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

A non-conjugated diene, bimodal distribution technology, applied in the field of synthesis of bimodal distribution ethylene-propylene-non-conjugated diene random copolymers, can solve the problem 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: 2013-11-06
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 Catalysts

[0031] Take a 100ml bottle with an air inlet pipe at the bottom, and carry out anhydrous and oxygen-free treatment in a vacuum and heating state, then add 50ml of dry hexane, pass high-purity nitrogen for bubbling, and then use dry medical glass Add 1 ml (0.0105 mol) of vanadium oxychloride into the syringe, and after stirring for 10 minutes, slowly add 0.0158 mol of O-(2-ethylhexyl)-2-ethylhexyl phosphate diluted with 5 ml of hexane, while adding dropwise, While blowing high-purity nitrogen gas, the reaction was stopped after 30 minutes, and a modified vanadium catalyst solution with a concentration of 0.2 mol / L was obtained, and the reaction vessel was closed and stored in the dark.

Embodiment 2

[0033] The polymerization was carried out in a 5L stainless steel jacketed reactor. Ethylene, propylene and hydrogen are prepared by mixing device at 1:3.2:0.22, and then fully mixed by circulating compressor. The polymerization is carried out in a 5L polymerization kettle. Oxygen was treated for 1 hour, the inert gas used was high-purity nitrogen, and then 2000ml of dry hexane (water ≤ 10ppm) was added to it, which contained 4ml of norbornene (ENB), the circulating compressor was turned on, and the polymerization kettle was fed Mixed gas, the mixed gas flow rate is 150L / hour, the mixed gas dissolved in hexane is saturated, then 1ml (0.2 mmol) of modified vanadium catalyst hexane solution is added successively, sesquialuminum is added, and the Al / V ratio is 10 / 1, the polymerization temperature is 30 °C, the polymerization pressure is 0.5 MPa, and the polymerization reaction time is 1 hour. After the polymerization reaction is completed, the glue solution is released from the b...

Embodiment 3-6

[0035] The polymerization operation process is the same as that of Example 1, wherein the activator was added in Examples 3 and 5 respectively, and the activator dose added in Examples 3 and 5 was 5mL / 1000mL hexane (ETCA / V=3), and the remaining conditions were 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] The use of vanadium system Ziegler-Natta catalyst for terpolymerization of ethylene, propylene and non-conjugated diene to prepare rubber elastomer is a well-known method in the industry. Representative main catalysts such as VOCl 3 ,, VCl 3 , VCl 4 ,, V(acac) 3 etc., another component is group I-III organometallic compounds (such as alkyl aluminum), these V-alkyl aluminum systems have played a major role 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 to study the production of broad-distributed or bimodal ethylene-propylene rubber, while the broad-distributed ethylene-propylene r...

Claims

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Application Information

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Patent Type & Authority Patents(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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