Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

The preparation method of impurity-free preyssler type heteropoly acid

A heteropolyacid, impurity-free technology, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of reducing product purity and high content, and achieve improvement Yield and purity, simple process and convenient operation

Active Publication Date: 2022-07-22
CHUZHOU UNIV
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 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 about the Preyssler type heteropolyacid, but it is all with potassium chloride and potassium acetate as raw material , 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • The preparation method of impurity-free preyssler type heteropoly acid
  • The preparation method of impurity-free preyssler type heteropoly acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The present embodiment provides the preparation method of impurity-free Preyssler-type heteropolyacid, comprising the following steps:

[0027] 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 reactor, at 120 ℃ condition The reaction was continued for 12 h to obtain a Preyssler-type heteropolyacid solution containing impurities.

[0028] 2. The Preyssler-type heteropolyacid solution containing impurities was taken out and cooled to room temperature to obtain a pale yellow solution.

[0029] 3. Add 15 mL of water and 10 g of ammonium chloride to the light yellow solution, stir well to form a precipitate, and filter with suction to take the white solid part.

[0030] 4. Wash the white solid with anhydrous methanol. After the washing is completed, drain the methanol on the surface of the white s...

Embodiment 2

[0034] The present embodiment provides the preparation method of impurity-free Preyssler-type heteropolyacid, comprising the following steps:

[0035] 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, and then put the above mixed solution into the reaction kettle, under the condition of 100 ℃ The reaction was continued for 18 h to obtain a Preyssler-type heteropolyacid solution containing impurities.

[0036] 2. The Preyssler-type heteropolyacid solution containing impurities was taken out and cooled to room temperature to obtain a pale yellow solution.

[0037] 3. Add 15 mL of water and 10 g of ammonium chloride to the light yellow solution, stir well to form a precipitate, and filter with suction to take the white solid part.

[0038] 4. Wash the white solid with anhydrous methanol. After the washing is completed, drain the methanol on the surf...

Embodiment 3

[0042] The present embodiment provides the preparation method of impurity-free Preyssler-type heteropolyacid, comprising the following steps:

[0043] 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, under the condition of 120 ℃ The reaction was carried out for 15h to obtain a Preyssler-type heteropolyacid solution containing impurities.

[0044] 2. The Preyssler-type heteropolyacid solution containing impurities was taken out and cooled to room temperature to obtain a pale yellow solution.

[0045] 3. Add 10 mL of water and 8 g of ammonium chloride to the light yellow solution, stir well to form a precipitate, and filter with suction to take the white solid part.

[0046] 4. Wash the white solid with anhydrous methanol. After the washing is completed, drain the methanol on the surfac...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
quality scoreaaaaaaaaaa
Login to View More

Abstract

The invention discloses an impurity-free Preyssler-type heteropoly acid and a preparation method thereof, belonging to the field of heteropoly acid preparation. The preparation method of the Preyssler type heteropolyacid comprises the following steps: adding phosphoric acid to the aqueous solution of sodium tungstate, and then reacting at 100-140° C. in the reactor for 12-24 hours, and the molar ratio of phosphoric acid to sodium tungstate is 4- 10:1; after cooling to room temperature, add ammonium chloride for suction filtration; wash with methanol solution and recrystallize; add a small amount of sorbic acid and ion-exchange the heteropolyacid solution; finally, vacuum dry the eluent. The preparation method of the impurity-free Preyssler-type heteropolyacid does not add any potassium ions, and at the same time saves the potassium acetate washing step, avoids the introduction of potassium ions into the product, and improves the yield and purity of the finished heteropolyacid, In addition, the preparation method has the advantages of simple process and convenient operation, and is suitable for industrialized large-scale production.

Description

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

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com