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Preparation method of EPDM (Ethylene-Propylene-Diene Monomer) rubber

A technology of EPDM rubber and ethylene, which is applied in the field of rubber materials, can solve the problems of less types of third monomers and unfavorable development of EPDM rubber, and achieve good processing performance, appropriate double bond content, and high conversion rate Effect

Active Publication Date: 2013-01-09
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are fewer types of third monomers, and there are various disadvantages, which are not conducive to the development of EPDM

Method used

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  • Preparation method of EPDM (Ethylene-Propylene-Diene Monomer) rubber
  • Preparation method of EPDM (Ethylene-Propylene-Diene Monomer) rubber
  • Preparation method of EPDM (Ethylene-Propylene-Diene Monomer) rubber

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Experimental program
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preparation example Construction

[0025] The embodiment of the present invention discloses a preparation method of EPDM rubber, comprising the following steps:

[0026] In an organic solvent, ethylene, propylene and a third monomer are polymerized under the action of a catalyst system to obtain EPDM rubber;

[0027] The third monomer is a polybutadiene rubber with a 1,2-polybutadiene content of more than 9% or a polyisoprene rubber with a 3,4-polyisoprene content of more than 9%, and the The weight average molecular weight of the third monomer is 200,000 to 1 million;

[0028] The catalyst system includes a vanadium-based catalyst, an aluminum alkyl compound and an activation accelerator;

[0029] The vanadium series catalyst is VOCl 3 , VO (P 204 ) 2 , V (acac) 3 、VOCl 3 nMOH, VO 2 Cl (trioctylamine), VO 2 Cl 3 3 (tributyl phosphate), VO(OH) (octahydroxyquinoline) 2 or VO(OH)·(α-benzoin oxime) 2 , M is an alkyl group of C5~C8, 2.5≤n≤3.5;

[0030] Alkyl aluminum compound is AlR 3 , AlR 2 X, Al 2...

Embodiment 1

[0040] In a 0.5L reactor fully replaced with nitrogen, add (1) 300ml hexane, (2) 0.10mmol VOCl 3 , (3) 3.0mmol trichlorotriethyldialuminum, molecular formula: Al 2 (C 2 h 5 ) 3 Cl 3 , (4) 100ml of hexane solution containing 0.15g polybutadiene rubber, the weight average molecular weight of the polybutadiene rubber is 2.0×10 5 , with a 1,2-polybutadiene content of 16% and (5) 0.60 mmol of ethyl trichloroacetate (ETCA);

[0041] Then, feed the mixed gas of ethylene and propylene into the reactor, the molar ratio of ethylene and propylene in the mixed gas is 1:2, the pressure reaches 0.4MPa, stir, and react at 20°C for 15min.

[0042] After the polymerization, 5ml of 5% by mass hydrochloric acid-ethanol solution was added to the polymerization product, washed with ethanol, and then dried under vacuum to obtain 12.2g of EPDM rubber.

[0043] According to differential calorimetry (DSC) analysis, the glass transition temperature of the obtained EPDM rubber is -56.6°C; 13 C NM...

Embodiment 2

[0045] In a 0.5L reactor fully replaced with nitrogen, add (1) 300ml hexane, (2) 0.10mmol VOCl 3 , (3) 3.0mmol trichlorotriethyldialuminum, molecular formula: Al 2 (C 2 h 5 ) 3 Cl 3 , (4) hexane solution containing 0.3g polybutadiene rubber, the weight average molecular weight of the polybutadiene rubber is 2.0×10 5 , with a 1,2-polybutadiene content of 21% and (5) 0.60 mmol of ethyl trichloroacetate (ETCA);

[0046] Then, feed the mixed gas of ethylene and propylene into the reactor, the molar ratio of ethylene and propylene in the mixed gas is 1:2, the pressure reaches 0.4MPa, stir, and react at 20°C for 15min.

[0047] After the polymerization, 5 ml of 5% by mass hydrochloric acid-ethanol solution was added to the polymerization product, washed with ethanol, and then dried under vacuum to obtain 13.3 g of EPDM rubber.

[0048] The performance of the obtained EPDM rubber is tested, and the results are shown in Table 1, and Table 1 is the performance parameters of the E...

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Abstract

The invention provides a preparation method of an EPDM (Ethylene-Propylene-Diene Monomer) rubber. The method comprises the steps of polymerizing an ethylene, a propylene and a third monomer in an organic solvent under the action of a catalyst system to obtain the EPDM rubber. The third monomer is polybutadiene rubber with the content of over 9% of 1, 2-polybutadiene or polyisoprene rubber with the content of over 9% of 3, 4-polyisoprene, and the weight-average molecular weight of the third monomer is 200000-1000000; The catalyst system comprises a vanadium catalyst, an alkyl aluminum compound and an activation promoter. The obtained EPDM rubber has appropriate double bonds, so that sulfonation of the rubber can be carried out by using sulfur, and the EPDM rubber has good vulcanizing property and good processability. The experimental result shows that in the prepared EPDM rubber, the mole percentage of the double bond is 2%-10.5%, and the molecular weight distribution index is 2-5.

Description

technical field [0001] The invention relates to the field of rubber materials, in particular to a preparation method of EPDM rubber. Background technique [0002] Ethylene-propylene rubber is a copolymer rubber with ethylene and propylene as the basic monomers. Compared with other rubber varieties, ethylene propylene rubber has the following advantages: 1. The main chain does not contain double bonds, is completely saturated, ozone resistance, aging resistance, chemical resistance and high temperature resistance; 2. Light specific gravity; 3. Excellent insulation performance ; Fourth, it is a rubber variety that can be highly oil-filled. Ethylene propylene rubber is one of the most promising types of rubber at present. Since its commercial production, its application fields have been continuously expanded, and it has been widely used in auto parts, building materials, wires and cables, heat-resistant rubber hoses, advanced sealing materials, lubricants Additives and polyol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F279/02C08F4/68C08J3/24
Inventor 那丽华张学全李继文于琦周张春雨蔡洪光毕吉福代全权张贺新白晨曦
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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