Synthesis method of bimodal-distribution ethylene-alpha-alkene-non-conjugated dialkene random copolymer

A non-conjugated diene, ethylene-propylene copolymer technology is applied in the field of synthesis of bimodal ethylene-α-olefin-non-conjugated diene random copolymers, and can solve the tunability of ethylene-propylene copolymer monomers It is not as good as other problems to achieve the effect of moderate molecular weight distribution and high Mooney viscosity

Active Publication Date: 2010-09-22
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Japanese Open Patent Gazette No. 57-131212 uses ethylene, α-olefin and non-conjugated diene as polymerized monomers, uses alkylaluminum chloride as cocatalyst, and vanadyl trichloride as main catalyst, and synthesizes a compound with An ethylene-propylene copolymer with excellent processability, but the main catalyst used is vanadyl trichloride; Japanese Patent Publication No. 61-264035 uses modified vanadium as the main catalyst and alkyl aluminum chloride as a cocatalyst, and ethylene, α- Olefins and non-conjugated diolefins are polymerized monomers. A single-pot polymerization process is used to synthesize ethylene-propylene copolymers with bimodal ...

Method used

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  • Synthesis method of bimodal-distribution ethylene-alpha-alkene-non-conjugated dialkene random copolymer
  • Synthesis method of bimodal-distribution ethylene-alpha-alkene-non-conjugated dialkene random copolymer
  • Synthesis method of bimodal-distribution ethylene-alpha-alkene-non-conjugated dialkene random copolymer

Examples

Experimental program
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Embodiment 1

[0032] Synthesis of Soluble Vanadium Complex Catalyst

[0033] Take a 100ml bottle with an inlet tube at the bottom, two-corner ground mouth bottle, conduct anhydrous and anaerobic treatment under vacuum and heating, then add 50ml of dry hexane, inject high-purity nitrogen for bubbling, and then use dry medical glass Add 1ml (0.0105mol) vanadyl trichloride into the needle tube, stir for 10 minutes, then slowly drop in 0.0158mol of di-isooctyl phosphate diluted with 5ml of hexane, while bubbling high-purity nitrogen gas, the reaction stops after 30 minutes , to obtain a soluble vanadium complex catalyst solution with a concentration of 0.2 mol / L, seal the reaction vessel and store it away from light.

Embodiment 2

[0035]The preparation of high molecular weight partial ethylene-propylene copolymer is carried out in the first reactor. Prepare ethylene, propylene, and hydrogen through a mixing device at a ratio of 1:2:0.15, and then fully mix them evenly through a circulating compressor. Oxygen treatment for 1 hour, the inert gas used is high-purity nitrogen, then add 2000ml of dry hexane (water content≤10ppm) to it, which contains 4ml of norbornene (ENB), open the circulation compressor, and feed into the polymerization tank Mixed gas, the mixed gas flow rate is 150L / hour, the mixed gas dissolved in hexane reaches saturation, then add 1ml (0.2mmol) of soluble vanadium complex catalyst hexane solution successively, add sesquialuminum, make Al / V The ratio is 10 / 1, the polymerization temperature is 30°C, the polymerization pressure is 0.5MPa, and the polymerization reaction time is 1 hour. After the polymerization reaction is completed, the glue is released from the bottom pipe of the polyme...

Embodiment 3-6

[0039] The polymerization operation process is the same as in Example 1, and the other conditions are shown in Table 1, and the analysis results are shown in Table 2. The blending results are shown in Table 3.

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Abstract

The invention relates to a synthesis method of a bimodal-distribution ethylene-alpha-alkene-non-conjugated dialkene random copolymer. The method comprises the following steps: a high-molecular weight part ethylene-propylene copolymer is synthesized from ethylene, propylene and hydrogen (the mol ratio is 1:1.0-3.0:0.15-0.30) and ethidene norbornylene 2-5 mL/L hexane; a low-molecular weight part ethylene-propylene copolymer is synthesized from the ethylene, the propylene and the hydrogen (the mol ratio is 1:3.0-4.5:0.9-2.0) and ethidene norbornylene 8-12 mL/L hexane; the main catalyst is soluble vanadium complex, and the cocatalyst is ethylaluminium sesquichloride; the mol ratio of Al to V is 1-100; the activating agent for the low-molecular weight part is ethyl trichloroacetate; and the mass ratio of the high-molecular weight part ethylene-propylene copolymer to the low-molecular weight part ethylene-propylene copolymer is 80/20-40/60. The copolymer has the advantages of high Mooney viscosity and moderate molecular weight distribution, and can be used for processing rubber for automobile gland strips.

Description

technical field [0001] The invention relates to a method for synthesizing a bimodal distribution ethylene-alpha-olefin-non-conjugated diene random copolymer. The bimodal distribution ethylene-alpha-olefin-non-conjugated diene random copolymer synthesis method uses a soluble vanadium catalyst as the main catalyst, an alkylaluminum halide as a co-catalyst, and is completed in the form of solution polymerization by blending high and low molecular weights , so that the synthesized copolymer rubber has excellent processing performance. Background technique [0002] It is a well-known method in the industry that vanadium system Ziegler-Natta catalysts are used for ternary copolymerization of ethylene, α-olefins, and non-conjugated dienes to prepare rubber elastomers. Representative main catalysts such as VOCl 3 ,, VCl 3 ,, VCl 4 ,, V(acac) 3 etc., the other component is the I-III group organometallic compound (such as alkylaluminum), these V-alkylaluminum systems play the rol...

Claims

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Application Information

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IPC IPC(8): C08F210/18
Inventor 王笑海邹向阳张红江金春玉陶青海东升魁刘洪伟王积悦杜鹃董颖周叔花于敛曼
Owner PETROCHINA CO LTD
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