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Preparation method for ethylene-series random copolymer

A random copolymerization, ethylene-based technology, applied in the field of preparation of olefin-based random copolymers, can solve the problems of reduced physical and mechanical properties, polymers are prone to gelation, etc.

Active Publication Date: 2017-07-04
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] EPDM rubber has become an indispensable type of rubber in the rubber field. There are many companies in the world producing this elastomer. There are no less than hundreds of grades of this elastomer. Among many grades, the application Brands used in the automotive industry have accounted for about 40% of the amount of ethylene-propylene rubber, mainly solid sealing strips, sponge strips, automotive hoses, etc. It is well known in the industry that the demand for ethylene-propylene rubber Mooney used in automotive sealing strips is very high, and The ethylene propylene rubber with too high Mooney will affect the processing of downstream industries, so this kind of ethylene propylene rubber with high Mooney needs to be filled with paraffin oil to reduce the Mooney viscosity without affecting the application, which requires more oil in the production of ethylene propylene rubber In one process, the paraffin oil added must meet the requirements of downstream manufacturers, so there is a lot of inconvenience
In order to improve the processing performance of ethylene-propylene rubber, Japanese Patent Publication No. 6-89072 and International Patent WO2007 / 018245 all use the fourth monomer vinyl norbornene (VNB). The molecular weight distribution of this tetrapolymer is 4 -10 or so, the processing performance of the polymer has been improved, but because the two double bonds in the vinyl norbornene molecule are very active, the resulting polymer is prone to gelation, which is why VNB cannot completely replace ENB so far The reason; mentioned in Japanese patent patent 6-18942, by secondary alcohol to VOCl 3 Modification is carried out so that the molecular weight distribution of the ethylene-propylene copolymer is about 5-25. Although the processability of this wide-distributed copolymer is improved, the physical and mechanical properties will be reduced, which cannot meet the needs of some fields.

Method used

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  • Preparation method for ethylene-series random copolymer

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preparation example Construction

[0033] A preparation method of ethylene random copolymer, comprising the following steps:

[0034] Step 1: Treat the reactor with nitrogen in anhydrous and oxygen-free manner under vacuum, then add solvent, ethylene, α-olefin, non-conjugated diene and molecular weight regulator into the reactor, and stir evenly;

[0035] Step 2: Add the main catalyst, co-catalyst and activator to carry out the polymerization reaction. The polymerization reaction temperature is 15-60°C, the reaction pressure is 0.01-2MPa, and the reaction time is 10-180 minutes. The preferred polymerization reaction temperature is 25-45°C , the reaction pressure is 0.1-1 MPa, and the reaction time is 20-60 minutes; and

[0036] Step 3: Add ethanol to terminate the reaction, then add anti-aging agent, remove the solvent from the obtained glue, then separate the glue to obtain the product ethylene random copolymer, and then dry the product to obtain dry glue, wherein there is 0.8 to 1wt in the dry glue % of anti...

Embodiment 1

[0071] The preparation of the ethylene-propylene copolymer is carried out in a 10L reactor with stirring, jacket cooling, inlet pipe, feed pipe, outlet pipe, and outlet pipe. Mix ethylene, propylene, and hydrogen through a mixing device, and then fully mix them uniformly through a circulating compressor. The 10L polymerization kettle is subjected to anhydrous and oxygen-free treatment under vacuum for 1 hour. The inert gas used is high-purity nitrogen, and then Add 5000ml of dry hexane (water content≤10ppm) to it, which contains 18ml of ethylidene norbornene (ENB), turn on the circulation compressor, feed the mixed gas into the polymerization kettle, the mixed gas flow rate is 150L / hour, make the hexane The dissolved mixed gas reaches saturation, and then 20ml of soluble vanadium compound VO(OEt)Cl containing 1mmol is added successively 2 The hexane solution of catalyst, add the mixture of monochlorodiethylaluminum (AM) and trichlorotriethyldialuminum (AQ), wherein the molar r...

Embodiment 2、3、4

[0073] The polymerization operation process was the same as in Example 1, except that the proportion of mixed aluminum in the cocatalyst was changed, and the addition of reactants and hydrogen were adjusted. See Table 1 for details.

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Abstract

The invention provides a preparation method for an ethylene-series random copolymer. The preparation method comprises the following steps: subjecting a reaction vessel to waterless oxygen-free treatment with nitrogen in a vacuum state, then adding a solvent, ethylene, alpha-olefin, unconjugated diene and a molecular weight regulator, and carrying out uniform mixing under stirring; adding a main catalyst, a cocatalyst and an activator for polymerization; adding ethanol to terminate polymerization and then adding an antioxidant; subjecting a glue solution obtained in the previous step to desolventization, and separating glue so as to obtain the product ethylene-series random copolymer; and drying the product so as to obtain dry glue, wherein the dry glue contains 0.8 to 1 wt% of the antioxidant; the main catalyst is alcohol-modified vanadium oxytrichloride; the cocatalyst is a mixture of aluminum diethyl monochloride and triethyldialuminum trichloride; the molecular weight regulator is diethyl zinc or hydrogen; the solvent is aliphatic alkane, cycloalkane or an aromatic compound; the activator is ethyl trichloroacetate; and the antioxidant is 2,6-di-t-butyl-p-cresol.

Description

technical field [0001] The invention relates to a method for preparing an olefin random copolymer. Background technique [0002] EPDM rubber has become an indispensable type of rubber in the rubber field. There are many companies in the world producing this elastomer. There are no less than hundreds of grades of this elastomer. Among many grades, the application Brands used in the automotive industry have accounted for about 40% of the amount of ethylene-propylene rubber, mainly solid sealing strips, sponge strips, automotive hoses, etc. It is well known in the industry that the demand for ethylene-propylene rubber Mooney used in automotive sealing strips is very high, and The ethylene propylene rubber with too high Mooney will affect the processing of downstream industries, so this kind of ethylene propylene rubber with high Mooney needs to be filled with paraffin oil to reduce the Mooney viscosity without affecting the application, which requires more oil in the production...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/18C08F4/68
CPCC08F210/18C08F4/68
Inventor 王笑海邹向阳金春玉单振国陶青海王萍
Owner PETROCHINA CO LTD
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