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Method for purifying phosphotungstic acid crystal

A purification method, phosphotungstic acid technology, applied in chemical instruments and methods, tungsten compounds, crystal growth, etc., to achieve the effects of low preparation cost, no pollution to the environment, and short process

Active Publication Date: 2016-11-09
CENT SOUTH UNIV
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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 how to reduce the production cost in the purification of phosphotungstic acid crystals, simplify the process steps, achieve green and pollution-free, and provide a purification method of phosphotungstic acid crystals

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 568g of industrial phosphotungstic acid (without molybdenum impurities) in water, and then add hydrochloric acid to make tungsten trioxide in the solution 80g / L, and the concentration of hydrochloric acid is 3mol / L. Using 15% 2-octanol as the extractant and sulfonated kerosene as the diluent, four-stage countercurrent extraction was performed; the loaded organic phase was subjected to five-stage countercurrent extraction with distilled water as the back-extraction reagent. The stripping solution was evaporated and crystallized to obtain 542 g of high-purity white phosphotungstic acid, with a yield of 95.4%.

Embodiment 2

[0025] Dissolve 660g of industrial phosphotungstic acid (without molybdenum impurities) in water, and then add sulfuric acid to make tungsten trioxide in the solution 50g / L, and the concentration of sulfuric acid is 4mol / L. Using 5% nonanol as the extractant and sulfonated kerosene as the diluent, five-stage countercurrent extraction was performed; the loaded organic phase was subjected to four-stage countercurrent extraction with distilled water as the stripping reagent. The stripping solution was evaporated and crystallized to obtain 647 g of high-purity white phosphotungstic acid, and the yield was 98%.

Embodiment 3

[0027] Dissolve 360g of industrial phosphotungstic acid (without molybdenum impurities) in water, and then add nitric acid to make tungsten trioxide in the solution 120g / L, and the concentration of nitric acid is 2mol / L. 50% decanol was used as the extractant, and the diluent was sulfonated kerosene, and then two-stage countercurrent extraction was performed; the loaded organic phase was subjected to six-stage countercurrent extraction with distilled water as the back-extraction reagent. The stripping solution was evaporated and crystallized to obtain 345 g of high-purity white phosphotungstic acid, with a yield of 95.8%.

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PUM

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Abstract

The invention belongs to the technical field of preparation of heteropoly acids and particularly relates to a method for purifying phosphotungstic acid crystal. Industrially acquired phosphotungstic acids typically comprise a high amount of impurities such as phosphorus, sulfur, molybdenum, sodium and calcium, and the invention is intended to purify the phosphotungstic acids with high impurity content. The method of the invention includes: dissolving industrial phosphotungstic acid with high impurity content in water, extracting with an alcohol extracting agent, back-extracting directly with distilled water to obtain high-concentration phosphotungstic acid solution, wherein the alcohol extracting agent can be returned and extracted directly after back-extraction and raffinate can also be returned directly to the dissolved phosphotungstic acid crystal for reuse; if comprising molybdenum, the obtained high-concentration phosphotungstic acid solution needs to be subjected to extraction, molybdenum removal and evaporative crystallization to prepare high-purity phosphotungstic acid crystal, and if not comprising molybdenum, the high-concentration phosphotungstic acid solution can be subjected directly to evaporative crystallization to obtain high-purity phosphotungstic acid crystal. The method of the invention has short process flow, low manufacture cost and high product yield, is environment-friendly and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, and more specifically relates to a method for purifying phosphotungstic acid crystals. Background technique [0002] Heteropolyacids are one of the most active catalysts used in acid-catalyzed reactions and redox reactions. It has good catalytic performance for hydration and esterification of olefins, etherification of epoxides, condensation of olefins and aldehydes, alkylation, epoxidation of olefins, and aromatication of alkyls. In addition, as a catalyst, heteropolyacid has the advantages of high catalytic activity, high selectivity, small corrosion, and easy control of the reaction. In addition, its own structure is stable and can be recycled and recycled. Therefore, it has attracted widespread attention, especially in the petrochemical industry. has broad applications. Phosphotungstic acid H 3 PW 12 o 40 ·nH 2 O is the most widely used in heteropolyacids, and its purity di...

Claims

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Application Information

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IPC IPC(8): C01G41/00C30B29/10
CPCC01G41/003C30B29/10
Inventor 李永立赵中伟
Owner CENT SOUTH UNIV
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