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Method for preparing EPDM g-SAN toughening agent containing high quantity EPDM

A technology of toughening agent and content, applied in the field of toughening agent preparation, can solve the problems of large amount of solvent, difficult treatment and high production cost, and achieve the effects of less amount of solvent, simple post-processing process and easy recovery.

Active Publication Date: 2009-12-09
SOUTH CHINA UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The significant disadvantage of the solution method is that the conversion rate of the monomer is low, which generally can only reach about 75% (wt), and the amount of solvent is large, and the ratio of (EPDM+St+An) / solvent (wt / wt) is lower than 1 / 4, that is, The solvent accounts for more than 80% of the mass of the entire polymerization system, and the product needs to be precipitated with a large amount of methanol. The recovered waste liquid is a mixture of solvent, residual monomer and methanol. The process of separating, purifying and recycling the components is complicated, and the investment in equipment is large. lead to high production costs
Japanese patent JP48017895 discloses a method for directly synthesizing AES by water-phase suspension polymerization using solubilized solvent, but the amount of n-hexane used as a solvent in this method is 10 times the mass of EPDM, and the conversion rate of monomer is only 70.8%, and the post-treatment of solvent is difficult , and the EPDM content of the prepared AES is only about 26wt%, the product belongs to AES engineering plastics and cannot be used as a toughening agent

Method used

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  • Method for preparing EPDM g-SAN toughening agent containing high quantity EPDM
  • Method for preparing EPDM g-SAN toughening agent containing high quantity EPDM
  • Method for preparing EPDM g-SAN toughening agent containing high quantity EPDM

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 48g of EPDM and 90g of toluene to a 1000ml three-neck round bottom flask equipped with a condensing reflux tube, a stirrer, and an oil bath heating temperature controller, stir and dissolve at a low speed of 60°C for 12 hours, and add 20.8g of benzene in which 0.48g of BPO has been dissolved. A mixed monomer of ethylene and 11.2 g of acrylonitrile. Control the stirring speed to be 150 rev / min, add 0.12 g of sodium lauryl sulfate powder after stirring for 10 minutes, and continue stirring for 5 minutes. 45 g of 2% polyvinyl alcohol-224 (PVA-224) aqueous solution was added dropwise to the reaction system, and the dropwise addition was completed within 15 minutes. At the same time, the stirring speed was gradually increased to 1200 rpm. Slowly add 250 g of deionized water into the flask, pass nitrogen gas for 15 minutes, and raise the reaction temperature to 80° C. within 5 minutes under the protection of nitrogen gas. After reacting for 20 hours, the system was cool...

Embodiment 2

[0041] Add 36g of EPDM, 30g of cyclohexanone, and 24g of n-heptane into a 1000ml three-necked round-bottomed flask equipped with a condensing reflux tube, a stirrer, and an oil bath heating and temperature controller, and stir and dissolve at a low speed of 60°C for 12 hours. A mixed monomer of 27 g styrene and 9 g acrylonitrile with 0.16 g tert-butyl peroxide 2-ethylhexanoate and 0.2 g dibenzoyl peroxide. Control the stirring speed to 120 rev / min, add 0.08 g of sodium dodecylbenzenesulfonate powder after stirring for 10 minutes, and continue stirring for 5 minutes. 30 g of 4% methylcellulose aqueous solution was added dropwise to the reaction system, and the dropwise addition was completed within 15 minutes, while adjusting the stirring speed to gradually increase to 1200 rpm. Slowly add 350 g of deionized water into the flask, pass nitrogen gas for 15 minutes, and raise the reaction temperature to 75° C. within 5 minutes under the protection of nitrogen gas. After reacting ...

Embodiment 3

[0044] Add 56g of EPDM and 140g of xylene into a 1000ml three-necked round-bottomed flask equipped with a condensing reflux tube, a stirrer, and an oil bath heating and temperature controller, stir and dissolve at a low speed of 60°C for 11 hours, and add and dissolve 0.6g of 1,1-bis A mixed monomer of 13.2 g of styrene and 10.8 g of acrylonitrile of (tert-butylperoxy)-3,3,5-trimethylcyclohexane. Control the stirring speed to 160 rev / min, add 0.12g sodium dodecylbenzenesulfonate powder and 0.1g T polyoxyethylene sorbitan monooleate (Tween80) after stirring for 10 minutes, and continue stirring for 5 minutes. 66 g of 1% methylcellulose aqueous solution was added dropwise to the reaction system, and the addition was completed within 15 minutes, while adjusting the stirring speed to gradually increase to 1000 rpm. Slowly add 264 g of deionized water into the flask, pass nitrogen gas for 15 minutes, and raise the reaction temperature to 90° C. within 5 minutes under the protection...

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Abstract

This invention discloses a method for preparing EPDM-g-SAN toughening agent with a high EPDM content. The method comprises: dissolving EPDM in an inert good solvent, adding mixed monomers of styrene and acrylonitrile, initiator and co-dispersant, stirring at a low speed to uniform mixing, dropping dispersant aqueous solution under high speed stirring, dropping deionized water, heating under nitrogen protection, filtering out the product, washing with water, and drying to obtain EPDM-g-SAN toughening agent with 50-75% of EPDM. When the EPDM-g-SAN toughening agent is melt-blended with SAN resin, an engineering plastic AES is obtained, which has high weathering, aging, yellowing and impact resistance. The method has such advantages as low solvent consumption, high monomer conversion rate, high grafting rate and simple product post-treatment. The EPDM-g-SAN toughening agent has high toughening efficiency.

Description

technical field [0001] The invention relates to the preparation of a toughening agent, in particular to a synthesis method of a graft copolymer EPDM-g-SAN toughening agent. Background technique [0002] Ethylenepropylene rubber (EPDM) and styrene (St) and acrylonitrile (An) mixed monomer (St-An) graft copolymer (AES) is for the synthesis of butadiene rubber and St-An graft copolymer ( The high cis-butadiene rubber used in ABS) contains a large amount of carbon-carbon double bonds that are easy to oxidize, which leads to a kind of styrene-based toughening resin developed by ABS with poor weather resistance and yellowing performance. It was developed by Copolymer-Rubber in 1970. It was put into production first, and then Japan's Idemitsu Petroleum Company, JSR Company and Germany's Bayer Company have been put into production one after another. The preparation methods of AES include direct synthesis method and blending method. The direct synthesis method is to use the solutio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F255/06C08F4/18C08F2/44
Inventor 王炼石张敦福蔡彤旻张安强曾祥斌
Owner SOUTH CHINA UNIV OF TECH