Method for preparing phosphotungstic heteropoly acid solution

A technology of phosphotungstic heteropoly acid and solution, which is applied in the preparation of tungsten compounds, chemical instruments and methods, tungsten compounds, etc., to achieve the effects of low equipment corrosion, high yield and good quality

Active Publication Date: 2017-07-25
CENT SOUTH UNIV
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Problems solved by technology

[0008] In order to solve the series of problems caused by the need to add a large amount of inorganic acid in the existing preparation method, the present invention provides a new method for preparing phosphotungstic heteropoly acid solution, which uses the combination of bipolar membrane electrodialysis and ion exchange method to prepare phosphorus The tungsten heteropolyacid solution aims to realize the acid adjustment mode without external acid in the preparation process, and remove most of the cations in the bipolar membrane electrodialysis process, reduce the burden of ion exchange transformation and impurity removal, and overcome the shortcomings of the traditional process. Obtain phosphotungstic heteropolyacid solution for preparing high-quality phosphotungstic heteropolyacid products

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  • Method for preparing phosphotungstic heteropoly acid solution
  • Method for preparing phosphotungstic heteropoly acid solution
  • Method for preparing phosphotungstic heteropoly acid solution

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Embodiment 1

[0065] The first stage of bipolar membrane electrodialysis: the feed liquid chamber (salt chamber) contains WO 3182.8g / L sodium tungstate solution, the initial pH value is 12.91; the alkali chamber solution is 0.05mol / L NaOH solution; the pole chamber solution is 0.1mol / L NaOH solution; the initial volume of the three-chamber solution is 4L. The current density of the first bipolar membrane electrodialysis is 500A / m 2 , the electrolysis time is 40min, and the tungsten-containing sodium salt solution with pH value of 6.78 is obtained, WO 3 The concentration is 228.5g / L;

[0066] Transformation: After the first stage of bipolar membrane electrodialysis, the solution is boiled for 4 hours for transformation; after transformation, the solution can be diluted with an appropriate amount of pure water, and sodium dihydrogen phosphate is added according to the P / W molar mass ratio of 1 / 12 to obtain WO containing 3 The mixed solution with a concentration of 155.6g / L has a pH of 7.89;...

Embodiment 2

[0070] The first stage of bipolar membrane electrodialysis: the material-liquid chamber contains WO 3 50g / L ammonium tungstate solution, add phosphoric acid according to the P / W molar mass ratio of 1 / 9, the initial pH value is 9.50, and the alkali chamber solution is 1.0mol / L NH 4 HCO 3 solution; pole chamber solution is 0.5mol / LNH 4 OH solution; the initial volume of the three-chamber solution is 5L. The current density of the first bipolar membrane electrodialysis is 750A / m 2 , the electrolysis time is 25min, the mixed solution of tungsten and phosphorus with pH value of 7.5 is obtained, WO 3 The concentration is 62.5g / L;

[0071] Transformation: After the first stage of bipolar membrane electrodialysis, the solution was transformed at 90 °C for 48 h; 3 The mixed solution with a concentration of 65.3g / L, the pH value is 7.25;

[0072] The second-stage bipolar membrane electrodialysis: take 4.1L of the mixed solution for the second-stage bipolar membrane electrodialysis...

Embodiment 3

[0075] The first stage of bipolar membrane electrodialysis: the material-liquid chamber contains WO 3 300.0g / L sodium tungstate solution, initial pH value is 13.5; alkali chamber solution is 1.0mol / L NaHCO 3 solution; the polar compartment solution is 1.0mol / L NaOH solution; the initial volume of the three compartment solutions is 4L. The current density of the first bipolar membrane electrodialysis is 600A / m 2 , the electrolysis time is 45min, and the tungsten-containing sodium salt solution with pH value of 5.50 is obtained, WO 3 The concentration is 375g / L;

[0076] Transformation: After the first stage of bipolar membrane electrodialysis, add sodium dihydrogen phosphate to the solution with a P / W molar mass ratio of 1 / 11, and boil for 12 hours for transformation; the transformed solution can be diluted with an appropriate amount of pure water to obtain WO containing 3 The mixed solution with a concentration of 220.5g / L, the pH value is 8.02;

[0077] The second stage o...

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Abstract

The invention discloses a method for preparing a phosphotungstic heteropoly acid solution. The method comprises the following steps: performing first-section bipolar membrane electrodialysis on a tungstate solution (or a mixed solution of tungsten and phosphorus), so the pH value of the solution is reduced to 5.5-7.5; performing heating conversion after phosphorous coordination for one-section electrodialysis solution (or the mixed solution of the tungsten and the phosphorus is directly subjected to heating conversion after one-section electrodialysis); cooling the solution, then performing second-section bipolar membrane electrodialysis, and controlling the pH value to be 1.0-3.0 to obtain a heteropolyphosphatotungstate solution; performing ion exchange transformation decontamination to obtain the phosphotungstic heteropoly acid solution. According to the method, inorganic acid is not consumed, and impurity anions are not introduced, so that not only a tungstate solution can be acidified, but also most of salt cations can be removed, thereby greatly reducing burdens on subsequent ion exchange for removing the salt cations. The obtained phosphotungstic heteropoly acid solution can be used for preparing a high-quality phosphotungstic heteropoly acid product, and the method for preparing the phosphotungstic heteropoly acid solution is a phosphotungstic heteropoly acid solution preparation process which is efficient in cleanness.

Description

technical field [0001] The invention belongs to the technical field of heteropoly acid preparation, in particular to a method for preparing phosphotungstic heteropoly acid solution. Background technique [0002] Because phosphotungstic heteropolyacid has the characteristics of high relative molecular weight, high degree of hydration, high solubility in water and some organic solvents, strong oxidation performance, strong acidity, etc., it has been widely used in functional material preparation, catalysis, phase transfer and other fields. widely used. [0003] Although there are many preparation processes of phosphotungstic heteropoly acid, fundamentally speaking, they are all based on two basic steps of "acidification" and "separation". Under the condition of high temperature, the tungstate solution and the soluble solution containing P are mixed and then acidified to form phosphotungstic heteropoly acid salt. According to the classification of acidification methods, there...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00B01D61/44
CPCB01D61/445B01D2311/2684C01G41/003C01P2002/72C01P2006/80
Inventor 张贵清关文娟姚琨李青刚曹佐英曾理肖连生尚广浩
Owner CENT SOUTH UNIV
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