Synthesis method of bimodal-distribution ethylene-propylene-nonconjugated diene random copolymer

A non-conjugated diene and bimodal distribution technology is applied in the field of synthesis of bimodal ethylene-propylene-non-conjugated diene random copolymers, which can solve the problems of wide molecular weight distribution of ethylene-propylene copolymers and achieve molecular weight The effect of moderate distribution and high Mooney viscosity

Active Publication Date: 2012-07-11
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Japanese Open Patent Publication No. 61-264035 uses modified vanadium as the main catalyst, alkylaluminum chloride as the co-catalyst, and ethylene, α-olefin and non-conjugated diene as polymerized monomers. For ethylene-propylene copolymers with peak distribution, the modified ligands used are secondary alcohols, but this process has a wider molecular weight distribution for the synthesized ethylene-propylene copolymers

Method used

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  • Synthesis method of bimodal-distribution ethylene-propylene-nonconjugated diene random copolymer
  • Synthesis method of bimodal-distribution ethylene-propylene-nonconjugated diene random copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Synthesis of Modified Vanadium Catalyst

[0031] 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) of vanadyl trichloride into the needle tube, and after stirring for 10 minutes, slowly add 0.0158mol of O-(2-ethylhexyl)-2-ethylhexyl phosphate diluted with 5ml of hexane dropwise, While bubbling high-purity nitrogen gas, the reaction stopped after 30 minutes to obtain a modified vanadium catalyst solution with a concentration of 0.2 mol / L. The reaction vessel was sealed and stored away from light.

Embodiment 2

[0033] Polymerization was carried out in a 5L stainless steel jacketed reactor. Prepare ethylene, propylene, and hydrogen through a mixing device at a ratio of 1:3.2:0.22, and then fully mix them uniformly through a circulating compressor. The polymerization is carried out in a 5L polymerization kettle, which is anhydrous and anhydrous 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 is saturated, then the modified vanadium catalyst hexane solution of 1ml (0.2mmol) is added successively, and sesquialuminum is added, so that the Al / V 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 reactio...

Embodiment 3-6

[0035] Polymerization operation process is identical with embodiment 1, and wherein, embodiment 3,5 adds activator respectively, and the activator dose that embodiment 3,5 adds is 5mL / 1000mL hexane (ETCA / V=3), all the other conditions are shown in table 1, The analysis results are shown in Table 2.

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Abstract

The invention relates to a synthesis method of a bimodal-distribution ethylene-propylene-nonconjugated diene random copolymer, which comprises the following steps: introducing a gas mixture of ethylene, propylene and hydrogen into a reaction kettle, adding a primary catalyst, a cocatalyst and an activating agent, and adding the non-conjugated diene for polymerization at 25-45 DEG C under the pressure of 0.3-0.6 MPa. The propylene/ethylene mol ratio is 1-6; the hydrogen accounts for 0.05-0.5 mol% in the comonomer; the addition amount of the non-conjugated diene in every 1000mL of hexane is 2-10mL; the acidic-phosphate modified vanadium compound is used as the primary catalyst, the halogenated alkyl aluminum is used as the cocatalyst, and the mol ratio of Al in the cocatalyst to V in the primary catalyst is (1-100)/1; the activating agent is ethyl trichloroacetate, and the mol ratio of the activating agent and the vanadium compound is (1-10)/1; and the copolymer has high Mooney viscosity and moderate molecular weight distribution, and is used in processing rubber of automobile seals.

Description

technical field [0001] The invention relates to a method for synthesizing a bimodal distribution ethylene-propylene-non-conjugated diene random copolymer. 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, propylene, 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 role of the main force in the synthesis of ethylene-propylene elastomers. However, the ethylene-propylene rubber synthesized by the catalytic system formed by the above-mentioned main catalyst and co-catalyst is difficult to process in the high Mooney state, so the industry is keen on researching and producing broad-distribution or bimodal distribution ethylene-propylene rubber, and w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/18C08F4/68C08F2/06
Inventor 王笑海张红江金春玉张春英陈可佳陶青海
Owner PETROCHINA CO LTD
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