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High-purity Wells-Dawson phosphotungstic acid and preparation method thereof

A high-purity technology of phosphotungstic acid, which is applied in the preparation of tungsten compounds, chemical instruments and methods, tungsten compounds, etc., can solve the problems of low product purity, and achieve the effects of simple process, improved yield and purity, and high purity

Active Publication Date: 2017-05-31
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] R.G.Finke (Inorg.Chem.26 (1987) 3886-3896), C.R.Graham (Inorg.Chem.47 (2008) 3679-3686), C.H.M.Hu (J.Catal.143 (1993) 437-448) et al. The preparation method about Wells-Dawson type phosphotungstic acid is disclosed, but it all uses sodium tungstate as raw material, and the residual impurities such as sodium phosphotungstate or sodium ions in the prepared Wells-Dawson type phosphotungstic acid are relatively high, The purity of the final product is not high

Method used

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  • High-purity Wells-Dawson phosphotungstic acid and preparation method thereof
  • High-purity Wells-Dawson phosphotungstic acid and preparation method thereof
  • High-purity Wells-Dawson phosphotungstic acid and preparation method thereof

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preparation example Construction

[0026] The preparation method of the high-purity Wells-Dawson type phosphotungstic acid provided in this embodiment comprises the following steps:

[0027] Heat phosphoric acid to 80-100°C; divide tungstic acid into 6-10 parts, and add them to 80-100°C deionized water in batches within 1-5 hours and mix evenly to obtain an aqueous solution of tungstic acid. In the aqueous solution of tungstic acid The molar concentration of tungstic acid is 1.5-3mol / L;

[0028] Add the aqueous solution of tungstic acid at 80-100°C to phosphoric acid at 80-100°C, and heat it in a water bath or microwave to 100-140°C for 12-24 hours to obtain a phosphotungstic acid solution, wherein the phosphoric acid and tungstic acid The molar ratio is 7.5-15:1; preferably, the aqueous solution of tungstic acid is mixed with phosphoric acid and heated to 105-125°C for 12-24 hours to obtain a phosphotungstic acid solution;

[0029] Mix phosphotungstic acid solution with inorganic acid and place it for 3-5 hou...

Embodiment 1

[0035] This embodiment provides a preparation method of high-purity Wells-Dawson type phosphotungstic acid, comprising the following steps:

[0036]Add 20ml of phosphoric acid into a 100ml four-necked flask with a cooling reflux device, stir and heat to 80°C; divide 10.0g of tungstic acid into 6 equal parts and dissolve them in batches in 20ml of deionized water within 1 hour to obtain an aqueous solution of tungstic acid , the temperature of the deionized water is kept at 80°C, then the aqueous solution of tungstic acid is added into the four-necked flask and stirred evenly with phosphoric acid, the four-necked flask is put into the hydrothermal synthesis kettle and heated to 100°C for 12 hours, cooled Get a phosphotungstic acid solution at room temperature, add 10ml of hydrochloric acid to the phosphotungstic acid solution and let it stand for 3 hours for acidification, then pour the acidified phosphotungstic acid solution into the separatory funnel, add 50ml of ether into th...

Embodiment 2

[0038] This embodiment provides a preparation method of high-purity Wells-Dawson type phosphotungstic acid, comprising the following steps:

[0039] Add 40ml of phosphoric acid into a 100ml four-necked flask with a cooling reflux device, stir and heat to 100°C; divide 10.0g of tungstic acid into 10 equal parts and dissolve them in batches in 20ml of deionized water within 5 hours to obtain an aqueous solution of tungstic acid , the temperature of the deionized water is kept at 100°C, then the aqueous solution of tungstic acid is added into the four-necked flask and stirred evenly, the four-necked flask is put into the synthesis kettle and heated by microwave to 140°C for 24 hours, then cooled to room temperature to obtain Phosphotungstic acid solution, add 15ml of hydrochloric acid to the phosphotungstic acid solution and leave it for 5 hours for acidification, then pour the acidified phosphotungstic acid solution into the separatory funnel, add 80ml of ether to the separatory ...

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Abstract

The invention relates to a high-purity Wells-Dawson phosphotungstic acid and a preparation method thereof, which belong to the field of phosphotungstic acid preparation. The preparation method for the high-purity Wells-Dawson phosphotungstic acid includes the following steps: an aqueous solution of tungstic acid is added into phosphoric acid which is 80 DEG C to 100 DEG C, reaction then takes place under 100 DEG C to 140 DEG C for 12 to 24 hours, so that a phosphotungstic acid solution is obtained, and the molar ratio of the phosphoric acid to the tungstic acid is (7.5 to 15) to 1; and after the phosphotungstic acid solution is acidized, diethyl ether is used for extraction and separation. Since the preparation method for the high-purity Wells-Dawson phosphotungstic acid uses the tungstic acid to replace sodium tungstate as a material, the introduction of Na ions into the product is prevented, and the yield and purity of the phosphotungstic acid product are increased; and moreover, the preparation method is simple in process, is convenient to operate, and is suitable for use in industrialized mass production. The invention further discloses the high-purity Wells-Dawson phosphotungstic acid which is prepared by using the preparation method.

Description

technical field [0001] The invention relates to the field of phosphotungstic acid preparation, and in particular to a high-purity Wells-Dawson type phosphotungstic acid and a preparation method thereof. Background technique [0002] Heteropolyacids (Polyoxometalates) are heteroatom (such as P, Si, Co, etc.) oxyacids and polyatomic (such as Mo, W, V, etc.) Acids, which have both strong acidity and redox properties, are widely used in the field of catalysts. Phosphotungstic acid is a commonly used heteropolyacid, which has strong acidity, excellent conductivity and strong oxidation performance, and has been widely used in the field of photocatalytic degradation of organic wastewater. Common phosphotungstic acid has two structures: Keggin type ([XM 12 o 40 ] n- ) and Wells-Dawson type ([X 2 m 18 o 62 ] n- ), among them, Keggin-type phosphotungstic acid is widely used, and there are many related research papers and patents, but Wells-Dawson-type phosphotungstic acid has ...

Claims

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Application Information

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IPC IPC(8): C01G41/00B01J27/188
CPCB01J27/188C01G41/003C01P2002/72C01P2002/82C01P2002/84C01P2006/80
Inventor 丁建飞薛雅琦马田林邵荣许伟
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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