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Styrene-hexachlorobutadiene-acrylonitrile ternary copolymerization catalyst and ternary copolymerization method

A technology of acrylonitrile terpolymerization catalyst and hexachlorobutadiene, which is applied in the field of styrene, hexachlorobutadiene and acrylonitrile terpolymerization catalyst and ternary copolymerization to achieve simple post-processing procedure and high copolymer yield. High efficiency, easy washing and separation effect

Inactive Publication Date: 2014-08-20
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the continuous improvement of people's requirements for the performance of ABS resin, relying solely on diene rubber as a toughening agent can no longer meet the demand, and new rubber varieties must be used to produce products with higher performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 20 ml of tetrahydrofuran, 0.03 mol of triisobutylaluminum, and 0.01 mol of butyl lithium to a single-mouthed glass bottle that has been evacuated several times and baked with nitrogen, and keep the temperature in a water bath at 50°C for 15 minutes to obtain aluminum- lithium catalyst.

[0023] Take 0.1 mole of styrene, 0.03 mole of hexachlorobutadiene, 0.03 mole of acrylonitrile, and 20ml of tetrahydrofuran, put them into an autoclave, add 1% catalyst by monomer weight, heat to 80°C, fill with nitrogen and pressurize to 0.3MP, Reacted for 8 hours, stopped heating, after cooling, after removing the pressure, the product was poured into methanol solution containing 5% hydrochloric acid to precipitate styrene, hexachlorobutadiene and acrylonitrile terpolymer, and the precipitate was washed with methanol until Neutral, vacuum-dried, the measured reaction yield was 52.2%.

Embodiment 2

[0025] Add 20 ml of anisole, 0.03 mol of triisobutylaluminum, and 0.02 mol of butyllithium to a one-mouth glass bottle that has been evacuated several times and baked with nitrogen, and keep the temperature in a water bath at 40°C for 15 minutes to obtain Aluminum-lithium catalyst.

[0026] Take 0.1 mole of styrene, 0.03 mole of hexachlorobutadiene, 0.03 mole of acrylonitrile, and 20ml of anisole, put them into an autoclave, add 0.9% catalyst by monomer weight, heat to 90°C, fill with nitrogen and pressurize to 0.5 MP, react for 7 hours, stop heating, after cooling, remove the pressure, pour the product into methanol solution containing 5% hydrochloric acid to precipitate styrene, hexachlorobutadiene and acrylonitrile terpolymer, and the precipitate is washed with methanol Wash until neutral, dry in vacuum, and the measured reaction yield is 57.8%.

Embodiment 3

[0028] Add 20 ml of 1,4-dioxane, 0.03 mole of triisobutylaluminum, and 0.03 mole of butyllithium to a single-mouthed glass bottle that has been evacuated several times and baked with nitrogen, and keep the temperature in a water bath at 45°C. After 15 minutes, the aluminum-lithium catalyst was obtained.

[0029] Take 0.1 mole of styrene, 0.03 mole of hexachlorobutadiene, 0.03 mole of acrylonitrile, and 20ml of 1,4-dioxane, put them into an autoclave, add 0.6% catalyst by monomer weight, heat to 100°C, and fill with nitrogen Pressurize to 0.8MP, react for 6 hours, stop heating, after cooling, remove the pressure, pour the product into methanol solution containing 5% hydrochloric acid to precipitate styrene, hexachlorobutadiene and acrylonitrile terpolymer, The precipitate was washed with methanol until neutral, and dried in vacuum. The reaction yield was measured to be 59.8%.

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PUM

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Abstract

The invention relates to a styrene-hexachlorobutadiene-acrylonitrile ternary copolymerization catalyst and a ternary copolymerization method, and is characterized in that: in a dry simple-aperture glass bottle in an inert gas atmosphere, dissolving triisobutyl aluminium and butyl lithium in a first solvent, sealing the glass bottle mouth with a latex tube, thermostatically placing in a water bath at 40-50 DEG C for 10-20 minutes, and cooling to obtain an aluminum-lithium catalyst; wherein the molar ratio of triisobutyl aluminium to butyl lithium is 1 :3-3 :1; the first solvent is selected from tetrahydrofuran, anisole, 1, 4-dioxane, cyclohexanone or toluene; and the ratio of the use amount of the first solvent to the sum of triisobutyl aluminium and butyl lithium is 20 ml: 0.04 to 0.09 mol. The styrene-hexachlorobutadiene-acrylonitrile ternary copolymerization catalyst has the advantages of simple preparation method, good catalytic activity, high catalytic efficiency, low reaction temperature, and high copolymer yield, the post-processing procedure of the prepared ternary copolymer is simple, and the copolymer product is easy to wash and separate after soaking with methanol.

Description

technical field [0001] The invention relates to a high polymer catalyst and a high polymer synthesis process, specifically a ternary copolymerization catalyst of styrene, hexachlorobutadiene and acrylonitrile and a ternary copolymerization method. Background technique [0002] Acrylonitrile-butadiene-styrene copolymer (ABS), as a thermoplastic engineering plastic, is widely used in various industries due to its excellent mechanical properties, chemical inertness and ease of processing, but ABS is inherently flammable. Defects. The self-charging ability of ABS is very poor, and polyol compound (PER) is usually added as a charring agent, but due to the poor compatibility between PER and ABS, the mechanical properties of flame-retardant ABS are seriously affected. Adding a polymer with a char-forming effect as a carbon source is a commonly used method at present. At present, the relevant research mainly focuses on the improvement of the flame retardancy of materials, but ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F236/18C08F220/44C08F212/12C08F4/52C08F4/48
Inventor 房江华胡敏杰王江波高浩其李正辉杨建平
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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