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Multi-metal cyanide complex catalyst and preparation thereof

A cyanide and catalyst technology, applied in the field of multimetal cyanide complex catalysts and their preparation, can solve the problems of reduced catalyst activity, complex preparation process, and high toxicity of cadmium ions, and achieve low unsaturation and short induction period , The effect of short polymerization induction period

Inactive Publication Date: 2005-12-21
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent No. 5,998,327 mentions the use of part of cadmium chloride instead of zinc chloride synthesis catalyst, and the polyether synthesized by the catalyst has a narrower molecular weight distribution, but the cadmium ion is highly toxic and difficult to use
Chinese patent application CN1459332 proposes to introduce 1% to 20% of nickel hexacyanocobaltate, iron hexacyanocobaltate, zinc hexacyanoferrate or nickel hexacyanocobaltate synthesis catalyst into the traditional zinc hexacyanocobaltate catalyst, but these substances The upper limit of the content is strictly limited, and more nickel hexacyanocobaltate, iron hexacyanocobaltate, zinc hexacyanoferrate or nickel hexacyanoferrate will significantly reduce the activity of the catalyst
In U.S. Patent No. 5,952,261, calcium chloride is used to partially replace zinc chloride to synthesize a calcium-containing cyanide complex catalyst, and the catalyst activity is improved, but the preparation process is complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The polymetallic catalyst of embodiment 1 tert-butanol-polypropylene oxide polyether coordination

[0033] Solution A: 8.7g manganese chloride tetrahydrate, 15g zinc chloride, 30ml tert-butanol, 30ml deionized water, mix and stir to completely dissolve the solid.

[0034] Solution B: 8g potassium hexacyanocobaltate, 150ml deionized water, mix and stir to completely dissolve the solid.

[0035] In a 1000ml three-necked flask, add solution A, and add solution B dropwise at 40°C. After the dropwise addition, add 250ml of 50% tert-butanol aqueous solution, raise the temperature to 70°C and keep it for 1h, cool down to 35°C, add 2g of polypropylene oxide polyether (referred to as PPG) with a molecular weight of 4000, and disperse Homogenize and filter. The filter cake was redispersed in 250 ml of 70% tert-butanol aqueous solution, 2 g of two-functional polypropylene oxide polyether with a molecular weight of 4000 was added, dispersed evenly, and filtered. Disperse the fil...

Embodiment 2 4

[0038] Example 2 tetracyanonickelate modified tert-butanol-polypropylene oxide polyether coordination multimetal catalyst

[0039] Solution A: 8.6g manganese chloride tetrahydrate, 15g zinc chloride, 30ml tert-butanol, 30ml deionized water, mix and stir to completely dissolve the solid.

[0040] Solution B: 6g potassium hexacyanocobaltate, 2g potassium tetracyanonickelate, 150ml deionized water, mix and stir to completely dissolve the solid.

[0041]In a 1000ml three-necked flask, add solution A, and add solution B dropwise at 40°C. After the dropwise addition, add 250ml of 50% tert-butanol aqueous solution, raise the temperature to 70°C and keep it for 1h, cool down to 35°C, add 2g of two-functional polypropylene oxide polyether with a molecular weight of 4000 (referred to as PPG) and disperse evenly ,filter. The filter cake was redispersed in 250 ml of 70% tert-butanol aqueous solution, 2 g of two-functional polypropylene oxide polyether with a molecular weight of 4000 was...

Embodiment 3 4

[0044] Example 3 Tetracyanonickelate-modified tert-butanol-polytetrahydrofuran oxirane copolyether coordination multimetal catalyst

[0045] Solution A: 10.3g manganese chloride tetrahydrate, 14g zinc chloride, 30ml tert-butanol, 30ml deionized water, mix and stir to completely dissolve the solid.

[0046] Solution B: 6g potassium hexacyanocobaltate, 2g potassium tetracyanonickelate, 150ml deionized water, mix and stir to completely dissolve the solid.

[0047] In a 1000ml three-necked flask, add solution A, and add solution B dropwise at 40°C. After the dropwise addition, add 250ml concentration of 50% tert-butanol aqueous solution, raise the temperature to 70°C and keep it for 1h, cool down to 35°C, add 2g polytetrahydrofuran-ethylene oxide (mol ratio is 1 : 1) Copolyether (referred to as PET), disperse evenly, and filter. The filter cake was redispersed in 250 ml of 70% tert-butanol aqueous solution, and 2 g of bifunctional polytetrahydrofuran ethylene oxide copolyether w...

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PUM

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Abstract

The invention discloses a kind of polymetallic cyanide complex compound catalyst and its preparation. Its skeleton structure contains several kinds of elements as zinc, manganese, cobalt and nickel. The catalyst of the invention is prepared by the mix solution of water-soluble zinc and manganic salts reacting with water-soluble cyaniding metal acid salts, organic ligand and functional polymer. When sythensizing catalyst through replacing hexacyanocobaltate with mix cyaniding metal acid salts of tetraacyanonickelate / hexacyanocobaltate, the properties of catalyst have no remarkable change, but the cost has been reduced, and the tetraacyanonickelate can replace 50% of the hexacyanocobaltate at most. The catalyst of the invention has short inductive period, and can be used to synthesize polyether, polyester, poly(ester ether) and poly(carbonic ether).

Description

technical field [0001] The invention relates to a catalyst for the polymerization of epoxy compounds and a preparation method thereof. Background technique [0002] Double metal cyanide complex catalyst (hereinafter referred to as DMC catalyst) is a catalyst developed by the American General Rubber Tire Company in the 1960s for the ring-opening polymerization of epoxides, cyclic anhydrides and episulfides. At present it is mainly used in the preparation of polyether polyols by ring-opening polymerization of epoxides. Compared with traditional basic catalysts (such as KOH, NaOH, etc.), DMC catalysts have higher activity, and the synthesized polyether polyols have higher molecular weight, lower unsaturation and narrower molecular weight distribution. It can be used in coatings, fibers, adhesives, elastomers, foams, surfactants and lubricants, etc. [0003] The DMC catalyst is usually a cyanide-coordinated double metal complex precipitate. Commonly used double metal cyanide ...

Claims

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Application Information

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IPC IPC(8): C08G59/68
Inventor 周集义王文浩王建伟李俊贤李新豪贾利亚
Owner LIMING RES INST OF CHEM IND