Preparation method of high-concentration VOCl2 solution

A high-concentration, solution technology, applied in chemical instruments and methods, vanadium compounds, vanadium halides, etc., can solve the problems of low upper limit of chlorine in hydrochloric acid, difficulty in obtaining high-concentration vanadium oxychloride solution, etc. The effect of high energy consumption

Pending Publication Date: 2022-04-01
大连融科储能集团股份有限公司
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AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to propose a high-concentration VOCl 2 The preparation method of the solution, the method has simple preparation steps, low cost, no pollution, and can realize high-concentration VOCl 2 Industrial production of solutions

Method used

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Embodiment 1

[0030] This embodiment discloses a high concentration VOCl 2 The preparation method of solution comprises the following steps:

[0031] (1) Dissolve 250gVO with 1L industrial concentrated hydrochloric acid (11mol / L) 2 , to obtain 4.9mol / L of VOCl 2 aqueous solution;

[0032] (2) Use electrolysis to reduce tetravalent vanadium to trivalent and reduce it to VCl 3 solution;

[0033] (3) Cooling and crystallization to obtain trivalent vanadium H 3 VCl 6 .nH 2 O crystals;

[0034] (4) The above-mentioned trivalent vanadium crystals are heated and dissolved in 5mol / L VOCl 2 solution, and adding V 2 o 5 , until all the trivalent vanadium is converted into tetravalent vanadium, and the concentration of 8mol / L VOCl is obtained 2 solution.

Embodiment 2

[0036] This embodiment discloses a high concentration VOCl 2 The preparation method of solution comprises the following steps:

[0037] (1) Dissolve 250gVO with 1L industrial concentrated hydrochloric acid (11mol / L) 2 , get VOCl 2 solution;

[0038] (2) Use electrolysis to reduce tetravalent vanadium to trivalent and reduce it to VCl 3 solution;

[0039] (3) adding crystal seeds and cooling crystallization to obtain trivalent vanadium crystals;

[0040] (4) The above-mentioned trivalent vanadium crystals are heated and dissolved in water, and V 2 o 5 , until all the trivalent vanadium is converted into tetravalent vanadium, and the obtained concentration is V 6mol / L, Cl - 15mol / L VOCl 2 solution.

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Abstract

The invention provides a preparation method of a high-concentration VOCl2 solution, which comprises the following steps: step 1, dissolving VO2 with concentrated hydrochloric acid to obtain a VOCl2 aqueous solution; step 2, reducing the VOCl2 aqueous solution into a VCl3 solution by an electrolytic method; step 3, cooling and crystallizing to obtain an H3VCl6. NH2O crystal; step 4, adding the H3VCl6. NH2O crystal into a vanadium oxychloride aqueous solution, and heating and dissolving to obtain a mixed solution of VOCl2 and VCl3; and step 5, VCl3 in the mixed solution in the step 4 is oxidized into VOCl2, and a high-concentration VOCl2 solution is prepared. The method has the advantages of simple preparation steps, low cost and no pollution, and can realize the industrial production of the high-concentration VOCl2 solution.

Description

technical field [0001] The present invention relates to VOCl 2 Preparation technology, especially involving a high-concentration VOCl 2 Solution preparation method. Background technique [0002] The current method of preparing vanadyl chloride is to reduce VOCl with zinc powder at 400°C in a closed tube 3 , can get VOCl 2 . Hydrogen can also be used as a reducing agent. The more effective preparation method is to make V 2 o 5 , VCl 3 and VOCl 3 Reaction by formula 1: [0003] V 2 o 5 +3VCl 3 +VOCl 3 →6VOCl 2 [0004] (Formula 1) [0005] The time of above-mentioned reaction is very long, will pass through 4-5 days, and raw material VCl 3 and VOCl 3 It is difficult to prepare, that is, it is difficult to obtain raw materials, so this method cannot be used for industrial production of vanadyl dichloride. [0006] The chlorine concentration of industrial hydrochloric acid is only less than 11mol / L, and the concentration of the vanadyl chloride solution that ca...

Claims

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Application Information

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IPC IPC(8): C01G31/00C01G31/04C25B1/01C25B1/50
Inventor 李宗麟宋明明阎成友刘国昌许盛
Owner 大连融科储能集团股份有限公司
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