Preparation method of Cu, Fe-doped vacancy Keggin type silicon tungsten polyoxometallate catalyst

A technology of silicotungstate and catalyst, which is applied in the direction of oxidative preparation of carbonyl compounds, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., which can solve the problems of low recycling rate, low catalytic activity and stable Poor performance and other problems, to achieve the effects of short production cycle, improved catalytic efficiency, and mild reaction conditions

Inactive Publication Date: 2014-08-06
NORTHWEST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of Cu, Fe-doped vacancy Keggin type silicotungstate catalyst, the catalyst uses transition metal Cu, Fe as counter ion, and its composition and properties are imp

Method used

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  • Preparation method of Cu, Fe-doped vacancy Keggin type silicon tungsten polyoxometallate catalyst
  • Preparation method of Cu, Fe-doped vacancy Keggin type silicon tungsten polyoxometallate catalyst
  • Preparation method of Cu, Fe-doped vacancy Keggin type silicon tungsten polyoxometallate catalyst

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Embodiment 1

[0027] (1) Weigh K 8 [β 2 -SiW 11 o 39 ]·14H 2 O white powder 3.24 g (1 mmol), dissolved in 20 ml deionized water to form solution A, weighed CuCl 2 2H 2 O0.068 g (0.4 mmol) was dissolved in 10 ml deionized water to form solution B, and solution B was slowly added dropwise to solution A to form solution C, which was slowly added dropwise to avoid precipitation during the process;

[0028] (2) Use 4 mol / L HCl solution to adjust the pH of solution C to 5.0, stir at room temperature for 3 h, use 4 mol / L HCl solution to maintain the pH of solution C at 4-6 during the process, and then Slowly evaporate the solution C to dryness, there is solid powder to separate out, continue heating until the quality is constant and does not become the catalyst precursor;

[0029] (3) Put the catalyst precursor in the muffle furnace, under N 2 Calcined at 320 °C for 12 h under protection, and ground the obtained solid into powder to obtain catalyst S1;

[0030] (4) by figure 1 and Figur...

Embodiment 2

[0032] (1) Weigh K 8 [β 2 -SiW 11 o 39 ]·14H 2 O white powder 3.24 g (1 mmol), dissolved in 20 ml deionized water to form solution A, weighed anhydrous FeCl 3 Dissolve 0.064 g (0.4 mmol) in 10 ml of deionized water to form solution B, slowly add solution B to solution A to form solution C, and add slowly to avoid precipitation during the process;

[0033] (2) Use 4 mol / L HCl solution to adjust the pH of solution C to 5.0, stir at room temperature for 3 h, use 4 mol / L HCl solution to maintain the pH of solution C at 4-6 during the process, and then Slowly evaporate the solution C to dryness, there is solid powder to separate out, continue heating until the quality is constant and does not become the catalyst precursor;

[0034] (3) Put the catalyst precursor in the muffle furnace under N 2 Calcined at 320 °C for 12 h under protection, and ground the obtained solid into powder to obtain catalyst S2;

[0035] (4) by figure 1 and Figure 4 It can be seen that the catalyst...

Embodiment 3

[0037] (1) Weigh K 8 [β 2 -SiW 11 o 39 ]·14H 2 O white powder 3.24 g (1 mmol), dissolved in 20 ml deionized water to form solution A, weighed CuCl 2 2H 2 O0.068 g (0.4 mmol) was dissolved in 10 ml deionized water to form solution B, and anhydrous FeCl was weighed 3 Dissolve 0.064 g (0.4 mmol) in 10 ml deionized water to form solution C, slowly add solutions B and C to solution A respectively to form solution D, and do not precipitate during the dropping process;

[0038] (2) Use 4 mol / L HCl solution to adjust the pH of solution D to 5.5, stir at room temperature for 3 h, use 4 mol / L HCl solution to maintain the pH of solution D at 4-6 during the process, and then Slowly evaporate the solution D to dryness, there is solid powder to separate out, continue heating until the mass is constant and does not become the catalyst precursor;

[0039] (3) Put the catalyst precursor in the muffle furnace under N 2 Calcined at 380 °C for 8 h under protection, and the obtained solid ...

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Abstract

The invention discloses a preparation method of a Cu, Fe-doped vacancy Keggin type silicon tungsten polyoxometallate catalyst. According to the invention, Cu and/or Fe salt with the molar ratio of 0.1-0.4 are/is added into Na10[alpha-SiW9O34].18H2O, K8[gamma-SiW10O36].10H2O and K8[beta2-SiW11O39].14H2O polyoxometallate precursors, full mixing, dissolution and evaporation for dryness are sequentially performed, and finally, calcining is performed at the temperature of 300-400 DEG C, so that the catalyst can be obtained. The preparation method is simple, low in cost, moderate in reaction condition and high in recovery rate; the raw materials are easy to get; when the catalyst is used for preparing benzaldehyde through catalytic oxidation of phenylcarbinol and 30% H2O2 is used as the oxidizing agent, the conversion rate can reach 87.1-96.9%, and the productive rate can reach 85.3-96.1%.

Description

technical field [0001] The invention relates to a preparation method of a Cu and Fe-doped vacancy Keggin type silicotungstate catalyst, which belongs to the technical field of catalysts. Background technique [0002] Polyoxometalates are a class of inorganic metal-oxygen clusters in which high-valent transition metals are bridged by oxygen, also known as polyacid compounds. Due to the diversity of its composition and structure, its adjustable acidity and redox properties, it has a wide range of applications in the fields of medicinal chemistry, biochemistry, electrochemistry, materials chemistry and catalytic chemistry. Polyoxometalates are used as catalysts, which have the characteristics of high catalytic activity, good selectivity, mild conditions, and no corrosion of equipment. They can be used as both acid catalysts and redox catalysts. At present, the commonly used polyacid catalysts are mainly saturated Keggin-type polyacid compounds. Due to their high stability, low...

Claims

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Application Information

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IPC IPC(8): B01J31/28C07C45/29C07C47/54
Inventor 薛岗林於成星武立州董新博闫永红张晓芬
Owner NORTHWEST UNIV
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