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Method for preparing high-purity heteropoly acid of Keggin structure

A heteropoly acid, high-purity technology, applied in chemical instruments and methods, inorganic chemistry, molybdenum compounds, etc., can solve the problems of low purity of phosphotungstic acid, complicated preparation process, etc., and achieve suitable for large-scale industrial production and product purity High, high yield effect

Active Publication Date: 2008-11-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of this method is complicated, and the purity of the obtained phosphotungstic acid is not high, and contains a large amount of phosphate

Method used

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  • Method for preparing high-purity heteropoly acid of Keggin structure
  • Method for preparing high-purity heteropoly acid of Keggin structure
  • Method for preparing high-purity heteropoly acid of Keggin structure

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Weigh 100 grams of sodium tungstate, dissolve it in 150 ml of water, add 16 grams of disodium hydrogen phosphate under stirring, heat to boiling, keep boiling under reflux for 4 hours, and obtain sodium phosphotungstate and phosphotungstic with a concentration of 35.7% by weight acid mixture.

[0036] In order to obtain phosphotungstic acid, add 200 grams of concentrated hydrochloric acid (at this time, the concentration of hydrochloric acid in the system is about 7.2mol / L) to the mixed solution of sodium phosphotungstic acid and phosphotungstic acid at 50°C, cool and precipitate for 12 hours, Filter and dry at room temperature for 5 hours to obtain 73.7 grams of white phosphotungstic acid. 3 PW 12 o 40 .29H 2 O meter, yield is 76.5%. The results of impurity content analysis are shown in Table 1.

[0037] Sample of phosphotungstic acid 31 P-NMR nuclear magnetic resonance spectrum see figure 1 . figure 1 The peak at the chemical shift -14.861ppm is the peak of th...

Embodiment 2

[0041] Weigh 100 grams of molybdenum trioxide and add it to 600 ml of 17.5% by weight phosphoric acid, heat to boiling, and keep boiling for 4 hours under reflux to obtain a phosphomolybdic acid solution with a concentration of 15% by weight.

[0042] In order to obtain pure phosphomolybdic acid, add 10 grams of concentrated nitric acid (the concentration of nitric acid in the system at this time is about 0.17mol / L) to the phosphomolybdic acid solution at -5°C, cool, precipitate for 12 hours, filter and dry. Obtain 85.6 grams of white yellow phosphomolybdic acid, with H 3 PMo 12 o 40 .6H 2 O meter, the yield is 77%. The results of impurity content analysis are shown in Table 1.

Embodiment 3

[0044] Weigh 100 grams of sodium tungstate, dissolve it in 200ml of water, add 7.5 grams of water glass solution (density 1.375, SiO 2 concentration is 23.5% by weight), heated to boiling, and kept boiling for 4 hours under reflux to obtain a mixed solution of sodium silicotungstate and silicotungstic acid with a concentration of 24% by weight. In order to precipitate silicotungstic acid, add 150 grams of concentrated hydrochloric acid (the concentration of hydrochloric acid in the system is about 5.1mol / L at this time) to the mixed solution of sodium silicotungstate and silicotungstic acid at 80°C, cool and precipitate for 10 hours , filtered and dried. Obtain 57.7 grams of high-purity white silicotungstic acid, with H 3 SiW 12 o 40 .7H 2 O meter, yield is 76.5%. The results of impurity content analysis are shown in Table 1.

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Abstract

The invention provides a preparation method of high-purity heteropolyacid with Keggin structure, which comprises the steps that an acid precipitant is added into heteropolyacid and / or the water solution of heteropolyacid salt so as to cause the heteropolyacid to precipitate out, and then the heteropolyacid is filtered and dried to obtain the high-purity heteropolyacid with the Keggin structure. The acid precipitant is mineral acid, more specifically, is selected from the mixture of hydrochloric acid and sulphuric acid or nitric acid, or hydrochloric acid, sulphuric acid and nitric acid with any volume ratio. The molar concentration of the acid precipitant in the reaction system is 0.1-8 mol / L. Compared with the prior art, the preparation method of the invention has simple process and high purity of products, does not use a great quantity of inflammable organic extractants when in production, and is applicable to being used as an acid catalyst.

Description

technical field [0001] The invention relates to a method for preparing a high-purity Keggin structure heteropolyacid, more specifically, the present invention relates to a method for preparing a high-purity Keggin structure heteropolyacid from an aqueous heteropolyacid and / or heteropolyacid salt solution. Background technique [0002] Heteropolyacid is a kind of acid with cage structure and pores obtained by acidification, condensation and dehydration of two or more inorganic oxoacid ions. Heteropolyacid has both strong acidity and redox property, so It can be used as an acid catalyst or as a redox catalyst. The heteropolyacid is evenly supported on a carrier, such as silicon oxide, aluminum oxide, silicon oxide-alumina mixture or activated carbon, to obtain a supported heteropolyacid catalyst. This supported heteropolyacid catalyst can be used in hydrocarbon conversion reactions requiring strong acidic catalysts, such as alkylation reactions, olefin hydration, aldehyde oxi...

Claims

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Application Information

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IPC IPC(8): B01J27/19C01G39/00
Inventor 项祖红何奕工
Owner CHINA PETROLEUM & CHEM CORP
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