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Preparing technology for production of EPT rubber vanadium catalyst

A kind of EPDM rubber and catalyst technology, which is applied in the field of preparation of vanadium-based catalysts, can solve the problems of small organic phase operation capacity, low vanadium concentration, and no industrial preparation significance, and overcome the high sensitivity and high temperature of water and air. Catalytic activity, environmental protection effect

Inactive Publication Date: 2005-02-23
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these works only use the extraction of vanadium compounds as a separation method in hydrometallurgy and analytical chemistry, not for the purpose of preparing vanadium compounds, and the organic phase used has a small operating capacity and low vanadium concentration, which is not meaningful for industrial preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 200mlH to a 1L beaker 2 O, 23.3g of solid NaOH was stirred to dissolve and heated to near boiling. In addition, 49.5g of V with a purity ≥ 99% 2 o 5 with 100mlH 2 O into a slurry, slowly poured into the NaOH solution, and stirred for about 20 minutes. A small amount of insoluble matter was filtered off and washed with 1N H 2 SO 4 Adjust the pH value of the aqueous solution to 8.28 with H 2 O diluted to 1000ml. Sampling, with (NH 4 ) 2 Fe(SO 4 ) 2 Standard solution titration, V (V) concentration is 0.533mol / L.

[0024] In a 20ml separatory funnel, add 10ml of di(2-ethylhexyl)phosphoric acid (hereinafter referred to as P204) and hexane mixed solution of 2-ethylhexanoic acid with a total concentration of 1.034mol / L respectively, wherein the concentration of P204 is 0.8mol / L, the concentration of 2-ethylhexanoic acid is 0.234mol / L, 5ml of the above-prepared V(V) raw material solution with a concentration of 0.533mol / L, and mix for 5 minutes. Add 3ml of 1N ...

Embodiment 2

[0029] 3.5g solid Na 2 CO 3 Add 125ml H 2 O is heated to dissolve and heated to boiling. Also known as 3.5g V 2 o 5 with 30mlH 2 O into a slurry. The preparation method of the following V(V) catalyst is the same as in Example 1, and finally a V(V) catalyst hexane solution with a concentration of 0.10 mol / L is obtained.

[0030] The polymerization method was the same as in Example 1. The polymer was analyzed: the propylene content was 37.4%, the iodine value was 9.5, and the intrinsic viscosity measured at 135° C. was 1.29 dl / g with decahydronaphthalene as the solvent.

Embodiment 3

[0032] Will 102.6g V 2 o 5 Add 100ml H 2 O into a paste. Another 100g oxalic acid H 2 C 2 o 4 2H 2 O was dissolved in 200ml of hot water.

[0033] Add 50mlH to a 1L beaker 2 O, slowly add 62ml of concentrated sulfuric acid, stir and heat to boiling. Slowly add V alternately 2 o 5 Serum and H 2 C 2 o 4 solution, stirred at 95°C for 60 minutes, and filtered off a small amount of insoluble matter to obtain VOSO 4 solution. with H 2 O diluted to 1000ml with KMnO 4 -(NH 4 ) 2 Fe(SO 4 ) 2 Standard solution oxidation-reduction titration, V(IV) concentration is 1.0mol / L, PH=0.5.

[0034] Add 92ml of di(2-ethylhexyl) phosphoric acid (hereinafter referred to as P204) and hexane mixed solution of 2-ethylhexanoic acid with a total concentration of 1.205mol / L in the separating funnel, wherein 2-ethylhexanoic acid is The proportion is 25 mol%, and NaOH aqueous solution is added to adjust the pH of the organic phase to 7.0. Add 110 ml of the V(IV) raw material solution...

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PUM

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Abstract

Ternary rubber vanadium series catalysts are prepared by: taking the V2O5, NaVO3 ore as start materials, organic phosphorus monoacid as extracting reagent, fatty carboxylic acid being as aided extracting reagent, and saturated alkane as solvent. By cross current extracting method, stable saturated alkane vanadium (IV) or vanadium (V) compounds used as catalyst for EPDM production directly can be obtained. This invention has the features of preparation simple, condition moderation, low cost, large scale production, without toxic and harm chlorine, good for environment protection. The prepared catalyst saturated alkane solution is high homogeneous stability, and non-sensitive to water and air ,which overcomes shortages of present catalysts sensitive to water and air, meanwhile, reduces the storing and transporation cost. The catalysts prepared has higher catalyzed activity than catalyst VOCl3, and the obtained rubber having similar molecular chain structure, monomer unit sequence structure and third monomer contents.

Description

technical field [0001] The invention belongs to a preparation technology of vanadium series catalyst used for producing ethylene-propylene-non-conjugated diene copolymer. Background technique [0002] The production of ethylene-propylene rubber at home and abroad mostly uses vanadium compounds as catalysts, and these vanadium compounds are limited to VX 3 , VX 4 , VOX 3 and VO(OR) 3-n x n , X is a halogen, mainly a chlorine atom, R is an alkyl group of 6-12 carbons, n is an integer of 0-2, wherein VOCl 3 and VO(OR) 3 It is the most commonly used catalyst in industrial production. Its main patent is VCl 3 (US Patent US5,367,037), VCl 4 (US Patents US5,367,037, US4,078,131), VOCl 3 (US Patents US5,367,037, US4,078,131) and VO(OR) 3-n Cl n (US Patents US3,173,903, US4,259,468). [0003] VCl 3 , VCl 4 and VOCl 3 by V 2 o 5 It is produced by high-temperature chlorination, and the large-scale use of chlorine gas not only damages the health of operators, but also c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/76C08F210/18
Inventor 张学全姜连升万雄李继文曹丽辉高巍
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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