Bimetallic cyanide complex catalyst and its prepn process

A catalyst and cyanide technology, which is applied in the field of catalysts for ring-opening polymerization of epoxy compounds and its preparation, can solve the problems of increasing post-processing procedures and hindering applications, and achieve the effects of eliminating loading procedures, narrow molecular weight distribution and high activity

Inactive Publication Date: 2006-03-01
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the activity of these supported catalysts is higher than that of unsupported catalysts, the mass fraction of the carrier is usually more than 90%, resulting in a total catalyst consumption of 1000 × 10 -6 Above the mass fraction, the catalyst must be removed from the polyether after polymerization, which increases the post-treatment process and hinders its application in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1 Calcium Sulfate Suspension Technology Preparation Catalyst

[0046] Solution A: 20g zinc chloride, 30ml tert-butanol, 30ml deionized water, mix and stir to completely dissolve the solid.

[0047] Solution B: 8gK 3 Co(CN) 6 , 150ml deionized water, mix and stir to dissolve the solid completely.

[0048]In a 1000ml three-neck flask, add 20g of 40% calcium chloride aqueous solution and 30g of 25% zinc sulfate aqueous solution to react to form a suspension, then add solution A, stir evenly, and add solution B dropwise at 40°C. After the dropwise addition, add 250ml of 50% tert-butanol aqueous solution, then raise the temperature to 70°C and keep it for 1h, cool down to 35°C, add 2g of diethylene glycol dibenzoate, disperse evenly, and filter. The filter cake was redispersed in 250 ml of 70% tert-butanol aqueous solution, 2 g of diethylene glycol dibenzoate was added, dispersed evenly, and filtered. The filter cake was then dispersed in 250ml of tert-butanol, a...

Embodiment 2

[0051] Example 2 Preparation of catalyst by calcium sulfate co-precipitation process

[0052] Solution 1: 8gK 3 Co(CN) 6 , 5g magnesium sulfate, 150ml deionized water, mix and stir to completely dissolve the solid.

[0053] Solution 2: 20g zinc chloride, 8g calcium chloride, 30ml tert-butanol, 30ml deionized water, mix and stir to completely dissolve the solid.

[0054] In a 1000ml three-necked flask, solution 2 was added, and solution 1 was added dropwise at 40°C. After the dropwise addition, add 250ml of 50% tert-butanol aqueous solution, then raise the temperature to 70°C and keep it for 1h, cool down to 35°C, add 2g of dipropylene glycol dibenzoate, disperse evenly, and filter. The filter cake was redispersed in 250 ml of 70% tert-butanol aqueous solution, 2 g of dipropylene glycol dibenzoate was added, dispersed evenly, and filtered. The filter cake was then dispersed in 250ml of tert-butanol, and 1g of dipropylene glycol dibenzoate was added, dispersed evenly, and fi...

Embodiment 3

[0057] Embodiment 3 Barium sulfate suspension process prepares catalyst

[0058] Solution A: 20g zinc chloride, 30ml tert-butanol, 30ml deionized water, mix and stir to completely dissolve the solid.

[0059] Solution B: 8gK 3 Co(CN) 6 , 150ml deionized water, mix and stir to dissolve the solid completely.

[0060] In a 1000ml three-necked flask, add 20g concentration of 30% barium chloride solution and 14g concentration of 25% zinc sulfate solution to react the precipitate suspension, then add solution A, stir evenly, and add solution B dropwise at 40°C. After the dropwise addition, add 250ml of 50% tert-butanol aqueous solution, then raise the temperature to 70°C and keep it for 1h, cool down to 35°C, add 2g of dimethoxyethyl phthalate, disperse evenly, and filter. The filter cake was redispersed in 250 ml of 70% tert-butanol aqueous solution, 2 g of dimethoxyethyl phthalate was added, dispersed evenly, and filtered. The filter cake was dispersed in 250ml of tert-butanol...

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PUM

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Abstract

The present invention discloses one kind of bimetallic cyanide complex catalyst and its preparation process. The bimetallic cyanide complex catalyst contains calcium sulfate, barium sulfate, etc. in 5-50 wt% to act as carrier. Compared with traditional similar catalyst, the present invention has less consumption and simple preparation process. When it is used in synthesizing polyether, the synthesized polyether has narrow molecular weight distribution and lower unsaturation degree. The catalyst of the present invention may be used in synthesizing polyether, polyether ester, etc. and is suitable for intermittent, semi-continuous and continuous synthesis process.

Description

technical field [0001] The invention relates to a catalyst for ring-opening polymerization of epoxy compounds and a preparation method thereof. Background technique [0002] Double metal cyanide complex catalysts (hereinafter referred to as DMC catalysts) are usually precipitated double metal complexes coordinated by cyanide. Commonly used double metal cyanide complexes include zinc hexacyanocobaltate, zinc hexacyanoferrate (2 or 3 valence), zinc tetracyanonickelate, zinc hexacyanoiridate and zinc replaced by iron, cobalt, nickel, etc. Precipitation of cyanide complexes. When this simple double metal cyanide complex is used as a catalyst, the activity is very low. When other ligands such as some metal halides and organic ligands are added to the DMC catalyst, its catalytic activity can be improved. [0003] Making the catalyst into a supported catalyst can further enhance the activity of the catalyst and improve the quality of the synthesized polyether. Many scholars have ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/04
Inventor 周集义王文浩王建伟李俊贤李新豪常伟林贾利亚
Owner LIMING RES INST OF CHEM IND
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