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Ternary star branched rare earth chloroether rubber and preparation method thereof

A technology of epichlorohydrin rubber and rare earth, which is applied in the field of ternary star-branched rare earth epichlorohydrin rubber and its preparation, and can solve the problem that the processing performance of epichlorohydrin rubber has not been effectively improved, the problem of vulcanization of epichlorohydrin rubber has not been solved, and the chlorine Ether rubber limitations and other issues, to achieve the effects of easy design and control, excellent vulcanization performance, and excellent processing performance

Active Publication Date: 2018-12-18
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Shen Zhiquan disclosed in the invention patent CN85104956B "the method of preparing high molecular weight polyalkylene oxide with rare earth complex catalyst", which involves homopolymers and copolymers of ethylene oxide / propylene oxide and epichlorohydrin, but It does not involve the epichlorohydrin rubber with a star-shaped branched structure, and the prepared epichlorohydrin rubber is limited to linear epichlorohydrin rubber, and the processing performance of the epichlorohydrin rubber has not been effectively improved; Terpolymer of propyl glycidyl ether, glycidyl methacrylate and other unsaturated cyclic ethers, the prepared epichlorohydrin rubber is limited to binary linear epichlorohydrin and ethylene oxide / propylene oxide Rubber, the vulcanization problem of epichlorohydrin rubber has not been solved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1. Preparation of rare earth catalyst

[0014] With rare earth catalyst Nd(P 204 ) 3 -Al(i-Bu) 3 -H 2 Take the preparation of O as an example. In a glove box, weigh a certain amount of Nd(P 204 ) 3 Put it into a Schlenk bottle with a magnetic stirrer, add a certain amount of toluene solvent, and then add a certain amount of Al(i-Bu) 3 , Stir at 50°C for 1h; then, add a certain amount of water and stir at 50°C for 30min to obtain a rare earth catalyst solution.

Embodiment 2

[0015] Example 2. Preparation of ternary star-shaped branched rare earth chloroether rubber

[0016] Add 5ml of toluene to the polymerization bottle after repeated baking, vacuuming and filling with argon, and then add monomer epichlorohydrin (ECH), ethylene oxide (EO), allyl glycidyl ether (AGE), The total amount of monomer [M] is 0.05 mol, and the molar ratio of ECH / EO / AGE is 60 / 35 / 5. After fully stirring and mixing, add the star branching agent 4-(diglycidylamino) phenyl according to the ratio Glycidyl ether (TGAP), the catalyst prepared in Example 1, wherein: [Nd] is 0.175mmol, [Al] / [Nd] molar ratio is 30, [H 2 The molar ratio of O] / [Nd] is 3.6, the molar ratio of [TGAP] / [Nd] is 2.9, and the reaction is carried out at 60°C for 8 hours. After the reaction, the polymer is dried by traditional post-treatment methods to obtain a ternary star The branched rare earth chloroether rubber has a monomer conversion rate of 78.3%. The product structure and performance analysis results a...

Embodiment 3

[0017] Example 3. Preparation of ternary star-shaped branched rare earth chloroether rubber

[0018] The other conditions are the same as in Example 2, the [TGAP] / [Nd] molar ratio is 4, and the monomer conversion rate is 75.5%. The results of the product structure and performance analysis are as follows: the molecular weight is bimodal, and the weight average molecular weight of the high molecular weight part is 8.6×10 4 , The number average molecular weight is 7.1×10 4 , The weight average molecular weight of the low molecular weight part is 1.6×10 4 , The number average molecular weight is 1.3×10 4 , High molecular weight peak accounted for 75.6%, glass transition temperature T g It is -46.6°C.

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Abstract

The invention discloses three-element star-branched rare-earth epichlorohydrin rubber (Pn-S) and a preparation method thereof. P is an epichlorohydrin / oxirane / unsaturated cyclic ether terpolymer branch chain, and S is star-branched agent residue; branching degree n is not less than 3, and number-average molecular weight of the Pn-S is 5*10<4>-80*10<4>; content of combined unsaturated cyclic ether is 2%-10%, and content of epichlorohydrin is 15%-85%; a catalyst is composed of three parts A, B and C, A is selected from rare-earth neodymium organic compounds, B is selected from alkyl aluminium, C is selected from active hydrogen compounds, and mole ratios satisfy that B:A=(5-50):1 and C:A=(1-10):1; the star-branched agent is selected from multi-epoxy-group compounds.

Description

Technical field [0001] The invention belongs to the technical field of polymer material synthesis, and relates to a type of ternary star-shaped branched rare earth chloroether rubber and a preparation method thereof. Background technique [0002] Chloroether rubber is an important special rubber with excellent heat resistance, oil resistance, weather resistance and electrical conductivity. It is widely used in many fields such as transportation, electronics and aerospace. Chloroether rubber is usually divided into epichlorohydrin homopolymer rubber, epichlorohydrin / ethylene oxide binary copolymer rubber and epichlorohydrin / ethylene oxide / allyl glycidyl ether terpolymer Rubber, among them, ternary chloroether rubber has attracted more and more attention because of its more excellent vulcanization properties. The traditional ternary chloroether rubber is prepared with "alkyl aluminum-water" or "alkyl aluminum-phosphoric acid-the third component" as the catalyst, and has been used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/26
Inventor 李杨郭方李婷婷牛慧魏志勇申凯华马红卫王艳色
Owner DALIAN UNIV OF TECH
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