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Preparation method of impurity-free Preyssler type heteropolyacid

A heteropolyacid, impurity-free technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as high content and reduced product purity, and achieve Simple process, improved yield and purity, and convenient operation

Active Publication Date: 2020-02-18
CHUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] M. H. Alizadeh (J. Am. Chem. Soc. 107 (1985) 2662-2669; J. Mol. Catal. A-Chem. 206 (2003) 89-93), R. Hekmatshoar (Catal. Commun. 9 (2008) 837-841), G. Romanelli (Chem. Eng. J. 161 (2010) 355-362) and others reported the preparation method of Preyssler type heteropolyacid, but they all use potassium chloride and potassium acetate as raw materials , the residual content of impurities such as potassium phosphotungstate or potassium ions in the prepared Preyssler type heteropolyacid is relatively high, which reduces the purity of the final product

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  • Preparation method of impurity-free Preyssler type heteropolyacid
  • Preparation method of impurity-free Preyssler type heteropolyacid

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Embodiment 1

[0027] The present embodiment provides the preparation method of impurity-free Preyssler type heteropolyacid, comprising the following steps:

[0028] 1. Dissolve 30g of sodium tungstate in 30mL of deionized water, add 28.5mL of phosphoric acid solution with a mass fraction of 85% dropwise within 2 hours under stirring conditions, and then put the above mixed solution into the reaction kettle. The reaction was carried out for 12 hours to obtain a Preyssler-type heteropolyacid solution containing impurities.

[0029] 2. Take out the Preyssler-type heteropolyacid solution containing impurities and cool it to room temperature to obtain a light yellow solution.

[0030] 3. Add 15mL of water and 10g of ammonium chloride to the light yellow solution, stir well to form a precipitate, and filter with suction to get the white solid part.

[0031] 4. Wash the white solid with anhydrous methanol. After washing, drain the methanol on the surface of the white solid and dissolve it in 30 m...

Embodiment 2

[0035] The present embodiment provides the preparation method of impurity-free Preyssler type heteropolyacid, comprising the following steps:

[0036] 1. Dissolve 33g of sodium tungstate in 30mL of deionized water, add 30.5mL of phosphoric acid solution with a mass fraction of 85% dropwise within 4 hours under stirring conditions, then put the above mixed solution into the reaction kettle, and put it under the condition of 100℃ The reaction was carried out for 18 hours to obtain a Preyssler-type heteropolyacid solution containing impurities.

[0037] 2. Take out the Preyssler-type heteropolyacid solution containing impurities and cool it to room temperature to obtain a light yellow solution.

[0038] 3. Add 15mL of water and 10g of ammonium chloride to the light yellow solution, stir well to form a precipitate, and filter with suction to get the white solid part.

[0039] 4. Wash the white solid with anhydrous methanol. After washing, drain the methanol on the surface of the ...

Embodiment 3

[0043] The present embodiment provides the preparation method of impurity-free Preyssler type heteropolyacid, comprising the following steps:

[0044] 1. Dissolve 27g of sodium tungstate in 30mL of deionized water, add 28mL of phosphoric acid solution with a mass fraction of 85% dropwise within 2 hours under stirring conditions, and then put the above mixed solution into the reaction kettle. After 15 hours of reaction, a Preyssler-type heteropolyacid solution containing impurities was obtained.

[0045] 2. Take out the Preyssler-type heteropolyacid solution containing impurities and cool it to room temperature to obtain a light yellow solution.

[0046] 3. Add 10mL of water and 8g of ammonium chloride into the light yellow solution, stir well to form a precipitate, and filter with suction to get the white solid part.

[0047] 4. Wash the white solid with anhydrous methanol. After washing, drain the methanol on the surface of the white solid and dissolve it in 30 mL of hot wat...

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Abstract

The invention discloses impurity-free Preyssler type heteropolyacid and a preparation method thereof, and belongs to the field of heteropolyacid preparation. The preparation method of the Preyssler type heteropolyacid comprises the following steps: adding phosphoric acid into an aqueous solution of sodium tungstate, and then reacting in a reaction kettle at 100-140 DEG C for 12-24 hours, wherein the molar ratio of phosphoric acid to sodium tungstate being (4-10): 1; after cooling to room temperature, adding ammonium chloride for suction filtration; washing with a methanol solution and recrystallizing; adding a small amount of sorbic acid and carrying out ion exchange on the heteropolyacid solution; and finally, carrying out vacuum drying on eluent. According to the impurity-free Preysslertype heteropolyacid preparation method, no potassium ions are added, meanwhile, the potassium acetate washing step is omitted, introduction of potassium ions into the product is avoided, the yield andpurity of the heteropolyacid finished product are improved, and the preparation method is simple in process, convenient to operate and suitable for industrial large-scale production and use.

Description

technical field [0001] The invention relates to the technical field of preparation of heteropolyacids, in particular to a method for preparing impurity-free Preyssler type heteropolyacids. Background technique [0002] Heteropoly acids (Polyoxometalates) are a class of oxygen-containing polyacid compounds formed by heteroatoms (such as P, Si, Fe, As, etc.) and polyatoms (such as W, V, Mo, etc.) through oxygen atom bridge coordination. . Heteropolyacids have the properties of strong proton acidity, strong redox ability, high thermal stability, non-toxic, odorless, and non-volatile properties, so they have been widely used in the field of catalysis. [0003] According to the ratio of heteroatoms to polyatoms, heteropolyacids can be divided into Keggin type, Wells-Dawson type, Preyssler type, Anderson type, Waugh type and Silverton type. Keggin-type and Wells-Dawson-type heteropolyacids are the two most widely studied types, and the understanding of their structures and prope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J27/188
CPCB01J27/188
Inventor 马田林刘晶晶王妮王宝雪徐祥刘学立
Owner CHUZHOU UNIV
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