Ta/W mixed heteropoly acid, preparation method and application thereof in acid catalysis and proton conduction

A technology of heteropolyacids and heteropolyanions, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. Single crystal structure and other issues, to achieve the effect of strong proton conductivity and high acid catalytic activity

Inactive Publication Date: 2017-02-01
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are not many heteropolyacids with well-defined structures: (1) Most polyacid compounds, especially complex polyacid compounds, only exist stably in a narrow pH range, and will transform into classical polyacids under strong acid conditions. Compounds with Keggin or Dawson structures; (2) It is difficult to obtain single crystal structures of such compounds
[0004] On the other hand, although based on V V 、Mo VI , W VI even Nb V The acidity of the V Little is known about how acidic

Method used

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  • Ta/W mixed heteropoly acid, preparation method and application thereof in acid catalysis and proton conduction
  • Ta/W mixed heteropoly acid, preparation method and application thereof in acid catalysis and proton conduction
  • Ta/W mixed heteropoly acid, preparation method and application thereof in acid catalysis and proton conduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of Ta / W mixed heteropolyacid

[0024] 1. Precursor mixture H 4 K 8 Na 8 [P 8 W 60 Ta 12 (H 2 O) 4 (OH) 8 o 236 ]·nH 2 O, marked as 1, synthesized according to the method described in the authorized patent (ZL201210236244.0) and literature reports (J. Am. Chem. Soc., 2012, 134, 19716−19721);

[0025] 2. Put 100g of activated cation exchange resin (Amberlite IR120B NA) into a chromatographic column with an inner diameter of 15mm, then pour 400mL of hydrochloric acid solution with a molar concentration of 1mol / L, and control the output rate to 1 drop / 2s. The chromatography column is acidic, then wash the chromatography column with deionized water to neutrality;

[0026] 3. Dissolve 3g of the precursor 1 obtained in step 1 in 5.0mL deionized water, then pour the above solution into the chromatographic column treated in step 2, control the output rate to 1 drop / 2s, and then use deionized water The chromatographic column was washed to neutrality, and t...

Embodiment 2

[0031] Acid catalytic activity test

[0032] In order to verify the acid catalytic activity of H-1, this example uses H-1 as a catalyst to catalyze the reaction of benzaldehyde with five alcohols. The specific method is as follows: take 3.3mmol of benzaldehyde, 25mmol of alcohol and 10mg of H-1, react in a reaction vessel for 90min, wherein the reaction temperature of reactions 5 and 9 is 100°C, and react 1, 2, 3, 4, 6, 7 and The reaction temperature of 8 is the reflux temperature, and the conversion rate of each reaction is shown in Table 1 by GC-MS after the reaction is finished.

[0033] Table 1 Reaction of benzaldehyde with various alcohols using H-1 as catalyst

[0034] alcohol product Conversion rate (%) a

[0035] Taking the reaction of benzaldehyde and ethylene glycol as an example, when using different heteropolyacids as catalysts, H-1 showed the highest catalytic activity. The specific method is as follows: 3.3mmol of benzaldehyde, 25mmol of ethyle...

Embodiment 3

[0040] Proton conductivity test

[0041] Take some of the prepared samples H-1, press them into thin slices with a thickness of 1 mm and a diameter of 1 cm with a tablet press, sandwich them into the loop of an electrochemical workstation, and test their conductivity under different humidity and temperature.

[0042] Under the conditions of temperature of 25°C and relative humidity of 30%, the electrical conductivity is 7.2×10 -3 S cm -1 . With the increase of relative humidity, the conductivity at 25°C gradually increases, and at 98% relative humidity, the conductivity reaches 5.0×10 - 2 S cm -1 . Such as Figure 5 As shown, in the case of keeping the relative humidity constant at 30%, the conductivity of H-1 increases with the increase of temperature within the tested temperature range (30°C, 45°C, 60°C, 75°C and 95°C). increase, reaching 7.2×10 at 95°C -2 S cm -1 . According to the calculation of Arrhenius curve, the electrical activation energy of H-1 proton con...

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Abstract

The invention discloses a Ta/W mixed heteropoly acid, a preparation method and application thereof in acid catalysis and proton conduction, belonging to the technical field of inorganic synthesis and acid catalysis. The invention has the essential technical scheme that the molecular formula of the Ta/W mixed heteropoly acid is H2O[P8W60Ta12(H2O)4(OH)8O236].125H2O, the Ta/W mixed heteropoly acid is composed of 1 tetramer Ta/W mixed heteropoly anion, 20 protons and 125 crystalline water molecules, and measured with dicinnamalacetone as an indicator in acetonitrile, the Hammett acid strength of the Ta/W mixed heteropoly acid is -2.91. The invention also discloses a preparation method of the Ta/W mixed heteropoly acid and application thereof in acid catalysis and proton conduction. The prepared Ta/W mixed heteropoly acid has the strongest acidity among the currently known heteropoly acids, and the strong acid property causes the Ta/W mixed heteropoly acid to have higher acid catalysis activity; and a large number of hydrogen bonds exist in the solid state structure of the prepared Ta/W mixed heteropoly acid and further form a hydrogen bond network, therefore the mixed heteropoly acid has stronger proton conducting power.

Description

technical field [0001] The invention belongs to the technical field of inorganic synthesis and acid catalysis, and specifically relates to a Ta / W mixed heteropolyacid, a preparation method and its application in acid catalysis and proton conduction. Background technique [0002] Heteropolyacids (HPAs) are an important class of compounds in polyacid chemistry, usually composed of polyanions and protons with typical structures. These polyanions have low basicity, so these heteropolyacids are generally strong Brønsted acids. Heteropolyacids have high-efficiency acid catalytic activity, especially in organic solvents, and their molar catalytic activity is usually 100-1000 times that of mineral acids such as sulfuric acid. Moreover, compared with mineral acids, the reactions catalyzed by heteropolyacids rarely have side reactions. Therefore, heteropolyacids are very suitable for catalyzing many kinds of homogeneous reactions in organic solvents. Since the industrialization of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J27/195C01G41/00C07C41/56C07C43/307C07D317/12
CPCB01J27/195B01J35/0033C01G41/006C01P2002/72C01P2002/82C01P2002/86C01P2006/40C01P2006/60C07C41/56C07D317/12C07C43/307
Inventor 李书军彭清坡陈学年翟建新张絜
Owner HENAN NORMAL UNIV
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