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Double metal cyanide catalyst preparation method

A double metal cyanide and catalyst technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve problems such as increasing costs, achieve high production efficiency, The effect of short production cycle and low production cost

Active Publication Date: 2013-07-03
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Continuous production of double metal cyanide catalysts can be realized in CN1457928A, but the cycle of production is 36 hours, which greatly increases its cost

Method used

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  • Double metal cyanide catalyst preparation method
  • Double metal cyanide catalyst preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 30 grams of zinc chloride to 225 mL of deionized water, and then add 117 grams of tert-butanol to form a metal salt mixture, marked as S1. Add 12 g of potassium hexacyanocobaltate to 225 mL of deionized water to form an aqueous cyanide solution, labeled S2.

[0025] The rotation speed of the hypergravity reactor was adjusted to 1800rpm and stabilized for 30 minutes. S1 and S2 were pumped from different inlets into the supergravity reactor for mixing at a feed rate of 6 mL / min. At the same time, return the effluent from the supergravity reactor to the reactor, circulate for one hour at a temperature of 10°C, stop the supergravity reactor, and centrifuge the collected white slurry liquid to remove the solvent. Dry under vacuum at 50°C to constant weight to obtain a white powder solid A, which is a double metal cyanide catalyst.

Embodiment 2

[0027] Add 300 grams of zinc chloride to 2250 mL of deionized water, and then add 1170 grams of tert-butanol to form a metal salt mixture, marked as S1. Add 131.6 g of potassium hexacyanoferrate to 2250 mL of deionized water to form an aqueous cyanide solution, labeled S2.

[0028] Adjust the rotating speed of the supergravity reactor to 20000rpm and keep it stable for 40 minutes. S1 and S2 were pumped from different inlets into the supergravity reactor for mixing at a feed rate of 60 mL / min. At the same time, the slip-out liquid in the supergravity reactor is returned to the reactor, circulated for 1.5 hours at a temperature of 30° C., the supergravity reactor is stopped, and the collected white slurry liquid is centrifuged to remove the solvent. Dry to constant weight under vacuum at 50°C, and finally obtain yellow solid powder B.

Embodiment 3

[0030] The water-soluble metal salt of the present embodiment is 35.84 grams of zinc sulfate, and the water-soluble cyanide is 12 grams of potassium hexacyanocobaltate. Others are the same as in Example 1 and are operated according to its process steps to obtain white solid powder C at last.

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Abstract

The invention relates to a double metal cyanide catalyst preparation method, which comprises the following steps: preparing water-soluble metal salt and water to obtain a solution with 0.01-2mol / L, adding alcohol or ether and / or ketone, ester or aldehyde, wherein weight ratio of alcohol or ether to water-soluble metal salt is 0.01-4.0: 1, the weight ratio of ketone, ester or aldehyde to the water-soluble metal salt is 0.01-4.0: 1; preparing water-soluble cyanide and water to obtain a solution with 0.01-2mol / L; respectively sending a metal salt mixed liquor and the cyanide aqueous solution to a rotary hypergravity reactor with rate of 0.1mL / min-60L / min, reacting for 0.6-1.5 hours under temperature condition of 10-50 DEG C; centrifuging and dewatering the obtained material liquid, and drying at 40-50 DEG C under vacuum to constant weight to obtain the double metal cyanide catalyst. The double metal cyanide catalyst preparation method has the advantages of simple technology and high production efficiency, and is suitable for continuous industrialization production.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of a high-activity double metal cyanide catalyst used for synthesizing polyether polyols. Background technique [0002] Double metal cyanide catalysts are usually composed of metal salts, metal cyanides and complexes, with M a 1 [M 2 (CN) b ] d ·xM 3 (X) c ·L1·L2·wH 2 The structure of O, where M 1 , M 2 , M 3 is a transition metal; L1, L2 are organic complexing agents; a, b, c, d are integers, and satisfy charge balance. Double metal cyanide catalysts can be used for the homopolymerization of compounds such as carbon dioxide, alkylene oxide, and cyclic anhydrides, or through copolymerization to prepare high molecular polymers such as polyether polyols and polyesters. In particular, it has been widely used in the preparation of polyether polyols. [0003] At present, in the reports on the preparation methods of double metal cyanide catalysts, i...

Claims

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Application Information

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IPC IPC(8): C07F19/00B01J31/22C07C43/13C07C41/03C08G65/28
Inventor 程亮张东恒魏观为翟月奎
Owner PETROCHINA CO LTD
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