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Preparation method and application of a weakly water-soluble loaded phosphotungstic heteropoly acid

A phosphotungstic heteropolyacid, water-soluble technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of increasing unsafe hidden dangers and endangering human health , easy-to-corrosion equipment and other problems, to avoid production safety problems, help the protection of the environment, and improve the effect of production safety performance

Active Publication Date: 2019-11-12
CHONGQING TECH & BUSINESS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Though this method avoids the defect of ether acidification preparation method, still there are following deficiencies: (1) although using C n h 2n+1 N + Cl - It is a complexing agent to replace ether, but organic solvents are still used. Most of the organic solvents are poisonous and volatile, which are harmful to human health and cause environmental pollution to a certain extent; (2) Drying and roasting need to be carried out under inert gas nitrogen conditions, increasing Unsafe hidden dangers in the production process, and increased production costs; (3) In order to meet the acidic conditions, concentrated hydrochloric acid needs to be added, which is easy to corrode the equipment, increases the maintenance cost of the equipment, and then increases the production cost

Method used

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  • Preparation method and application of a weakly water-soluble loaded phosphotungstic heteropoly acid
  • Preparation method and application of a weakly water-soluble loaded phosphotungstic heteropoly acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Generation of active tungstic acid

[0025] First weigh sodium tungstate (Na 2 WO 4 2H 2 O) Dissolved in water to obtain sodium tungstate aqueous solution, water volume (ml) and Na 2 WO 4The mass (g) ratio is 10:1, transfer it to a separatory funnel, and set aside; then measure 0.8mol / L HCl solution in a beaker, and the volume of HCl (ml) and Na 2 WO 4 The mass (g) ratio is 10:1; then the sodium tungstate aqueous solution is added dropwise to the HCl solution at a uniform speed to obtain a yellow-green precipitate, and stirred; after the sodium tungstate is completely added dropwise, continue to stir for 40 minutes, deposit for 2 hours, and suction filter to obtain a yellow-green precipitate. The green solid is tungstic acid.

[0026] (2) Preparation of water-soluble phosphotungstic heteropolyacid

[0027] After step (1) is completed, first follow H 3 PO 4 Volume (ml) and Na 2 WO 4 The mass (g) ratio is 15:1, measure dilute H with a concentration of 0.12m...

Embodiment 2

[0034] A preparation method of a solid heteropolyacid that catalyzes and strengthens the degradation of perilla stalks, the same as in Example 1, wherein:

[0035] In step (1), the volume of water (ml) and Na 2 WO 4 The ratio of mass (g) is 8:1, the concentration of HCl is 0.7mol / L, the volume of HCl (ml) and Na 2 WO 4 The mass (g) ratio is 8:1, the stirring time is 50min, and the deposition is 2.5h.

[0036] In step (2), H 3 PO 4 Volume (ml) and Na 2 WO 4 The mass (g) ratio is 10:1, H 3 PO 4 The concentration is 0.13mol / L, and the stirring time is 50min.

[0037] In step (3), the mass (g) of citric acid is 25% of the mass (g) of sodium tungstate, the mass (g) of the loading matrix is ​​5% of the mass (g) of sodium tungstate, the stirring time is 50min, and the mass of KCl The mass (g) is 8% of the mass (g) of sodium tungstate, and the yield of supported TS-1 phosphotungstic heteropoly acid is 74.48%.

[0038] In step (4), the number of perilla stalks selected is 20...

Embodiment 3

[0041] A preparation method of a solid heteropolyacid that catalyzes and strengthens the degradation of perilla stalks, the same as in Example 1, wherein:

[0042] In step (1), the volume of water (ml) and Na 2 WO 4 The ratio of mass (g) is 15:1, the concentration of HCl is 0.9mol / L, the volume of HCl (ml) and Na 2 WO 4 The mass (g) ratio is 15:1, the stirring time is 60min, and the deposition is 3h.

[0043] In step (2), H 3 PO 4 Volume (ml) and Na 2 WO 4 The mass (g) ratio is 20:1, H 3 PO 4 The concentration is 0.11mol / L, and the stirring time is 60min.

[0044] In step (3), the mass (g) of citric acid is 15% of the mass (g) of sodium tungstate, the mass (g) of the loading matrix is ​​30% of the mass (g) of sodium tungstate, the stirring time is 30min, and the mass of KCl The mass (g) is 12% of the mass (g) of sodium tungstate, and the yield of supported TS-1 phosphotungstic heteropoly acid is 67.09%.

[0045] In step (4), the number of perilla stalks is 40-60 mes...

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Abstract

The invention belongs to the technical field of phosphotungstic heteropoly acid preparation, and particularly relates to a preparation method and application of load type phosphotungstic heteropoly acid with weak water solubility. The invention provides a method for preparing phosphotungstic heteropoly acid by dilute acidification stirring type modification; the method has the advantages that normal temperature and pressure are adopted for preparation conditions, any organic solvent is not used, the operation is simple, and the energy consumption and the cost are low; the prepared phosphotungstic heteropoly acid is small in water solubility, great in specific surface area and higher in catalytic activity. As an acid site on the surface of the phosphotungstic heteropoly acid having catalytic activity and phosphotungstic heteropoly acid redox carriers (e and II<+>) are diffused, oxidation is generated with biomass plant tissue under a hydrothermal condition; the phosphotungstic heteropoly acid is mainly applied to catalysis, biology, medicines, materials and other aspects, such as waste biomass catalytic degradation and toxic and harmful (waste) gas and sewage (wastewater) treatment in chemical industry production; a chelate of the phosphotungstic heteropoly acid has an anticancer effect, and also can be applied to electrode materials. The prepared load type phosphotungstic heteropoly acid is used for catalytically strengthening degradation of perilla stem, thus realizing efficient conversion of biomass.

Description

technical field [0001] The invention belongs to the technical field of preparation of phosphotungstic heteropolyacid, and in particular relates to the preparation of weakly water-soluble and loaded phosphotungstic heteropolyacid and a method for catalytically degrading perilla stalks. Background technique [0002] Phosphotungstic heteropolyacid, also known as polymetallic oxygen cluster, is a new type of multifunctional solid acid catalyst, which has the advantages of good stability, high selectivity, mild reaction conditions, low corrosion, and no pollution to the environment. It has been successfully applied It is used in olefin hydration, alkylation and isomerization reactions, and in petroleum refining such as gasoline etherification, diesel / gasoline oxidative desulfurization, gasoline alkylation desulfurization, etc. The existing preparation methods of heteropolyacid mainly include ether acidification extraction method, ion exchange method, electrodialysis method and so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18A62D3/38A62D101/28
CPCA62D3/38A62D2101/28B01J27/188
Inventor 王星敏王露魏星跃谭双
Owner CHONGQING TECH & BUSINESS UNIV
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