Method for preparing phosphotungstic acid using ammonium paratungstate as raw material

A technology of ammonium paratungstate and phosphotungstic acid, applied in chemical instruments and methods, tungsten compounds, phosphorus oxyacids, etc., to achieve high yield, suitable for large-scale industrial production, and reduce production costs

Active Publication Date: 2009-02-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] To sum up, at present, most of the preparations of phosphotungstic acid use sodium tungstate as raw material, and ammonium paratungstate (NH 4 ) 10 [W 12 o 42 h 2 ]·4H 2 Reports and patents on preparation of phosphotungstic acid by O (abbreviated as APT)

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  • Method for preparing phosphotungstic acid using ammonium paratungstate as raw material
  • Method for preparing phosphotungstic acid using ammonium paratungstate as raw material

Examples

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Embodiment 1

[0037] Weigh 50 grams of concentrated hydrochloric acid and prepare 600 mL of hydrochloric acid solution with a concentration of 0.8 mol / L. Pour the hydrochloric acid solution into a glass beaker, and add 20 grams of ammonium paratungstate powder into the beaker at 15°C (the molar ratio of hydrochloric acid to ammonium paratungstate is 75 : 1), after stirring for 2.0 hours, an active tungstic acid precipitate was generated, left to stand, filtered, and washed.

[0038] Add 18.5 g of the obtained active tungstic acid precipitate into 100 mL of 2.0 mol / L phosphoric acid aqueous solution (the molar ratio of phosphoric acid to ammonium paratungstate is 31:1), raise the temperature to 60°C, and keep the temperature constant for 2 hours to obtain a clear and transparent phosphotungstic acid solution. Evaporate, concentrate, dry, crystallize to obtain 16.24 grams of high-purity white phosphotungstic acid. 3 PW 12 o 40 29H 2 O meter, yield is 74.8%.

Embodiment 2

[0040] Weigh 50 grams of concentrated hydrochloric acid and prepare 600 mL of hydrochloric acid solution with a concentration of 0.8mol / L. Pour the hydrochloric acid solution into a glass beaker, and add 20 grams of ammonium paratungstate powder into the beaker at 5°C (the molar ratio of hydrochloric acid to ammonium paratungstate is 75 : 1), stirring and reacting for 3.0 hours to generate active tungstic acid precipitation, then add 1.0 gram of aging agent aluminum chloride (molar concentration is 0.01mol / L), filter after aging for 2 hours, wash and leave standstill, filter, wash.

[0041] Add 19.8 g of the obtained active tungstic acid precipitate into 500 mL of 0.06 mol / L phosphoric acid aqueous solution (the molar ratio of phosphoric acid to ammonium paratungstate is 5:1), raise the temperature to 55°C, and keep the temperature for 2 hours to obtain a clear and transparent phosphotungstic acid solution. Evaporate, concentrate, dry, and crystallize to obtain 16.55 grams of h...

Embodiment 3

[0043] Weigh 50 grams of concentrated hydrochloric acid and prepare 600 mL of hydrochloric acid solution with a concentration of 0.8 mol / L. Pour the hydrochloric acid solution into a glass beaker, and add 20 grams of ammonium paratungstate powder into the beaker at 15°C (the molar ratio of hydrochloric acid to ammonium paratungstate is 75 : 1), stirred and reacted for 1.5 hours to generate active tungstic acid precipitates, left standstill, filtered, and washed.

[0044] Add 18.8 g of the obtained active tungstic acid precipitate into 500 mL of 0.06 mol / L phosphoric acid aqueous solution (the molar ratio of phosphoric acid to ammonium paratungstate is 5:1), raise the temperature to 55°C, and keep the temperature for 2 hours to obtain a clear and transparent phosphotungstic acid solution. Add 10 grams of hydrochloric acid (molar concentration is 0.2mol / L) with a weight concentration of 36% to this solution at 55°C to form a white precipitate, filter, dry, and crystallize to obta...

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Abstract

The invention discloses a method for preparing phosphotungstic acid by taking ammonium paratungstate as raw material. It comprises following steps: (1) mixing ammonium paratungstate with inorganic acid at 0-60 Deg. C and getting active tungstate, and the molar ratio between inorganic acid and ammonium paratungstate is 10: 1 -100: 1; (2) mixing active tungstate and phosphoric acid at 20-90 Deg. C and getting phosphotungstic acid solution; and the molar ratio between phosphoric acid which accounts as H3PO4 and ammonium paratungstate is 1.1: 1- 50: 1; (3) making phosphotungstic acid precipitate from solution, drying, crystallizing and getting crystal phosphotungstic acid. By adding inorganic acid precipitant to precipitate phosphotungstic acid, then crying and crystallizing, it can increase its purity further. The invention is characterized by simple process, non use of high concentration of strong acid and flammable organic extractant, low content of phosphate radical in product and suitility for being uses as catalyst.

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 by using ammonium paratungstate as raw material. 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 kind of structure is both It has strong acidity and redox properties, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/16C01G41/00B01J27/188
Inventor 何奕工项祖红
Owner CHINA PETROLEUM & CHEM CORP
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