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Modified terpolymer EP rubber and preparation method thereof

A EPDM rubber and modification technology, applied in the field of modified EPDM rubber and its preparation, can solve the problems of low production efficiency, difficult vulcanization of EPDM, long reaction time, etc. Simple and easy to implement, high grafting rate

Active Publication Date: 2017-04-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the reaction time of existing solution grafting method is too long, and production efficiency is low, and the side chain double bond of the ethylene-propylene rubber obtained by modification of existing grafting method just disappears after grafting MAH, makes the vulcanization of ethylene-propylene rubber more difficult

Method used

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  • Modified terpolymer EP rubber and preparation method thereof
  • Modified terpolymer EP rubber and preparation method thereof
  • Modified terpolymer EP rubber and preparation method thereof

Examples

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preparation example Construction

[0024] The present invention provides a kind of preparation method of modified ethylene-propylene-diene rubber, the method comprises under the ring-opening cross-metathesis reaction condition of olefin, in the presence of the ionic catalyst of structure shown in formula (2), EPDM The nadic acid anhydride of rubber and structure shown in formula (1) contacts in organic solvent,

[0025]

[0026] In formula (2), R 1 hydrogen, C2-C20 alkenyl, C2-C20 alkynyl, C1-C20 alkyl, C6-C20 aryl, C2-C20 carboxylate, C1-C20 alkoxy, C2- C20 alkenyloxy, C2-C20 alkynyloxy, C6-C20 aryloxy, C1-C20 alkylthio, C1-C20 alkylsulfonyl or C1-C20 alkylsulfinyl,

[0027] x 1 and x 2 are independently anionic ligands,

[0028] L 1 and L 2 each independently is a neutral ligand, and optionally L 1 and L 2 A neutral ligand capable of connecting to each other to form a two-coordinate;

[0029] Y is an anion, preferably a halide ion, more preferably an iodide ion, most preferably I 5 - ;

[0030]...

preparation example 1

[0095] This preparation example is used to illustrate the preparation of ionic catalysts.

[0096] Under nitrogen protection, add 0.76g of iodine, 0.85g of the compound shown in formula (7) (commercially purchased from Bailingwei Technology Co., Ltd.) and 20mL of dichloromethane into a 100mL three-necked flask, and stir at room temperature (25°C) for 0.5 Hour. The obtained mixture was separated by aluminum oxide column chromatography (the developing solvent was dichloromethane), and the obtained eluate was concentrated and washed with cyclohexane to obtain 1.31 g of a catalyst as a yellow solid. The obtained catalyst was subjected to H NMR spectroscopy ( 1 H-NMR) and carbon nuclear magnetic resonance ( 13 C-NMR) and X-ray single crystal diffraction analysis, confirmed that the obtained catalyst has a structure shown in formula (5).

[0097] 1 H-NMR(400MHz,DMSO)δ(ppm):1.35-2.06(m,33H),1.81(s,18H),2.62(m,4H),6.11(d,1H),7.38-7.50(m,5H ),7.59-7.67(m,3H).

[0098] 13 C-NMR (...

preparation example 2

[0102] This preparation example is used to illustrate the preparation method of Nadic anhydride of structure shown in formula (1).

[0103] Add 15.7 grams (0.16 mol) of maleic anhydride and 40 mL of toluene to a 100 mL reaction flask, place the reaction flask in a constant temperature cold bath, stir and cool to 5°C, and add cyclopentadiene 14 dropwise through a constant pressure dropping funnel. gram (0.2mol), control the temperature in the reaction bottle not to exceed 15°C, after the dropwise addition, raise the reaction temperature to 120°C and continue to stir for 1 hour, cool and precipitate white crystals, filter out the crude Nadic anhydride, and then recrystallize with toluene , filtered and dried to obtain 19.0 g of Nadic anhydride, the melting point (mp) of Nadic anhydride was 165.8°C-167°C, and the yield was 72.3%.

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Abstract

The invention discloses modified terpolymer EP rubber and a preparation method thereof. The method comprises the following steps: under a condition of an open loop cross-metathesis reaction of alkene, in the existence of an ion type catalyst with the structure shown in the formula (2), terpolymer EP rubber and nadic anhydride with the structure shown in formula (1) are contacted in an organic solvent. The preparation method of modified terpolymer EP rubber has the advantages of high grafting ratio, rapid reaction, simple steps, and easy enforcement. The grafting ratio of modified terpolymer EP rubber is 0.4-4wt%; compared with modified terpolymer EP rubber and unmodified terpolymer EP rubber, degree of unsaturation is 0.44-0.71mol / kg, and sulfuration speed is improved.

Description

technical field [0001] The invention relates to a modified EPDM rubber and a preparation method thereof. Background technique [0002] Ethylenepropylene diene monomer (EPDM) has excellent physical and chemical properties such as high elasticity, viscoelasticity, and electrical insulation, and its application in engineering plastics toughening and ozone aging resistance is very prominent. However, since EPDM rubber is a non-polar rubber, its oil resistance, chemical resistance, self-adhesion and mutual adhesion are poor, and it is difficult to blend with polar polymers, so its application range is limited. Therefore, it is particularly important to modify EPDM rubber to enhance its compatibility with polar polymers. [0003] In the prior art, mainly by grafting EPDM rubber with maleic anhydride (MAH), a strong polar group is introduced into the rubber molecular chain, so that the graft has strong polarity and reactivity, thereby The prepared graft has wide application prosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F255/06C08F232/08
Inventor 邵明波陈建军徐一兵唐正伟常学工
Owner CHINA PETROLEUM & CHEM CORP
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