Preparation method of silicotungstic heteropoly acid

A technology of phosphotungstic heteropoly acid and phosphotungstic acid, which is applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as poor production safety, and achieve improved production and operation safety. The effect of technical effects

Active Publication Date: 2012-10-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the prior art uses flammable low-boiling point organic extractants, resulting in poor production safety, and provides a new preparation method of phosphotungstic heteropoly acid

Method used

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  • Preparation method of silicotungstic heteropoly acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Dissolve sodium tungstate with a concentration of 0.01 g / ml and disodium hydrogen phosphate in a concentration range of 0.05 g / ml in 200 ml of hot water. While heating and stirring, add concentrated hydrochloric acid to the solution. After the solution is clear, add 20 Mol / liter C 16 H 33 N + Cl - In the chloroform solution, C 16 H 33 N + Cl - The added amount is 0.05 mol / g sodium tungstate, while vigorously stirring, the phosphotungstic heteropoly acid catalyst is obtained. The catalyst was separated by centrifugation, washed with deionized water until the pH of the washing solution was 5, and then dried under nitrogen flow for 3 hours at a drying temperature of 180°C; and then roasted under nitrogen flow at a temperature of 500°C and a roasting time of 3 hours to produce phosphorus Tungsten heteropoly acid 8.5 g H 3 PW 12 O 40 ·X H 2 O(x=0-30) catalyst.

[0018] The XRD spectrum of the sample phosphotungstic acid is shown in figure 1 . From figure 1 It can be seen tha...

Embodiment 2

[0020] Dissolve sodium tungstate with a concentration of 0.05 g / ml and disodium hydrogen phosphate in a concentration range of 0.1 g / ml in 200 ml of hot water. While heating and stirring, add concentrated hydrochloric acid to the solution. After the solution is clear, add concentration 20 mol / L C 18 H 37 N + Cl - In the methylene chloride solution, C 18 H 37 N + Cl - The added amount is 0.1 mol / g sodium tungstate, while vigorously stirring, to obtain phosphotungstic heteropoly acid catalyst. The catalyst was separated by centrifugation, washed with deionized water until the pH of the washing solution was 5, and then dried under nitrogen flow for 10 hours at a drying temperature of 120°C; and then roasted under nitrogen flow at a roasting temperature of 300°C and a roasting time of 8 hours to produce phosphorus Tungsten heteropoly acid 44 g H 3 PW 12 O 40 ·X H 2 O(x=0-30) catalyst.

[0021] The XRD spectrum of the sample phosphotungstic acid and figure 1 Similarly, there are char...

Embodiment 3

[0023] Dissolve sodium tungstate with a concentration of 0.1 g / ml and disodium hydrogen phosphate in a concentration range of 0.15 g / ml in 200 ml of hot water. While heating and stirring, add concentrated hydrochloric acid to the solution. After the solution is clear, add concentration 20 moles / liter C 22 H 45 N + Cl - In ethanol solution, C 22 H 45 N + Cl - The added amount is 0.2 mol / g sodium tungstate, while vigorously stirring, to obtain phosphotungstic heteropoly acid catalyst. The catalyst was separated by centrifugation and washed with deionized water until the pH of the washing solution was 5, and then dried under nitrogen flow for 15 hours at a drying temperature of 80°C; and then roasted under nitrogen flow at a roasting temperature of 350°C and a roasting time of 6 hours to produce phosphorus Tungsten heteropoly acid 88 g H 3 PW 12 O 40 ·X H 2 O(x=0-30) catalyst.

[0024] The XRD spectrum of the sample phosphotungstic acid and figure 1 Similarly, there are characteris...

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Abstract

The invention relates to a preparation method of silicotungstic heteropoly acid, and aims to mainly solve the problem that employment of inflammable low-boiling point organic extracting agent can result in poor production security in the prior art. The method of the invention includes the following steps of: a) dissolving sodium tungstate and sodium hydrogen phosphate in water to generate a mixed solution of phosphotungstic acid and sodium phosphotungstate under heating and acidic conditions, with the sodium tungstate and the sodium hydrogen phosphate in a weight ratio of 1:0.1-1:10; b) dissolving CnH2n+1N<+>Cl<-> in an organic solvent to obtain an organic solution of CnH2n+1N<+>Cl<->, wherein n is a positive integer from 10 to 30, and with the sodium tungstate adding amount as the reference, the adding amount of CnH2n+1N<+>Cl<-> content is 0.01-1 mol/g sodium tungstate; and c) adding the organic solution of CnH2n+1N<+>Cl<-> into the mixed solution of phosphotungstic acid and sodium phosphotungstate for reaction, then carrying out centrifugation, washing, drying and roasting on the product, thus obtaining silicotungstic heteropoly acid. The technical scheme in the method of the invention well solves the problem, and can be used in the industrial production of silicotungstic heteropoly acid.

Description

Technical field [0001] The invention relates to a preparation method of phosphotungstic heteropoly acid. Background technique [0002] Keggin structure heteropoly acid has strong acidity. In organic medium, the molar catalytic activity of heteropoly acid reaches 100 to 1000 times that of sulfuric acid. Heteropoly acid is relatively stable, non-toxic and easy to handle, and does not produce side reactions such as sulfidation, chlorination and nitrification. As a new type of catalytic material, heteropolyacid has shown broad application prospects in the fields of oil refining and chemical industry, and has been successfully applied in olefin hydration, alkylation and isomerization reactions. Among them, phosphotungstic acid H 3 PW 12 O 40 .nH 2 O (n is a positive integer from 0 to 30) is the most widely used and representative of heteropoly acids. [0003] H.S. Booth et al. reported the synthesis method of phosphotungstic acid as early as 1939, see the literature Inorganic Synthesi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188
Inventor 杨洪云高焕新金国杰丁琳陈璐康陈军
Owner CHINA PETROLEUM & CHEM CORP
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