Preparation method for double metal cyanide catalyst for polycarbonate synthesis

A double metal cyanide and catalyst technology, applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of low unit content, low activity and long reaction time and other problems, to achieve performance improvement, high catalytic efficiency, and solve the effect of long reaction time

Active Publication Date: 2011-09-14
HEBEI UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is for low activity, long reaction time, CO 2 Defects such as low unit content provide a method for preparing a double metal cyanide catalyst for polycarbonate synthesis. The double metal catalyst prepared by this method can catalyze CO with high activity. 2 Copolymerized with epoxide, the activity reached more than 30kg polymer / g catalyst within 4 hours of reaction, and the CO in the obtained polycarbonate 2 The content of the unit reaches about 0.45 (the CO in the completely alternating copolycarbonate 2 The content of the unit is 0.5)

Method used

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  • Preparation method for double metal cyanide catalyst for polycarbonate synthesis
  • Preparation method for double metal cyanide catalyst for polycarbonate synthesis
  • Preparation method for double metal cyanide catalyst for polycarbonate synthesis

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Preparation of DMC-1 containing only tert-butanol ligand:

[0038] (1) will 1×10 -1 Add 50ml of tert-butanol (t-BuOH) in a beaker to 50ml of zinc chloride, stir until the zinc chloride is completely dissolved, then add 300ml of deionized water (solution 1). Will 2.5×10 -2 mol of potassium hexacyanocobaltate was dissolved in 250 ml of deionized water in a second beaker (Solution 2).

[0039] (2) Add solution 2 dropwise to solution 1 under the condition of rapid stirring at 30° C., and the dropping time is controlled at 30-60 minutes. After the dropwise addition, continue to stir for 1 hour to obtain the catalyst slurry, and then use filtration to separate the precipitate.

[0040] (3) Add the precipitate to 100ml of tert-butanol and stir for 10min, then add 500ml of water and continue to stir for 10min, then filter and separate the precipitate. Repeat this step and the total volume of the solvent remains unchanged, and the consumption of tert-butanol is gradually inc...

Embodiment 2

[0042] Embodiment 2: Catalyst preparation mode is the same as embodiment 1, just organic ligand does not use tert-butanol, but uses dimethyl ether (DME), obtains the structural formula of gained catalyst DMC-2 through analysis: Zn 3 [Co(CN) 6 ] 2 1.4ZnCl 2 2.1DME 0.6H 2 o

Embodiment 3

[0043] Embodiment 3: catalyst preparation mode is the same as embodiment 1, just organic ligand does not use tert-butanol, but uses dioxane (Dioxane), obtains the structural formula of gained catalyst DMC-3 through analysis:

[0044] Zn 3 [Co(CN) 6 ] 2 1.5ZnCl 2 2.1Dioxane 0.5H 2 o

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Abstract

The invention discloses a preparation method for a double metal cyanide catalyst for polycarbonate synthesis. The preparation method comprises the following steps of: firstly dissolving soluble metallic salt in organic ligand, and then adding deionized water to serve as a solution 1; dissolving water-soluble metallic cyanide salt in the deionized water to serve as a solution 2, wherein the volume ratio of the solution 1 to the solution 2 is 0.1: 1-5: 1; and then dripping the solution 2 to the solution 1 to obtain a solid catalyst after stirring and drying. In the invention, the influence of the deionized water to the synergic action between the organic ligand and the soluble metal salt is avoided; the synergic action between the organic ligand and the soluble metal salt in the DMC (Di Methyl Carbonate) catalyst is exerted at the greatest degree; and the reaction time when the catalyst catalyzes a copolymerization of propylene oxide and CO2 does not exceed 8h, the activity reaches to above 30Kg polymer/g catalyst, and the CO2 unit content in the polymer reaches up to 45.0%.

Description

technical field [0001] The invention belongs to a preparation method of a double metal catalyst, in particular to a preparation method and application of a double metal cyanide catalyst for polycarbonate synthesis. Background technique [0002] CO since the industrial revolution 2 The sharp increase in emissions has led to a series of environmental problems. A low-carbon economy not only requires us to reduce CO 2 emissions, and how to effectively use cheap and low-toxic CO 2 It has also become a research hotspot. Using CO 2 Copolymerize with epoxy to form aliphatic polycarbonate, which is CO 2 Utilizing one of the most valuable and promising directions in research, aliphatic polycarbonate has been used in new polyurethane materials, biomedical materials, gas barrier materials, tougheners for brittle materials, reinforcing agents for rubber materials, and new liquid crystals. Materials, unsaturated polyesters, adhesives, photoresists, solid electrolytes and electronic d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/26B01J31/22C08G64/34
Inventor 刘宾元郑厚超张莉
Owner HEBEI UNIV OF TECH
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