preparation method of catalyst and preparation method of chlorine-containing unsaturated polyester
  • Preparation method of catalyst and preparation method of chlorine-containing unsaturated polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Catalyst preparation:

[0050] Add 21.8g of pyrophthalic anhydride, 16.66g of isophorone diamine and 346g of DMAC into a 2000ml three-necked flask, start stirring, stir and dissolve until the viscosity no longer increases, and obtain a polyamic acid solution; add 0.77g to the solution sebacic acid and 2.31g of N-phenyl-N'-phenylbisphthalimide with formula A structure, continue to stir until dissolved, add 0.04g of acetic anhydride, 0.04g of pyridine, and continue to stir for 3h to prepare polyimide solution. The polyimide solution was mixed with 1038g of water and pulverized with a wet pulverizer, and the obtained solid was filtered and washed with boiling water 4 times, each time with 308g of water. The solid obtained after washing was dried in absolute vacuum at 140° C. for 24 hours to prepare catalyst a.

[0051] Resin preparation:

[0052] Connect a condenser, a water separator and an agitator to a 1000ml three-necked flask, add 100g of chlorinated o-xylene gas-p...

Embodiment 2

[0056] Catalyst preparation:

[0057] Add 29.4g of biphenyl dianhydride, 16.83g of isophorone diamine, and 262g of DMF into a 2000ml three-necked flask, start stirring, stir and dissolve until the viscosity no longer increases, and obtain a polyamic acid solution; add 1.85g to the solution Dodecanedioic acid and 9.25g of N-phenyl-N'-phenylbisphthalimide of the formula B structure, continue to stir until dissolved, add 0.09g of acetic anhydride, 0.09g of pyridine, continue to stir for 3h, Prepare polyimide solution. The polyimide solution was mixed with 1048g of water and pulverized with a wet pulverizer, and the obtained solid was filtered and washed with boiling water 4 times, each time with 462g of water. The solid obtained after washing was dried in absolute vacuum at 145° C. for 24 hours to prepare catalyst b.

[0058] Resin preparation:

[0059] Connect a condenser, a water separator and an agitator to a 1000ml three-necked flask, add 100g of chlorinated o-xylene gas-p...

Embodiment 3

[0063] Catalyst preparation:

[0064] Add 32.2g of benzophenone dianhydride, 11.286g of 1,4-cyclohexanediamine and 174g of NMP into a 2000ml three-necked flask, start stirring, stir and dissolve until the viscosity no longer increases, and obtain a polyamic acid solution; add 2.61g of dodecanedioic acid and 20.87g of N-phenyl-N'-phenylbisphthalimide with formula A structure, continue to stir until dissolved, add 0.13g of acetic anhydride, 0.13g of pyridine, and continue to stir 3h, made of polyimide solution. The polyimide solution was mixed with 1739g of water and pulverized with a wet pulverizer, and the obtained solid was filtered and washed four times with 522g of water each time. The solid obtained after washing was dried in absolute vacuum at 150° C. for 24 hours to obtain catalyst c.

[0065] Resin preparation:

[0066] Connect the condenser tube, water separator and stirrer on the 1000ml three-necked flask, add 100g of chlorinated o-xylene gas-phase oxidation by-pro...

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Abstract

The invention discloses a preparation method of a catalyst and a preparation method of chlorine-containing unsaturated polyester. The preparation method of the catalyst comprises the following steps: carrying out imidization process on acetic anhydride and organic alkali by using a solution compounded from polyamide acid, solid acid and a biphthalimide monomer, crushing in a water-phase solution by using a wet crusher, washing, and carrying out vacuum drying to prepare the porous structure catalyst of the polyimide carrier. The preparation method of the chlorine-containing unsaturated polyester comprises the following steps: carrying out reflux dehydration on a chloro-o-xylene gas-phase oxidation byproduct and dihydric alcohol in a solvent, and adding a catalyst to prepare an unsaturated polyester solution; and after dehydration is finished, cooling the solution, adding activated carbon for decoloration, filtering, and evaporating out the solvent to obtain the unsaturated polyester. The application problem of by-products can be effectively solved, and the problem of solid waste of a production line is solved. The flame retardance and the heat resistance of the cured unsaturated polyester resin are improved.

Description

technical field [0001] The invention relates to polyester, in particular to a catalyst for chlorine-containing unsaturated polyester and a method thereof, and a preparation method for chlorine-containing unsaturated polyester. Background technique [0002] Chlorinated phthalic anhydride is a very important solid monomer for the synthesis of polyimide. Chlorinated phthalic anhydride can be used to synthesize biphenyl dianhydride, benzophenone dianhydride, diphenyl ether dianhydride, triphenylene dianhydride, diphenyl sulfide Ether dianhydride, bisphenol A diether dianhydride, bischlorobisphthalimide and other monomers can be used to synthesize polyimides of various structures. [0003] The current mainstream chlorinated phthalic anhydride synthesis method is mainly through chlorination and purification of o-xylene to prepare 3(4)-mixed chlorinated o-xylene (the ratio is roughly 45:55), and then the mixed chlorinated o-xylene is passed through Chlorophthalic acid is prepared ...

Claims

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Application Information

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IPC IPC(8): C08G63/87C08G63/682C08G63/81
Inventor 张鑫曾伟王磊黎源
Owner WANHUA CHEM GRP CO LTD
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