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Method for preparing phosphotungstic heteropoly acid with Keggin structure

A technology of phosphotungstic heteropolyacid and tungstate, which is applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of reducing the safety of large-scale industrial production, complex preparation process, and large amount of organic solvents. Achieve the effect of high product output rate, simple process and reduced corrosion

Inactive Publication Date: 2012-09-12
CENT SOUTH UNIV
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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 heteropolyacid contains a large amount of phosphate radicals.
CN1544483A improved the appeal method, used organic solvent C 2 -C 20 Ether is used for complex extraction to reduce the phosphate in phosphotungstic heteropoly acid, but the amount of organic solvent is large, which reduces the safety of large-scale industrial production
This method needs to use a large amount of concentrated sulfuric acid, corrode equipment, and the impurity content in phosphotungstic heteropoly acid is high, and the production cycle is extremely long

Method used

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  • Method for preparing phosphotungstic heteropoly acid with Keggin structure
  • Method for preparing phosphotungstic heteropoly acid with Keggin structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 16.5 grams of sodium tungstate dihydrate, add 50 mL of deionized water, and stir until the sodium tungstate is completely dissolved; adjust the pH of the solution to 7.0 with 3 mol / L hydrochloric acid; continue stirring for 2 hours, and then transfer to 100 mL of polytetrafluoroethylene In an ethylene-lined autoclave, stand at 135°C for 10 hours, cool naturally, transfer the solution into a beaker, add 0.5mol / L phosphoric acid solution dropwise to pH=2.25, stir for 4 hours, add potassium chloride When the solution is saturated, crystallize overnight at 15°C, purify, filter, and dry to constant weight to obtain 13.48 g of white product. 3 PW 12 o 40 29H 2O meter, yield is 95%. The FT-IR spectrum of the product phosphotungstic acid is shown in figure 1 . figure 1 From figure 1 It can be seen that the product is at 1079cm -1 、983cm -1 、890cm -1 、800cm -1 、595cm -1 、525cm -1 、483 cm -1 、426 cm -1 There is an obvious absorption peak at , which is compl...

Embodiment 2

[0030] Weigh 16.5 grams of sodium tungstate dihydrate, add 100 mL of deionized water, and stir until the sodium tungstate is completely dissolved; adjust the pH of the solution to 7.0 with 3 mol / L hydrochloric acid, continue stirring for 2 hours, and then transfer to 100 mL of polytetrafluoroethylene In the lined high-pressure reactor, keep it at a constant temperature of 120°C for 10 hours, cool it naturally, transfer the solution into a beaker, add 2mol / L phosphoric acid solution dropwise to pH=2.5, stir for 4 hours, add potassium chloride to Saturated, crystallized overnight at 15°C, purified, filtered, and dried to constant weight to obtain 12.1 g of white product, press H 3 PW 12 o 40 29H 2 O meter, productive rate is 85.5%.

Embodiment 3

[0032] Weigh 16.5 grams of sodium tungstate dihydrate, add 50 mL of deionized water, and stir until the sodium tungstate is completely dissolved; adjust the pH of the solution to 6.5 with 3mol / L hydrochloric acid, continue stirring for 2 hours, and then transfer to 100 mL of polytetrafluoroethylene In a lined high-pressure reactor, keep it standing at 150°C for 10 hours, cool naturally, transfer the solution into a beaker, add 0.5mol / L phosphoric acid solution to pH=2.5, stir for 2 hours, add sodium chloride to the solution Saturated, crystallized overnight at 15°C, purified, filtered, and dried to constant weight to obtain 11.2 g of white product, press H 3 PW 12 o 40 29H 2 O meter, productive rate 79%.

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Abstract

The invention discloses a method for preparing phosphotungstic heteropoly acid with a Keggin structure. The method comprises the following steps of: (1) contacting a tungstate solution and an inorganic acid solution; (2) transferring the solution to a high-pressure reaction kettle, and activating at high temperature under high pressure to obtain an active intermediate; (3) contacting the obtained substance and phosphoric acid to obtain a phosphotungstic acid solution; and (4) adding an inorganic salt precipitator into the phosphotungstic acid solution, precipitating phosphotungstic acid by salting-out and crystallization, filtering, purifying and drying to obtain the Keggin phosphotungstic heteropoly acid. By the method, a process flow is simple, the yield of the heteropoly acid is high, and the preparation cost is reduced obviously; high-concentration strong acid in the conventional method is not used in the preparation process, so that the corrosivity to equipment is reduced greatly; and an inflammable low-boiling point organic extractant is not used, and the safety of preparation is improved greatly.

Description

technical field [0001] The invention relates to a method for preparing phosphotungstic heteropolyacid with Keggin structure, in particular to a method for preparing heteropolyacid with Keggin structure with high purity through acidification-hydrothermal activation-phosphorylation-inorganic salt precipitation and crystallization using tungstate as raw material sour method. Background technique [0002] The heteropoly acid of Keggin structure generally refers to the inorganic compound expressed by the following chemical formula: H x Y M 12 o 40 ·nH 2 O, where: Y: represents P, Si and other atoms, called heteroatoms or central atoms, M: represents W, Mo and other atoms, called coordination atoms or polyatoms, x: is 3 or 4, n is 0~30 positive integer of . [0003] Phosphotungstic heteropolyacid with Keggin structure is the most typical type of heteropolyacid, which refers to the heteropolyacid with Kegein structure, with tungsten atom as coordination atom, phosphorus atom a...

Claims

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Application Information

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IPC IPC(8): C01G41/00
Inventor 陈启元李洁黎东维
Owner CENT SOUTH UNIV
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