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Method for preparing high-purity phosphotungsticacid

A technology of pure phosphotungstic acid and phosphotungstic acid, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of large amount of organic solvent, complicated preparation process, and reduce the safety of large-scale industrial production. The effect of reduced corrosion, simple process and improved safety

Active Publication Date: 2007-06-13
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 obtained phosphotungstic acid contains a large amount of phosphate
CN1,544,483A improved the above method by using organic solvent C 2 -C 20 Ether is used for complex extraction to reduce the phosphate in phosphotungstic acid, but the amount of organic solvent is large, which reduces the safety of large-scale industrial production

Method used

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  • Method for preparing high-purity phosphotungsticacid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh 50 grams of sodium tungstate to make 1000ml of sodium tungstate aqueous solution with a concentration of 0.15mol / L; weigh 50 grams of concentrated hydrochloric acid to make 600ml of hydrochloric acid solution with a concentration of 0.8mol / L (H + with WO 4 2- The molar ratio is 3.2), pour this hydrochloric acid solution into a glass beaker, add the prepared sodium tungstate solution dropwise into the beaker at 15°C, let stand after the dropwise addition, filter, and wash to obtain active tungstic acid precipitate.

[0038] Add 38.5 g of the obtained active tungstic acid precipitate into 1000 ml of 0.06 mol / L phosphoric acid aqueous solution, raise the temperature to 55°C, and obtain a clear and transparent phosphotungstic acid solution. Adding 150 grams of 36% hydrochloric acid (molar concentration is 1.3 mol / L) to this solution at 12° C. generates a white precipitate, which is filtered and crystallized to obtain 33.20 grams of high-purity white phosphotungstic a...

Embodiment 2

[0040] Take by weighing 50 grams of sodium tungstate, make it into 1875ml of sodium tungstate aqueous solution with a concentration of 0.08mol / L; take 25 grams of concentrated hydrochloric acid, make it into 560ml of hydrochloric acid solution with a concentration of 0.4mol / L + with WO 4 2- The molar ratio is 1.5), pour this hydrochloric acid solution into a glass beaker, add the prepared sodium tungstate solution dropwise into the beaker at 45°C, and add 4.0 grams of aging agent aluminum chloride (molar concentration: 0.01mol / L), filter after aging for 0.5 hours, and wash.

[0041] Add 41.5 g of the obtained active tungstic acid precipitate into 1000 ml of 0.06 mol / L phosphoric acid aqueous solution, and fully stir at room temperature for 2 hours to obtain a clear and transparent phosphotungstic acid solution. Add 25 grams of hydrochloric acid (molar concentration is 0.24mol / L) that weight concentration is 36% to this solution at 74 ℃, generate white precipitate, filter, cr...

Embodiment 3

[0045] Take by weighing 50 grams of sodium tungstate, be made into concentration and be 150ml of sodium tungstate aqueous solution of 1.0mol / l; Take by weighing 100 grams of concentrated nitric acid (H + with WO 4 2- Molar ratio is 6.7), is made into the nitric acid solution 400ml that concentration is 2.5mol / l. Add the prepared nitric acid solution dropwise to the sodium tungstate solution at 8°C, then add 10 grams of aluminum nitrate (molar concentration: 0.049 mol / L), age for 8 hours, filter and wash. Add 39.2 grams of the obtained active tungstic acid precipitate into 100ml of 3.0mol / L phosphoric acid aqueous solution, stir well at room temperature, then raise the temperature to 80°C to obtain a clear and transparent phosphotungstic acid solution; add 100g of phosphotungstic acid to the solution at 50°C Weight concentration is 85% sulfuric acid (molar concentration is 5mol / L), generates white precipitate, filters, and crystallizes, promptly obtains the white phosphotungs...

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Abstract

This invention introduces a method for preparing pure PTA with sodium wolframate as the raw material including : 1, contacting sodium wolframate solution with inorganic acid solution till depositing active tungstenic acid, 2, contacting the deposition with phosphoric acid till dissolving the active tungstenic completely to get PTA solution, 3, adding an inorganic acid precipitator to the solution to deposit, filter and crystallize the deposition to get pure PTA, in which, the mol concentration of the precipitator in the system is 0.1-6mol / 1.

Description

technical field [0001] The invention relates to a method for preparing tungsten-containing heteropolyacid, more specifically, the invention relates to a method for preparing high-purity phosphotungstic acid. Background technique [0002] The heteropoly acid of Keggin structure generally refers to the inorganic compound expressed by the following general chemical formula: [0003] h k YZ 12 o 40 ·nH 2 o [0004] in: [0005] Y: Represents atoms such as P and Si, which are called central atoms or heteroatoms. [0006] Z: Represents atoms such as Mo and W, which are called polyatoms. [0007] k: 3 or 4 [0008] n: a positive integer from 0 to 30 [0009] The heteropolyacid of Keggin structure is a kind of acid with cage structure and pores obtained by acidifying, condensing and dehydrating two or more inorganic oxoacid ions. The heteropolyacid of this type of structure has both strong acidity and It also has redox properties, so it can be used as an acid catalyst or a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00B01J27/188
Inventor 何奕工项祖红
Owner CHINA PETROLEUM & CHEM CORP
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