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Ethylene Propylene Rubber Polymerization Catalyst Deactivation Method

A technology of polymerization catalyst and ethylene propylene rubber, which is applied in the field of deactivation of ethylene propylene rubber polymerization catalyst, can solve the problems of low catalyst removal efficiency, high reaction temperature and pressure, and high catalyst residual amount, and achieves fast deactivation reaction speed and high reaction temperature. And the effect of low pressure and high vanadium removal efficiency

Active Publication Date: 2019-05-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst deactivation process commonly used in domestic ethylene-propylene rubber equipment uses methanol or water as the deactivation reagent. The methanol deactivation process requires high reaction temperature and pressure, and then multi-stage alkaline washing is required to completely remove the catalyst in the glue. , and the water deactivation process has a low removal efficiency of the catalyst in the EPDM rubber glue, and is prone to water washing and emulsification, which eventually leads to a high catalyst residue in the glue, which affects product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1.5L solid content is 6.0% polymerized glue (glue containing catalyst) into the reaction flask, stirred and kept at 70 ° C, gradually added dropwise 0.5% sodium methoxide (methanol) solution 40 milliliters (equivalent to 3.0 times of the main / co-catalyst consumption), the dropwise addition time is 30 minutes, after the dropwise addition, continue to stir for 20 minutes, stand still for 30 minutes, and get the glue solution for analysis. The analysis results show that the vanadium content is less than 40ug / g, and the aluminum content is less than 45ug / g.

[0022] Add 1.5L of desalinated water to the above static glue, continue to keep the temperature at 70°C, stir for 20 minutes, and stand for 20 minutes to separate layers. After washing with desalted water, the glue will separate quickly, the interface is clear, and the pH value of the upper glue is 7. Between ~8, the glue solution was taken for analysis. The vanadium content is less than 8ug / g, and the aluminum conten...

Embodiment 2

[0024] Add 1.5L of polymerized glue (glue containing catalyst) with a solid content of 6.0% into the reaction flask, stir and keep the temperature at 40°C, gradually add 9 milliliters of 3.0% sodium ethylate (ethanol) solution dropwise (equivalent to 4.0 times of main / co-catalyst consumption), the dropping time is 30 minutes, after dropwise addition, continue to stir for 60 minutes, stand still for 90 minutes, and get the glue solution for analysis. The analysis results showed that the vanadium content was less than 43ug / g, and the aluminum content was less than 49ug / g.

[0025] Add 1.5L of desalinated water to the above-mentioned static glue, continue to keep the temperature at 40°C, stir for 60 minutes, and stand for 60 minutes to separate layers. After washing with desalted water, the glue is separated quickly, the interface is clear, and the pH value of the upper layer of glue is 7. Between ~8, the glue solution was taken for analysis. The vanadium content is less than 10...

Embodiment 3

[0027] Add 1.5L of polymerized glue (glue containing catalyst) with a solid content of 6.0% into the reaction flask, stir and keep the temperature at 60°C, and gradually add 23 milliliters of 1.0% sodium methylate (methanol) solution dropwise (equivalent to 3.5 times of main / co-catalyst consumption), the dropping time is 30 minutes, continue to stir for 30 minutes after dropping, stand still for 60 minutes, and get the glue solution for analysis. The analysis results showed that the vanadium content was less than 41ug / g, and the aluminum content was less than 44ug / g.

[0028] Add 1.5L of desalinated water to the above static glue, continue to keep the temperature at 60°C, stir for 30 minutes, and stand for 30 minutes to separate layers. After washing with desalted water, the glue will separate quickly, the interface is clear, and the pH value of the upper glue is 7. Between ~8, the glue solution was taken for analysis. The vanadium content is less than 9ug / g, and the aluminum...

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Abstract

The invention provides a polymerization catalyst deactivation method for ethylene propylene rubber. The polymerization catalyst deactivation method comprises the following steps: (1) adding a catalyst containing rubber solution obtained by a polymerization reaction into a reaction flask, carrying out stirring at a constant temperature, gradually dropwise adding a methanol or ethanol solution containing a deactivator, continuing stirring, and carrying out standing; and (2) adding desalted water into the rubber solution obtained after standing in the step (1), continuing stirring at a constant temperature, carrying out standing and stratification until the pH value of a supernatant rubber solution is in a range of 7 to 8, and subjecting the rubber solution to analyzing.

Description

technical field [0001] The invention relates to a method for deactivating an ethylene-propylene rubber polymerization catalyst. Background technique [0002] The industrial production process of solution method EPDM rubber generally uses ethylene, propylene and non-conjugated dienes as raw materials, uses Ziegler-Natta's vanadium or titanium compounds as the catalytic system, and saturated hydrocarbon solution as the solvent. Carrying out continuous polymerization is the basic process. The main disadvantage of this process is that the utilization rate of the catalyst is not high, the catalytic efficiency is low, and the content of catalyst residue in the polymerization product is relatively high. If the catalyst residues (vanadium, ash, chloride) are not removed, first, it will affect the electrical insulation performance of ethylene propylene rubber; second, it will seriously affect the thermal stability and aging resistance of ethylene propylene rubber; Contains chlorine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F6/08C08F210/18
CPCC08F6/08C08F210/18
Inventor 王刚杜娟单振国郑翔王萍张春英杨博刘振国宫立波
Owner PETROCHINA CO LTD
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