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 polymer material synthesis, can solve the problems of the limitation of epichlorohydrin rubber and the processing performance of epichlorohydrin rubber has not been effectively improved, and achieve excellent processing performance, easy molecular structure parameters, and high activity Effect

Active Publication Date: 2017-06-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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, the preparation of rare earth catalyst

[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 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 epichlorohydrin, the total amount of monomer [M] is 0.05mol, after fully stirring and mixing, add star branch according to the proportion Catalyst prepared by oxidizing agent ethylene glycol diglycidyl ether (EGDE), embodiment 1, wherein: [Nd] is 0.175mmol, [Al] / [Nd] mol ratio is 30, [H 2 The molar ratio of O] / [Nd] is 3.6, and the molar ratio of [EGDE] / [Nd] is 28.5. The reaction is carried out at 60°C for 8 hours. Rare earth chloroether rubber, the monomer conversion rate is 55.8%. 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 25.4×10 4 , the number average molecular weight is 19.8×10 4 , the weight average molecular weight o...

Embodiment 3

[0017] Embodiment 3, the preparation of star branched rare earth chloroether rubber

[0018] Other conditions are the same as in Example 2, the [EGDE] / [Nd] molar ratio is 57.1, and the monomer conversion rate is 57.6%. 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 26.9×10 4 , the number average molecular weight is 13.0×10 4 , the weight average molecular weight of the low molecular weight part is 2.3×10 4 , the number average molecular weight is 1.7×10 4 , the high molecular weight peak accounts for 60.0%, the glass transition temperature T g -27.8°C.

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Abstract

The invention discloses a class of star-branched rare earth chloroether rubber and a preparation method thereof. Its structure has the following characteristics: Pn-S, wherein: P is an epichlorohydrin polymer branch prepared by using a rare earth catalyst, and S is a star shape branching agent residue; n is 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 rare earth catalyst is composed of the following three parts: A, B and C, and the molar ratio of each component is: B:A=(5-50):1, C:A=(1-10):1 , wherein: A is selected from rare earth neodymium organic compounds, B is selected from aluminum alkyls, and C is selected from compounds containing active hydrogen; the star branching agent is selected from polyepoxy compounds.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and relates to a class of 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 epichlorohydrin homopolymer rubber is widely used because of its simple structure, low price and easy availability. The traditional epichlorohydrin homopolymer epichlorohydrin rubber is prepared by using "alkylaluminum-water" or "alkylaluminum-phosphoric acid-the third component" as a ...

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申凯华牛慧王艳色马红卫魏志勇
Owner DALIAN UNIV OF TECH
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