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Preparation method of impurity-free Preyssler type heteropolyacid

A heteropolyacid, impurity-free technology, applied in chemical instruments and methods, inorganic chemistry, phosphorus compounds, etc., can solve the problem of low product purity, achieve the effect of simple process, convenient operation, and improved yield and purity

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, so that the purity of the final product is not high

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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 a kind of preparation method of impurity-free Preyssler type heteropolyacid, comprising the following steps:

[0028] 1. Dissolve 33g of sodium tungstate in 30mL of deionized water, add 26.5mL of phosphoric acid solution with a mass fraction of 85% dropwise within 1 hour under stirring conditions, then put the above mixed solution into the reaction kettle, and put it under the condition of 120℃ 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 NaCl 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 so...

Embodiment 2

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

[0036] 1. Dissolve 30g of sodium tungstate in 30mL of deionized water, add 30.5mL of phosphoric acid solution with a mass fraction of 85% dropwise within 1.5 hours under stirring conditions, and then put the above mixed solution into the reaction kettle. 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 10mL water and 10gNaCl 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 white solid and dissolve it in 30 mL of hot wat...

Embodiment 3

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

[0044] 1. Dissolve 28g of sodium tungstate in 30mL of deionized water, add 28mL of phosphoric acid solution with a mass fraction of 85% dropwise within 1.5 hours under stirring conditions, and then put the above mixed solution into the reaction kettle. After 18 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 water and 8gNaCl to 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 water at 90°C. Af...

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

Description

technical field [0001] The invention relates to the 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 properties has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45
CPCC01B25/45C01P2002/82C01P2002/84
Inventor 马田林王宝雪刘晶晶王妮徐祥刘学立
Owner CHUZHOU UNIV
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