Preparation method of double-metal cyanidation complex catalyst

A double metal cyanation and complex technology, which is applied in the field of preparing double metal cyanide complex catalysts, can solve the problems of cumbersome process, high cost, easy introduction of unstable factors and the like, and achieves simplified preparation process and reduced cost , the effect of shortening the preparation cycle

Active Publication Date: 2012-10-17
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This preparation method is cumbersome, the preparation cycle is long, and instability factors are easily introduced.
At the ...

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  • Preparation method of double-metal cyanidation complex catalyst
  • Preparation method of double-metal cyanidation complex catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A double metal cyanide complex catalyst is prepared by the following steps:

[0035] (1) 0.01mol potassium cobaltcyanide is dissolved in 50mL water to obtain potassium cobaltcyanide solution, and 0.037mol zinc chloride is dissolved in the mixed solution of 150mL water and 75mL tert-butanol to obtain zinc chloride solution; under vigorous stirring , the potassium cobalt cyanide solution was slowly dropped into the zinc chloride solution, and the dripping was completed in 30 minutes, and then 0.03mol 18-crown-6 was added, and the vigorous stirring was continued for 5 hours;

[0036] (2) Centrifuge the precipitate, grind the resulting precipitate in a ball mill and liquefy the slurry with a mixture of 125mL tert-butanol and 125mL water, stir and keep it warm for 1h; 1h;

[0037] (3) Centrifuge and precipitate the slurry with pure tert-butanol and stir for 1 h, centrifuge and separate the precipitate; dry the precipitate in a vacuum oven at 45° C. for 15 h to obtain a whit...

Embodiment 2

[0041] A kind of preparation method of double metal cyanide complex catalyst, its raw material and operation are the same as embodiment 1, just do not add 18-crown ether-6 from beginning to end. By elemental analysis (see Table 2) and infrared spectroscopy (see figure 2 ) determined that the double metal cyanide complex catalyst obtained at last consists of Zn 3 [Co(CN) 6 ] 2 1.6ZnCl 2 1.1t-BuOH 1.8H 2 O.

[0042] The elemental analysis result of the double metal cyanide complex catalyst that table 2 embodiment 2 obtains

[0043] Element mass fraction (%)

Embodiment 3

[0045] Under nitrogen protection, 7 mg of the catalyst obtained in Example 1 and 24.9 g of propylene oxide were added to a fully dried 130 ml autoclave, filled with 18 g of carbon dioxide, and the temperature was raised to 80°C. React 15h under stirring condition and emit product, vacuum removes unreacted propylene oxide, obtains polycarbonate polyalcohol 28.7g, test result shows that carbonate bond content is 44% in the product, and by-product (cyclic carbonate) content is 3%. The catalytic efficiency is about 4100g / g.

[0046] Under nitrogen protection, 7 mg of the catalyst obtained in Example 2 was added to a fully dried 130 ml autoclave, and then 24.9 g of propylene oxide was added, 18 g of carbon dioxide was charged, and the temperature was raised to 80° C. React 15h under stirring condition and emit product, vacuum removes unreacted propylene oxide, obtains the very high polycarbonate polyol 26.8g of viscosity, test result shows that carbonate bond content is 35% in the...

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Abstract

The invention discloses a preparation method of a double-metal cyanidation complex catalyst. The method comprises the steps that: a metal cyanide aqueous solution is added into a metal salt solution; crown ether is added and a reaction is carried out; an obtained precipitate is separated by centrifugation; the precipitate is grinded, an organic ligand/water mixed liquid is used for pulping and washing the precipitate; a precipitate is then obtained by centrifugation; puling washing and centrifugation are repeated once or twice; an organic ligand is added into an obtained precipitate for pulping, and a precipitate is separated by centrifugation again; the precipitate is dried, such that the double-metal cyanidation complex catalyst is obtained. With the preparation method provided by the invention, a preparation period is substantially reduced; dosages of the metal salt and the ligand are greatly reduced; and the cost is reduced. The catalytic efficiency of the double-metal cyanidation complex catalyst provided by the invention is equal to a double-metal cyanidation complex catalyst prepared by prior art, but is higher than a catalyst which is not prepared by using crown ether under same conditions. The carbonate bond content of a polymer obtained under the catalytic effect of the double-metal cyanidation complex catalyst provided by the invention is higher than that of the catalyst which is not prepared by using crown ether. Also, the high catalytic performance of the catalyst provided by the invention make the catalyst suitable for the productions of polyether glycol.

Description

technical field [0001] The invention relates to a method for preparing a double metal cyanide complex catalyst (DMC). Background technique [0002] The catalyst systems that can be catalyzed and copolymerized to prepare polycarbonate polyols found at present are: metal acetate (K.Soga et al, Makromol.Chem., 1978,179,2837), porphyrin aluminum catalyst system (S.Inoue ct al., Macromol., 1986.19, 8) and polymer-loaded bimetallic complexes (Chen Liban, CN 1032010C), etc., but these systems all have many shortcomings, and the catalytic yield of metal acetate is relatively low. The cost of porphyrin aluminum catalyst is high and it is not suitable for industrial production. The carbonate bond content of the catalytic product of the high polymer supported bimetallic catalyst system is generally lower than 30%, and the lower carbonate bond content makes it closer to polyether than polycarbonate. [0003] Since the 1980s, double metal cyanide complex catalysts have been used to cat...

Claims

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Application Information

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IPC IPC(8): C08G64/34C08G65/04
Inventor 张敏杨永
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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