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Ethylene-propylene-diene monomer (EPDM) and preparation method

A technology of EPDM rubber and compounds, which is applied in the field of polymer material preparation, can solve the problems of reduced catalyst activity and low catalytic efficiency, and achieve the effects of appropriate double bond content, high catalytic efficiency and low cost

Active Publication Date: 2014-07-30
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The EPDM rubber prepared by the prior art has good vulcanization performance and processability, but the third monomer used in the prior art will reduce the activity of the catalyst in the process of preparing the EPDM rubber, so the existing The preparation method of EPDM rubber provided by the technology has low catalytic efficiency

Method used

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  • Ethylene-propylene-diene monomer (EPDM) and preparation method
  • Ethylene-propylene-diene monomer (EPDM) and preparation method
  • Ethylene-propylene-diene monomer (EPDM) and preparation method

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preparation example Construction

[0021] The invention provides a kind of preparation method of EPDM rubber, comprising:

[0022] Under the action of vanadium-based catalysts, alkylaluminum compounds and organic chlorides, polyfunctional compounds, propylene and ethylene are polymerized to obtain EPDM rubber; the multifunctional compounds include trimethylolpropane Acrylates, diethylene glycol diacrylate, divinylbenzene or N,N'-methylenebisacrylamide.

[0023] The present invention uses the multifunctional compound as the third monomer to carry out polymerization reaction with ethylene and propylene, and the addition of the third monomer will not reduce the catalytic activity of the vanadium-based catalyst. Compared with the prior art, the present invention provides The preparation method of EPDM rubber has higher catalytic efficiency. In addition, the low price of the multifunctional compound makes the preparation method of the EPDM rubber provided by the present invention relatively low in cost; moreover, t...

Embodiment 1

[0043] Replace the reactor with nitrogen for 3 times and keep the seal of the reactor; under the condition of stirring, add 0.1mmol of VOCl in the reactor successively 3 , 2.0mmol of Al 2 (C 2 h 5 ) 3 Cl 3 , 2.0mmol of Al 3 (C 2 h 5 ) 3 Cl 3 With the mixed solution of the trimethylolpropane triacrylate (TMPTA) of 1.1g, the ethyl trichloroacetate (ETCA) of 0.6mmol and the hexane of 300mL after mixing, in the mixture that passes through is 1: 2 mixed gas of ethylene and propylene, carry out the polymerization reaction at 0.4MPa, 20°C for 30min; add 5% hydrochloric acid ethanol solution to the obtained reaction product, wash with ethanol, vacuum the washed reaction product After drying, 20.5 g of EPDM rubber was obtained.

[0044] The EPDM rubber that the embodiment of the present invention 1 obtains is carried out nuclear magnetic resonance test, test result is as follows figure 1 as shown, figure 1 For the nuclear magnetic resonance spectrogram of the EPDM rubber th...

Embodiment 2

[0047] Replace the reactor with nitrogen for 2 times and keep the seal of the reactor; under the condition of stirring, add 0.1mmol of VOCl to the reactor successively 3 , 6.0mmol of Al(C 2 h 5 ) 2 Cl 2 , 0.6mmol of ethyl trichloroacetate, 1.06g of TMPTA and 300mL of hexane are mixed, and a mixed gas of ethylene and propylene with a mass ratio of 1:3 is introduced into the obtained mixture at 0.4MPa and 30°C. 30min polymerization reaction; add 5% ethanol hydrochloric acid solution to the obtained reaction product, wash with ethanol, and vacuum dry the washed reaction product to obtain 15.6 g of EPDM rubber.

[0048] Test the double bond content of the EPDM rubber obtained in Example 2 of the present invention according to the method described in Example 1, and the test result is that the double bond mass content of the EPDM rubber obtained in Example 2 of the present invention is 6.2%; According to the method described in Example 1, the glass transition temperature, number...

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Abstract

The invention provides a preparation method of an ethylene-propylene-diene monomer (EPDM). The preparation method comprises the step of subjecting a polyfunctional compound, ethylene and propylene to polymerization reaction in the presence of a vanadium catalyst, alkylaluminum compounds and organic chloride, thus obtaining the EPDM, wherein the polyfunctional compound includes trimethylolpropane triacrylate, diethylene glycol diacrylate, divinyl benzene or N,N'-methylene bisacrylamide. The polyfunctional compound is adopted as a third monomer to carry out polymerization reaction with ethylene and propylene, and the catalytic activity of the vanadium catalyst can not be reduced by addition of the third monomer. Compared with the prior art, the preparation method of the EPDM has relatively high catalytic efficiency. Besides, the polyfunctional compound is low in price, so that the preparation method of the EPDM is relatively low in cost. The prepared EPDM has proper content of double bonds and is odourless.

Description

technical field [0001] The invention relates to the technical field of preparation of polymer materials, in particular to a EPDM rubber and a preparation method thereof. Background technique [0002] EPDM rubber is a terpolymer of ethylene, propylene and non-conjugated dienes. It has excellent oxidation resistance, ozone resistance and erosion resistance. At the same time, because EPDM rubber belongs to the polyolefin family, it is Also has excellent vulcanization. EPDM rubber can be widely used in the automotive industry, construction industry and electrical and electronic industries. [0003] At present, the third monomers used in the industrial production of EPDM rubber include non-conjugated dienes such as ethylidene norbornene (ENB), dicyclopentadiene (DCPD) and 1,4-hexadiene (HD). The Chinese patent application number 201310033554.7 discloses a preparation method of EPDM rubber. The specific process is: fully replace the reactor with nitrogen, and then add polymeriza...

Claims

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Application Information

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IPC IPC(8): C08F210/18
Inventor 那丽华张学全白晨曦张春雨于琦周毕吉福代全权张贺新胡雁鸣
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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