Double-metal cyanide catalyst for copolymerization of carbon dioxide and epoxide and preparation method of double-metal cyanide catalyst

A double metal cyanide and epoxy technology, applied in the chemical field, can solve the problems of uneconomical recycling of chelating agents, high catalyst manufacturing costs, and impact on industrial applications, etc., to achieve shortened induction period, low production cost, and high yield Effect

Active Publication Date: 2020-06-16
合肥普力先进材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the catalyst preparation method adopted, the amount of metal halide and chelating agent is generally far excessive, generally 3-20 times that of metal cyanide, and in industrial applications, the recovery cost of chelating agent is high, when using polymer chelating agent When using chelating agents, the recovery of chelating agents is not economically cost-effective. The cost of treating these wastewater containing a large amount of chelating agents is very high, and the cost of catalyst manufacturing is high, which affects industrial applications.

Method used

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  • Double-metal cyanide catalyst for copolymerization of carbon dioxide and epoxide and preparation method of double-metal cyanide catalyst
  • Double-metal cyanide catalyst for copolymerization of carbon dioxide and epoxide and preparation method of double-metal cyanide catalyst
  • Double-metal cyanide catalyst for copolymerization of carbon dioxide and epoxide and preparation method of double-metal cyanide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Complex M 1 Preparation of LX:

[0039] (1)a) Preparation of complex L-1:

[0040]

[0041] Under a nitrogen atmosphere, dissolve 0.3 g of (2-phenyliminomethylphenyl) aniline in 18 mL of toluene, add an equivalent amount of zinc chloride at -78 ° C, stir at room temperature overnight, and remove Solvent, the crude product was recrystallized from dichloromethane and cyclohexane. 0.42g of the product was obtained. Yield: 90.1%.

[0042] Elemental analysis structure: C: 61.22; H: 4.10; Cl: 9.55; N: 7.47; Zn: 17.43

[0043] b) Preparation of complex L-5:

[0044]

[0045] The complex L-5 was prepared by the same method as above, wherein the reactant zinc bromide was replaced with zinc chloride in a), and the yield was 93.7%.

[0046] Elemental analysis structure: C: 54.63; H: 3.81; Br: 19.11; N: 6.62; Zn: 15.71 (2) complexes L-2, L-3, L-4, L-6, L-7, L- Preparation of 8:

[0047] The complexes L-2, L-3, L-4, L-6, L-7, and L-8 were prepared by a similar method i...

Embodiment 2-9

[0051] Preparation of DMC catalyst:

[0052] Weigh a certain amount of metal M 1 Complex M 1 LX and metal salt M 2 e x f , Metal M 2 Add the cyanide in the ball mill tank respectively, add a small amount of solvent (ethylene glycol / glycerol / tert-butanol / acetone), and then put steel balls. The ball mill jar is placed in a ball mill with a rotational speed of 25-60 Hz to run for 10-60 minutes. After the catalyst is ground, it is washed several times with a mixed solution of alcohol solvent and water, filtered, and the white insoluble matter is dried to a constant weight in a vacuum oven at 60°C, and ground for later use. The preparation parameters of Examples 2-9 are shown in Table 2.

[0053] Table 2

[0054]

Embodiment 10～17

[0056] All reaction conditions, parameters and product parameters are as shown in Table 3, and the reaction steps are summarized as follows:

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PUM

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Abstract

The invention provides a double-metal cyanide catalyst for copolymerization of carbon dioxide and epoxide. The structural formula is M1a [M2 (CN) bLc] dXi, and the catalyst is obtained by mixing a complex M1LX of metal M1, cyanide of metal M2 and metal salt M1eXf and performing reaction under mechanical ball milling, wherein M1LX is a compound with a structure as shown in the following formula (II) which is described in the specification, M2 is selected from one of Co<2+>, Co<3+>, Fe<2+>, Fe<3+>, Cd<2+> and Mn<3+>, and X is selected from one or more of F<->, Cl<->, Br<->, I<->, NO3<->, SO4<2->or organic carboxylate anions. The preparation method of the catalyst is simple, convenient and green, the catalyst is high in catalytic efficiency, good in activity and good in stability, and in a carbon dioxide / epoxide copolymerization reaction, higher catalytic activity and higher selectivity of a polymer product and polycarbonate chain links on a polymer main chain can be embodied in a polymerization reaction under the conditions of relatively lower catalyst concentration and higher initiator concentration.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a double metal cyanide catalyst for the copolymerization of carbon dioxide and epoxides, a preparation method thereof, and an application of the catalyst for catalyzing the copolymerization of carbon dioxide and epoxides. Background technique [0002] Carbon dioxide and epoxide can be directly copolymerized to prepare aliphatic polycarbonate resin, and the obtained aliphatic polycarbonate resin can be used as engineering plastics, low-temperature pyrolysis materials, biodegradable plastic masterbatches, oil-resistant rubber raw materials, polyurethane raw materials, special structure Use of ceramics, metal materials, etc. The research on carbon dioxide / epoxide copolymerization, especially the development of new carbon dioxide / epoxide copolymerization catalysts has received extensive attention. ZnEt was first reported by Inoue (Inoue S., Koinuna H., Tsuruta T., Macromol Chem., 1969, 130-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34C08G64/02
CPCC08G64/34C08G64/0208
Inventor 罗铭毛红兵王慧君
Owner 合肥普力先进材料科技有限公司
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