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Preparation method of phosphotungstic 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: 2016-08-03
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 phosphotungstic 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 with a concentration 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 clarified, add 20 mol / L C 16 h 33 N + Cl - in chloroform solution, C 16 h 33 N + Cl - The addition amount is 0.05 mol / g sodium tungstate, while stirring vigorously, obtain phosphotungstic heteropolyacid catalyst. Centrifuge to separate the catalyst, wash the catalyst with deionized water until the pH of the washing solution is 5, and then dry it under nitrogen flow for 3 hours at a drying temperature of 180°C; then roast it under nitrogen flow at a temperature of 500°C for 3 hours to produce phosphorus Tungsten heteropoly acid 8.5 g H 3 PW 12 o 40 ·xH 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 that the 2θ of the chara...

Embodiment 2

[0020] Dissolve sodium tungstate with a concentration of 0.05 g / ml and disodium hydrogen phosphate with a concentration range of 0.1 g / ml in 200 ml of hot water, add concentrated hydrochloric acid to the solution while heating and stirring, and after the solution is clarified, add concentration 20 mol / L C 18 h 37 N + Cl - solution in dichloromethane, C 18 h 37 N + Cl - The addition amount of the sodium tungstate is 0.1 mol / g, while vigorously stirring to obtain a phosphotungstic heteropolyacid catalyst. Centrifuge to separate the catalyst, wash the catalyst with deionized water until the pH of the washing solution is 5, and then dry it under nitrogen flow for 10 hours at a drying temperature of 120°C; then roast it under nitrogen flow at a temperature of 300°C for 8 hours to produce phosphorus Tungsten heteropoly acid 44 g H 3 PW 12 o 40 ·xH 2 O(x=0~30) catalyst.

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

Embodiment 3

[0023] Dissolve sodium tungstate with a concentration of 0.1 g / ml and disodium hydrogen phosphate with a concentration of 0.15 g / ml in 200 ml of hot water, add concentrated hydrochloric acid to the solution while heating and stirring, and after the solution is clarified, add a concentration of 20 mol / L C 22 h 45 N + Cl - ethanol solution, C 22 h 45 N + Cl - The addition amount of the sodium tungstate is 0.2 mol / g, while vigorously stirring to obtain a phosphotungstic heteropolyacid catalyst. Centrifuge to separate the catalyst, wash the catalyst with deionized water until the pH of the washing solution is 5, and then dry it under nitrogen flow for 15 hours at a drying temperature of 80°C; then roast it under nitrogen flow at a temperature of 350°C for 6 hours to produce phosphorus Tungsten heteropoly acid 88g H 3 PW 12 o 40 ·xH 2 O(x=0~30) catalyst.

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

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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] The heteropoly acid with Keggin structure has strong acidity. In organic medium, the molar catalytic activity of heteropoly acid reaches 100-1000 times that of sulfuric acid. Heteropoly acids are relatively stable, non-toxic and easy to handle, and do not produce side reactions such as sulfidation, chlorination and nitration. As a new type of catalytic material, heteropolyacids have shown broad application prospects in the fields of oil refining and chemical industry, and have 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 most representative heteropoly acid. [0003] H.S.Booth et al reported the synthesis method of phosphotungstic acid as early as 1939, see the literature Ino...

Claims

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Application Information

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Patent Type & Authority Patents(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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