A kind of method for preparing keggin polycation chloride crystal

A chloride, polyaluminum chloride technology, applied in chemical instruments and methods, crystal growth, single crystal growth and other directions, can solve the problems of difficult preparation of Keggin structure polycationic chloride crystals, and achieve the effect of simple preparation

Active Publication Date: 2021-07-16
INNER MONGOLIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of the foregoing, the invention provides a novel preparation of Keggin-GaAl 12 The method of chloride single crystal and polycrystalline powder solves the difficult problem of Keggin structure polycation chloride crystal preparation

Method used

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  • A kind of method for preparing keggin polycation chloride crystal
  • A kind of method for preparing keggin polycation chloride crystal
  • A kind of method for preparing keggin polycation chloride crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) PAC solid-phase synthesis reaction: at 80°C, slowly dissolve 3.7g of aluminum powder into 87ml of C=5mol / lAlCl 3 In the solution, the degree of alkalization was set to 0.8. After all the aluminum powder had reacted, the solution was filtered and evaporated at room temperature to obtain a solid that was washed with isopropanol to obtain a PAC solid, which was dried in an oven for use.

[0031] (2) Keggin-GaAl 12 Chloride synthesis reaction: Dissolve 4.5g of the above-mentioned PAC solid in 25ml of methanol, sonicate in an ultrasonic instrument for about 10min, and after the solid is completely dissolved, dissolve the solid GaCl 3 Dissolve in the solution to make n(Al) / n(Ga)=1.6, evaporate and crystallize at room temperature. 15 days to get pure Keggin-GaAl 12 Chloride crystals.

Embodiment 2

[0033] (1) PAC solid-phase synthesis reaction: 2.6g of pure Al(OH) 3 Slowly dissolve in 12ml C=5.1mol / l HCl solution, after it is completely dissolved, add 50ml of water to make the degree of alkalization 1.2. Under the condition of 80°C, after all the solids have reacted, the solution was filtered and evaporated at room temperature, and the obtained solids were washed with isopropanol to obtain PAC solids, which were dried in an oven for future use.

[0034] (2) Keggin-GaAl 12Chloride synthesis reaction: Dissolve 4.5g of PAC solid in 25ml of methanol, sonicate in an ultrasonic instrument for about 10min, after the solid is completely dissolved, dissolve the solid GaCl 3 Dissolve in the solution to make n(Al) / n(Ga)=6.4, evaporate and crystallize at room temperature. 15 days to get pure Keggin-GaAl 12 Chloride crystals.

Embodiment 3

[0036] (1) PAC solid-phase synthesis reaction: at 80°C, slowly add 19.3g of aluminum powder to 103ml of C=5.3mol / l AlCl 3 In the solution, the degree of alkalinity was set to 1.3. After all the aluminum powder had reacted, the solution was filtered and evaporated at room temperature to obtain a solid that was washed with isopropanol to obtain a PAC solid, which was dried in an oven for future use.

[0037] (2) Keggin-GaAl 12 Chloride synthesis reaction: Dissolve 4.5g of PAC solid in 25ml of methanol, sonicate in an ultrasonic instrument for about 10min, after the solid is completely dissolved, dissolve the solid GaCl 3 Dissolve in the solution to make n(Al) / n(Ga)=26, evaporate and crystallize at room temperature. 15 days to get pure Keggin-GaAl 12 Chloride crystals.

[0038] In the above cases, single crystal particles with a size of about 3mm and polycrystalline powder can be obtained. The analysis results are shown in the attached figure 1 , 2, 3.

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Abstract

The invention provides a novel preparation of Keggin-GaAl 12 A method for chloride single crystal and polycrystalline powder belongs to the technical field of inorganic polymer synthesis. Inorganic polymer cluster MeAl with thirteen metal cores 12 ([MeO 4 al 12 (OH) 24 (H 2 O) 12 ] 7+ , Me=Al, Ga) is a typical Keggin-type polycation, which plays an important role in modern materials chemistry. But Keggin‑MeAl 12 (Me=Al, Ga) chloride crystals have not been obtained. In this method, the spontaneous hydrolysis product polyaluminum chloride PAC solid is dissolved in a methanol solvent, and then the gallium chloride solid is dissolved in the solution, slowly crystallized at room temperature, and Keggin-GaAl is precipitated 12 Chloride crystals. The obtained single crystal particles were confirmed by X-ray single crystal diffraction analysis to have a Keggin type structure of the cation.

Description

technical field [0001] The invention relates to the technical field of inorganic polymer synthesis, in particular to a novel preparation of Keggin-GaAl 12 Chloride single crystal and polycrystalline powder method. Background technique [0002] Inorganic polymer cluster MeAl with thirteen metal cores 12 ([MeO 4 Al 12 (OH) 24 (H 2 O) 12 ] 7+ , Me=Al, Ga) is a typical Keggin-type polycation, which plays an important role in modern materials chemistry. Keggin-MeAl 12 (Me=Al, Ga) polychlorides are widely used in all aspects of production and life: chemical agents for sewage treatment, surfactants, additives for nanomaterials, pillar propping agents for montmorillonite materials, and coal dyeing agents for fuels , and as a key ingredient in deodorants and antiperspirants, among others. [0003] Keggin-Al 13 and Keggin-GaAl 12 The polychloride is an important form of the hydrolysis reaction of group III elements, its formation mechanism and preparation process have been...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B7/14C30B29/12
Inventor 王晖贾长伟孙忠
Owner INNER MONGOLIA UNIVERSITY
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