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Ethylene-propylene-diene methylene using liquid-state oligomers of diolefin as third monomer and method for preparing same

A technology of EPDM rubber and oligomers, which is applied in the field of EPDM rubber and its preparation, can solve the problems of slow vulcanization speed, easy explosion, high price, etc., achieve good copolymerization ability, and be conducive to industrialization , good processing performance

Active Publication Date: 2012-11-07
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

DCPD [2，3] The advantages of ENB are low price and active polymerization performance. The disadvantages are high toxicity, easy explosion in the late stage of distillation, and slow vulcanization speed; ENB is currently the third monomer commonly used in countries all over the world. Its advantages are good polymerization and fast copolymerization speed. The vulcanization speed can be similar to that of styrene-butadiene rubber, and the production process is relatively mature. The disadvantage is that the synthesis and separation of ENB are difficult, expensive, and will greatly reduce the polymerization activity, making the price of EPDM much higher than that of general-purpose rubber. At the same time, in the production process The smell is strong, and the residual ENB is difficult to remove, which is not conducive to environmental protection [4，5] ; 1,4-hexadiene is slightly lower than ENB in ​​terms of vulcanization speed, etc., and the most obvious disadvantage is high cost. Therefore, these types of dienes are not completely satisfactory, which hinders the further development of ethylene-propylene rubber. The study of the third monomer has not made breakthrough progress in ten years

Method used

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  • Ethylene-propylene-diene methylene using liquid-state oligomers of diolefin as third monomer and method for preparing same
  • Ethylene-propylene-diene methylene using liquid-state oligomers of diolefin as third monomer and method for preparing same
  • Ethylene-propylene-diene methylene using liquid-state oligomers of diolefin as third monomer and method for preparing same

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the 0 and 5L reactors fully replaced with nitrogen, respectively add: (1) 300ml hexane; (2) 0.10mmol vanadium catalyst; (3) 3.0mmol trichlorotriethyldialuminum, molecular formula: Al 2 (C 2 h 5 )3 Cl 3 ; 0.15g diene liquid oligomer A, 1,2-structure content at 20%; (4) ethyl trichloroacetate of 0.60mmol, (hereinafter referred to as: ETCA); (5) pass into ethylene and propylene mixed gas , the molar ratio of ethylene and propylene in the mixed gas is 1:2, the pressure reaches 4MPa, stir, and react at 20°C for 15min.

[0029] After the polymerization, 5 ml of 5% by mass hydrochloric acid-ethanol solution was added to the polymer product, washed with ethanol, and then dried under vacuum to obtain 12.2 g of polymer.

[0030] Through differential calorimetry (DSC) analysis, the glass transition temperature of gained polymer is 55.6 ℃; 13 C-NMR spectral analysis, the combined propylene molar content (C 3 mol%): 34%, double bond content: 1.2%; GPC analysis shows that the...

Embodiment 2-6

[0032] Use 1.0g, 2.5, 3.7g, 4.5g, 6g of diene liquid oligomer A respectively, and the polymerization conditions are: (1) 0.5L reactor; (2) Vanadium-based catalyst: 0.10mmol; (3) Al 2 (C 2 h 5 ) 3 Cl 3 : 3.0mmol, diolefin liquid oligomer A, 1,2-structure content at 20%; (4) ETCA: 0.60mmol; (5) 300ml solvent hexane; (6) ethylene, propylene molar ratio in the mixed gas is 1:2, pressure: 4MPa, react at 20°C for 15min.

[0033] The rest carry out polymerization reaction and polymer analysis test with [embodiment 1] same method and condition. The results are listed in Table 1.

[0034] Table 1

[0035] no

Embodiment 7-11

[0037] Respectively use 2.5g diene liquid oligomer A, 1,2-structure content at 30%, 40%, 50%, 65%, 80% substitute [embodiment 1] in the diene liquid oligomer A of 0.15g , 1,2-structure content at 20%, the polymerization conditions are: (1) 0.5L reactor; (2) vanadium series catalyst: 0.10mmol; (3) Al 2 (C 2 h 5 ) 3 Cl 3 : 3.0mmol, diene liquid oligomer A: 2.5g; (4) ETCA: 0.60mmol; (5) 300ml solvent hexane; (6) the molar ratio of ethylene and propylene in the mixed gas is 1: 2, pressure: 4MPa , reacted at 20°C for 15min.

[0038] The rest carry out polymerization reaction and polymer analysis test with [embodiment 1] same method and condition. The results are listed in Table 2.

[0039] Table 2

[0040] no

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Abstract

The invention provides ethylene-propylene-diene methylene taking liquid-state oligomers of diolefin as a third monomer and a method for preparing same. Combined propylene cells account for 20 to 45 molar percent of the ethylene-propylene-diene methylene, the third monomer which is a liquid-state oligomer of diolefin accounts for 0.5 to 15 molar percent of the ethylene-propylene-diene methylene, and the total molar percentage of the combined cells of ethylene, propylene and the third monomer is 100 percent; and the liquid-state oligomer of diolefin of the third monomer is selected from liquid-state oligomers with different double-bond structures and double-bond contents, including the liquid polybutadiene containing 20 to 80 percent of 1,2-strucutres and liquid polyisoprene containing over90 percent of 1,4-strucutres. Because the side chains contain more double bonds, the ethylene-propylene-diene methylene has good curing and processing properties, and can vulcanize sulfur; the polymer has the molecular weight distribution indexes from 2 to 10; the ethylene-propylene-diene methylene can be used for manufacturing industrial rubber products of automobile parts, waterproof materials,telecom cables and the like.

Description

technical field [0001] The invention belongs to EPDM rubber with diene liquid oligomer as the third monomer and a preparation method thereof. Background technique [0002] Ethylene-propylene rubber (EPR) is a kind of copolymerized rubber with ethylene and propylene as basic monomers after the invention of Ziegler-Natta catalyst and the advent of polyethylene and polypropylene. The industrial production methods of ethylene-propylene rubber mainly include solution polymerization and suspension polymerization. Compared with other rubber varieties, EPR has the following advantages: 1. The main chain does not contain double bonds and is completely saturated, making it an ozone-resistant, aging-resistant, chemical-resistant, high-temperature-resistant hydrocarbon rubber; 2. Specific gravity It is the lightest among elastomers, which helps to use the least material in a certain volume; 3. It has excellent insulation performance and can be an excellent material for wires and cables...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F279/02
Inventor 那丽华张春雨郝秀峰于琦周张学全
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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