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Binary star branched rare earth chloroether rubber and preparation method thereof

A technology of epichlorohydrin rubber and binary star, which is applied in the field of binary star-branched rare earth epichlorohydrin rubber and its preparation, can solve the problems of the limitation of epichlorohydrin rubber and the ineffective processing performance of epichlorohydrin rubber, etc., and achieve Excellent processing performance, easy design and regulation, and easy-to-obtain effect by synthesis method

Active Publication Date: 2017-06-16
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 for preparing high molecular weight polyalkylene oxide with rare earth complex catalyst", which involves homopolymers and copolymers of ethylene oxide / propylene oxide and epichlorohydrin, but No epichlorohydrin rubber with star branched structure is involved, the prepared epichlorohydrin rubber is limited to linear epichlorohydrin rubber, and the processing performance of epichlorohydrin rubber has not been effectively improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1, rare earth catalyst Nd(P 204 ) 3 -Al(i-Bu) 3 -H 2 Preparation of O

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

Embodiment 2

[0015] Embodiment 2, the preparation of binary star-branched rare earth chloroether rubber

[0016] Add 5ml of toluene to the polymerization bottle after repeated baking, vacuuming and filling with argon, then add monomer epichlorohydrin and ethylene oxide, the total amount of monomer [M] is 0.05mol, monomer epoxy chloride Propane / ethylene oxide molar ratio [ECH] / [EO] is 6 / 4. After fully stirring and mixing, add star branching agent 4-(diglycidylamino)phenyl glycidyl ether (TGAP ), the prepared catalyst of embodiment 1, wherein: [Nd] is 0.175mmol, [Al] / [Nd] molar ratio is 30, [H 2 The molar ratio of O] / [Nd] is 3.6, and the molar ratio of [TGAP] / [Nd] is 2.9. The reaction is carried out at 60°C for 8 hours. The branched rare earth chloroether rubber has a monomer conversion rate of 67.1%. The product structure and performance analysis results are as follows: the molecular weight is bimodal distribution, and the weight average molecular weight of the high molecular weight part ...

Embodiment 3

[0017] Other conditions are the same as in Example 2, the [TGAP] / [Nd] molar ratio is 4, and the monomer conversion rate is 65.4%. The product structure and performance analysis results are as follows: the molecular weight is bimodal distribution, and the weight average molecular weight of the high molecular weight part is 7.2×10 4 , the number average molecular weight is 6.5×10 4 , the weight average molecular weight of the low molecular weight part is 1.1×10 4 , the number average molecular weight is 0.9×10 4 , the high molecular weight peak accounts for 66.4%, the glass transition temperature T g -43.5°C.

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Abstract

The invention discloses a class of binary star-branched rare earth chloroether rubber and a preparation method thereof. P is an epichlorohydrin / ethylene oxide binary copolymer branched chain prepared by using a rare earth catalyst, and S is a star-branched agent residues; the degree of branching n is not less than 3, and the number average molecular weight of Pn-S is 5×10 4 -80×10 4 The mass percentage of combined epichlorohydrin is 10%-90%; the rare earth catalyst is composed of three parts: A, B and C, A is selected from rare earth neodymium organic compounds, B is selected from alkyl aluminum, and C is selected from active hydrogen-containing The compound has a molar ratio of B:A=5-50:1, C:A=1-10:1; the star-shaped branching agent is selected from polyepoxide group compounds.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and relates to a class of binary star-branched rare-earth chloride ether rubber and a preparation method thereof. Background technique [0002] Chlorine ether rubber is an important special rubber with excellent heat resistance, oil resistance, weather resistance and electrical conductivity. It is widely used in transportation, electronic appliances, aerospace and many other fields. Chlorine ether rubber is usually divided into epichlorohydrin homopolymer rubber, epichlorohydrin / ethylene oxide binary copolymer rubber and epichlorohydrin / ethylene oxide / allyl glycidyl ether terpolymer Rubber, among which dichloroether rubber is widely used because of its best technical economy. The traditional dichloroether rubber is prepared by using "alkylaluminum-water" or "alkylaluminum-phosphoric acid-the third component" as a catalyst, and has been used in industrial production, but the tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/26
Inventor 李杨郭方庄彬彬李婷婷牛慧申凯华马红卫魏志勇王艳色
Owner DALIAN UNIV OF TECH
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