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Metal cyanide coordination catalyst and preparation method and application thereof

A technology of coordination catalysts and cyanides, which is applied in the field of catalysts for polymer synthesis, and can solve problems such as the inability to increase the degree of copolymer alternation

Active Publication Date: 2012-05-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the catalyst prepared by the existing preparation technology catalyzes epoxide and its reaction with acid anhydride or CO 2 (especially PO) cannot increase the degree of alternation of the copolymer during copolymerization

Method used

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  • Metal cyanide coordination catalyst and preparation method and application thereof
  • Metal cyanide coordination catalyst and preparation method and application thereof
  • Metal cyanide coordination catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The preparation of embodiment 1 metal cyanide complex catalyst

[0055] Step 1: Add 0.80g K 3 Co(CN) 6 (0.0024mol) was dissolved in 50mL of deionized water I, and 2mL (1.57g) of tert-butanol was added to obtain a mixed solution I', and an aqueous hydrochloric acid solution was added to adjust the mixed solution I' to pH<7, and the dissolution was uniform and transparent, and then the mixture was mixed under stirring conditions. 4.0 g (0.029 mol) of zinc chloride was dissolved in 20 mL of deionized water II into an aqueous solution of zinc chloride (mixed solution II'), stirred and reacted at 40 ° C for 24 hours, and suction filtered to obtain a semi-dry solid filter cake;

[0056] Step 2: Disperse the mixture of the filter cake obtained in the previous step and 0.5g zinc chloride (0.0037mol) in anhydrous tert-butanol in which 2.0g 1-phenylimidazole (N-phenylimidazole, 0.0139mol) was dissolved (20 mL), stirred at 60°C for 10 hours, and filtered with suction to obtain ...

Embodiment 2

[0061] The preparation of embodiment 2 metal cyanide complex catalyst

[0062] With embodiment 1, just add 2.1g EO in the mixed solution I ' of step one 20 PO 70 EO 20 (Pluronic P123, Aldrich), is 4.2wt% of deionized water 1 weight (50g). Finally, 1.5 g of a solid metal cyanide complex catalyst was obtained.

[0063] Elemental analysis results: Zn: 19.4wt%; Co: 9.6wt%; Cl: 6.3wt%; C: 28.84wt%; H: 3.27wt%; N: 16.35wt%

[0064] SEM observation (see figure 1 A): spherical shape, the average particle size is less than 100nm;

[0065] XRD result (see figure 2 A) It shows a broad peak in the interval of 2θ=13~25°;

[0066] The average pore size measured by nitrogen adsorption method was 8nm.

[0067] Infrared spectrum (see image 3 A) The peaks at 2294 and 472 wavenumbers are the characteristic infrared absorption peaks of CN and Co-C bonds in the catalyst; the absorption peaks at 1500 and 1200 wavenumbers indicate the presence of organic ligands in the catalyst.

Embodiment 3

[0068] The preparation of embodiment 3 metal cyanide coordination catalyst

[0069] Same as Example 1, except that in step 2, 1-phenylimidazole is replaced by equimolar diphenyl sulfoxide, anhydrous tert-butanol is replaced by anhydrous tetrahydrofuran of equal volume, and the slurry is dispersed in anhydrous tetrahydrofuran. The pulping temperature is the reflux temperature of tetrahydrofuran. 1.8 g of a solid metal cyanide complex catalyst was obtained.

[0070] Elemental analysis results: Zn: 19.2wt%; Co: 9.2wt%; Cl: 2.8wt%; C: 26.04wt%; H: 1.03wt%; N: 15.78wt%.

[0071] SEM observation (see figure 1 B) In flake shape, thickness: 20-40nm;

[0072] XRD results show a broad peak in the interval of 2θ=13~25°;

[0073] The average pore size measured by nitrogen adsorption method was 45nm.

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Abstract

The invention discloses a metal cyanide coordination catalyst and a preparation method and application thereof. The catalyst has the structural formula of M1a[M2(CN)bL1c]d(X)m(L2)n.xSu.yL3.zH2O. The method for preparing the metal cyanide coordination catalyst comprises the following steps of: regulating mixed solution I' which consists of L3, M3e[M2(CN)bL1c]f, deionized water I, alcohol and / or anether solvent to have a pH value of less than 7; and adding the solution I' into mixed solution II' which consists of M1(X)g salt, Su or a Su precursor, and deionized water II, and stirring for reaction at the temperature of between 20 and 120 DEG C for 0.5 to 200 hours; and separating, drying, the repeatedly dispersing to form slurry in an anhydrous organic solvent in which L2 is dissolved, distilling, separating and drying to prepare the metal cyanide coordination catalyst. The catalyst has the advantages of porous structure of less than 100nm, presence of coordination of M1 and L2 on a chemical structure, and obvious alternative selectivity in the process of catalyzing the copolymerization of epoxide and carbon dioxide.

Description

technical field [0001] The invention belongs to the field of catalysts for polymer synthesis, and in particular relates to a metal cyanide coordination catalyst and its preparation method and application. Background technique [0002] In the 1960s, the American General Tire Rubber Company first discovered that double metal cyanide (DMC) is an efficient catalyst for catalyzing the homopolymerization of epoxides to prepare polyether polyols. / kg), narrow molecular weight distribution (M w / M n <1.2) and other advantages, its quality is obviously better than that of polyether prepared by KOH catalysis. In recent years, the research on the preparation of DMC catalysts has mainly focused on the research that can eliminate the problem of high molecular weight "tailing" in the synthesis process of polyether polyols, and to develop the application field of DMC catalysts, such as being used to catalyze carbon dioxide (CO 2 ) and epoxy copolymerization to prepare polycarbonate, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/64C08G63/82C08G65/02
Inventor 张兴宏魏人建杜滨阳孙学科戚国荣
Owner ZHEJIANG UNIV
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