Preparation method of MIL-100(Fe) packaged phosphotungstic heteropolyacid catalyst

A technology of phosphotungstic heteropolyacid and catalyst, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., and can solve the problem of low yield of supported heteropolyacid catalysts , harsh conditions and other problems, to achieve the effect of high catalyst synthesis yield, low synthesis temperature and pressure, and low synthesis energy consumption

Active Publication Date: 2013-07-10
日照经济技术开发区客商服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods all need to be carried out under the conditions of high temperature and high pressure static crystallization, and there are problems such as harsh conditions and low yield of the synthesized supported heteropolyacid catalyst.

Method used

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  • Preparation method of MIL-100(Fe) packaged phosphotungstic heteropolyacid catalyst
  • Preparation method of MIL-100(Fe) packaged phosphotungstic heteropolyacid catalyst
  • Preparation method of MIL-100(Fe) packaged phosphotungstic heteropolyacid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 0.34 g of sodium tungstate and 0.012 g of disodium hydrogen phosphate into a three-necked flask filled with 5 mL of deionized water, and then add 2.02 g of Fe(NO 3 ) 3 . 9H 2 O, after magnetic stirring for about 30 min, add 0.70 g of 1,3,5-benzenetricarboxylic acid, stir for 30 min, add 0.5 mL of 1 mL / L hydrofluoric acid dropwise, continue stirring for 1 h, reflux to condense, and heat up to 95 °C Afterwards, the constant temperature was maintained for 12 h, and the reactor was a three-necked flask with a reflux condenser. After the reaction, the samples were filtered, washed with a sufficient amount of deionized water, and dried in a drying oven at constant temperature for 5 h.

[0025] The dried samples were further purified with ethanol and ammonium fluoride, respectively. First, treat with absolute ethanol at 70 °C for 10 h, then treat with 30 mmol / L ammonium fluoride solution at 80 °C for 10 h, and finally wash thoroughly with deionized water. The drying t...

Embodiment 2

[0027] Add 0.21 g of sodium tungstate and 0.0074 g of disodium hydrogen phosphate into a three-necked flask filled with 15 mL of deionized water, and then add 0.81 g of FeCl 3 . 6H 2 O, after magnetic stirring for about 30 min, add 0.51 g of 1,3,5-trimethylbenzenetricarboxylate, stir for 30 min, add 0.5 mL of 1 mL / L hydrofluoric acid dropwise, continue stirring for 1 h, reflux to condense, and heat up After reaching 95 °C, keep the constant temperature for 12 h, and the reactor is a three-necked flask with a reflux condenser. After the reaction, the samples were filtered, washed with a sufficient amount of deionized water, and dried in a drying oven at constant temperature for 5 h.

[0028] The dried samples were further purified with ethanol and ammonium fluoride, respectively. First, treat with absolute ethanol at 60 °C for 15 h, then treat with 40 mmol / L ammonium fluoride solution at 70 °C for 15 h, and finally wash thoroughly with deionized water. The drying temperatur...

Embodiment 3

[0030] Add 0.34 g of sodium tungstate and 0.012 g of disodium hydrogen phosphate into a three-necked flask filled with 5 mL of deionized water, and then add 2.02 g of Fe(NO 3 ) 3 . 9H 2 O, after magnetic stirring for about 30 min, add 0.63 g of 1,3,5-trimethylbenzenetricarboxylate, stir for 30 min, add 0.5 mL of 1 mL / L hydrofluoric acid dropwise, continue stirring for 30 min, reflux to condense, and heat up After reaching 80 °C, keep the constant temperature for 20 h, and the reactor is a three-necked flask with a reflux condenser. After the reaction, the samples were filtered, washed with a sufficient amount of deionized water, and dried in a drying oven at constant temperature for 5 h.

[0031] The dried samples were further purified with ethanol and ammonium fluoride, respectively. First, treat with absolute ethanol at 80 °C for 20 h, then treat with 50 mmol / L ammonium fluoride solution at 60 °C for 10 h, and finally wash thoroughly with deionized water. The drying tem...

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Abstract

The invention discloses a preparation method of an MIL-100(Fe) packaged phosphotungstic heteropolyacid catalyst. The preparation method comprises the steps of: adding raw materials for synthesizing phosphotungstic heteropolyacid into a certain amount of deionized water based on certain proportion; subsequently adding a certain amount of an iron source, mixing and stirring, further adding a certain amount of an organic ligand, mixing, stirring, adding a certain amount of an acid solution, and mixing and stirring; mixing, stirring and reacting for 5-20 hours under normal pressure at 80-95 DEG C; and filtering the obtained solid, washing for 10-20 hours at 60-80 DEG C by using absolute ethyl alcohol, subsequently treating for 10-15 hours at 60-80 DEG C by using a 30-60mmol / L ammonium fluoride solution, sufficiently washing by using deionized water, and finally drying for 5-10 hours at 100-200 DEG C so as to obtain the MIL-100(Fe) packaged phosphotungstic heteropolyacid catalyst. The method is temperate in synthesis condition, low in synthesis energy consumption and high in catalyst synthesis yield.

Description

technical field [0001] The invention belongs to a preparation method of a supported heteropolyacid catalyst, in particular to a preparation method of a MIL-100 (Fe) encapsulated phosphotungstic heteropolyacid catalyst. Background technique [0002] Heteropolyacids (salts) are polyoxometalates (Polyoxometalates, POMs), which are composed of {MO 6} octahedron and {MO 4}Tetrahedron is composed of basic building units, and a considerable number and variety of structures are produced by connecting polyhedrons with corners, edges or planes. Due to the strong proton acidity and adjustable redox properties of heteropolyacids (salts), they have attracted the attention of researchers in the field of catalysis. Among the many heteropolyacids (salts), Keggin structure heteropolyacids (salts) are the most widely studied. The general formula of this series is [XM 12 o 40 ] n- (X=P, Si, M=Mo, W), where X is called a heteroatom and M is called a coordination atom. [0003] Because he...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/34
Inventor 张富民石静钟依均朱伟东
Owner 日照经济技术开发区客商服务有限公司
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