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Method for preparing phosphotungstic acid crystals from tungstenic mixed phosphoric and sulfuric acid solution

A technology of sulfur-phosphorus mixed acid and phosphotungstic acid, which is applied in the preparation of tungsten compounds, chemical instruments and methods, tungsten compounds, etc., can solve the problems of shortening the process and achieve the effects of no pollution to the environment, short process and low production cost

Active Publication Date: 2016-12-07
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is how to shorten the process in the preparation of phosphotungstic acid crystals, reduce costs, not pollute the environment, and realize large-scale industrial production, and provide a method for preparing phosphotungstic acid from tungsten-containing sulfur-phosphorus mixed acid solution crystal method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 5L of industrial solution containing tungsten, sulfuric acid and phosphoric acid, including 100g / L tungsten trioxide, 200g / L phosphoric acid, 0.5mol / L sulfuric acid, 5.4g / L iron ion, 2g / L manganese ion and 0.8g / L calcium ion , sodium ions 2g / L and other impurity ions. At first adjust sulfuric acid concentration to 2.5mol / L; Then take 15% secondary octanol as extractant, diluent is sulfonated kerosene, then carry out four-stage countercurrent extraction, compare O / A (oil phase / water phase)= 1:1; the loaded organic phase uses water as the stripping reagent, and performs five-stage countercurrent stripping, compared to O / A (oil phase / water phase) = 5:1. The concentration of tungsten trioxide in the stripping solution is 479.4g / L, and high-purity white phosphotungstic acid is obtained by evaporation and crystallization. Calculated based on the concentration of tungsten trioxide obtained from the back-extraction solution, the yield can reach 95.9%.

Embodiment 2

[0029] Take 2L of industrial solution containing tungsten, sulfuric acid and phosphoric acid, in which tungsten trioxide is 30g / L, phosphoric acid is 100g / L, sulfuric acid is 1mol / L, iron ion is 5.4g / L, manganese ion is 4g / L, calcium ion is 0.6g / L, Sodium ion 5g / L and other impurity ions. First adjust the concentration of sulfuric acid to 1.5mol / L; then use 15% nonanol as the extractant, diluent is sulfonated kerosene, and then carry out four-stage countercurrent extraction, the ratio is O / A=1:3; load the organic phase with Water is used as the stripping reagent, and the five-stage countercurrent stripping is carried out, and the ratio O / A=3:1. The concentration of tungsten trioxide in the stripping liquid is 240.2g / L, and high-purity white phosphotungstic acid is obtained by evaporation and crystallization. Calculated on the basis of the concentration of tungsten trioxide obtained in the stripping liquid, the yield is up to 89%.

Embodiment 3

[0031] Take 8L of industrial solution containing tungsten, sulfuric acid and phosphoric acid, in which tungsten trioxide is 150g / L, phosphoric acid is 60g / L, sulfuric acid is 1mol / L, iron ion is 2.4g / L, manganese ion is 3g / L, calcium ion is 0.7g / L, Sodium ions 15g / L and other impurity ions. First adjust the concentration of sulfuric acid to 2mol / L; then use 50% decyl alcohol as the extractant, and the diluent is sulfonated kerosene, and then carry out five-stage countercurrent extraction, the ratio is O / A=3:1; the organic phase is loaded with water As a stripping reagent, five-stage countercurrent stripping is carried out, and the ratio O / A=6:1. The concentration of tungsten trioxide in the stripping solution is 285.2g / L, and high-purity white phosphotungstic acid is obtained by evaporation and crystallization. Calculated on the basis of the concentration of tungsten trioxide obtained in the stripping liquid, the yield is up to 95.1%.

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Abstract

The invention discloses a method for preparing phosphotungstic acid crystals from tungstenic mixed phosphoric and sulfuric acid solution. The method includes the following steps: firstly, regulating the concentration of sulfuric acid in the tungstenic mixed phosphoric and sulfuric acid solution; adding an organic alcohol extraction agent for extraction to obtain a loaded organic phase; subjecting the obtained loaded organic phase to reverse extraction with distilled water to obtain reverse extract liquid; subjecting the reverse extract liquid to heating and evaporative crystallization to obtain the phosphotungstic acid crystals. The method is simple in process, short in process flow, low in preparation cost, free of pollution to the environment and easy 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 preparing phosphotungstic acid crystals from a tungsten-containing sulfur-phosphorus mixed acid solution. Background technique [0002] The heteropolyacid of Keggin structure is one of the most active catalysts used in acid-catalyzed reactions and redox reactions. It has good catalytic performance for the hydration and esterification of olefins, the etherification of epoxides, the condensation of olefins and aldehydes, the alkylation of olefins, the epoxidation of olefins, and the aromatication of alkylenes. 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...

Claims

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Application Information

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