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Preparation method of vanadium oxytrichloride

A vanadium oxychloride and vanadium source technology, applied in the field of materials, can solve the problems of toxic and harmful substances, personal and environmental hazards, etc., and achieve the effects of low toxicity, strong shape controllability, simple and reliable process

Inactive Publication Date: 2020-03-31
DALIAN RONGKE ENERGY STORAGE GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to propose a vanadium-containing catalyst VOCl in view of the problem that the current preparation process of vanadyl trichloride produces toxic and harmful substances, which are prone to highly toxic hazards to the human body and the environment. 3 The preparation method, which does not produce toxic and harmful substances, avoids the harm of highly corrosive and highly toxic chlorine gas to the human body and the environment

Method used

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  • Preparation method of vanadium oxytrichloride
  • Preparation method of vanadium oxytrichloride

Examples

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Embodiment 1

[0040] This embodiment discloses a kind of preparation method of vanadyl trichloride, comprising the following steps:

[0041] 1. Weigh 50gV 2 o 5 , add 200mL of secondary water, stir at a speed of 200rpm, and mechanically stir until the reaction system is uniform.

[0042] 2. Add 72.61g of diammonium hydrogen phosphate while stirring, so that the ratio of vanadium to phosphorus in the solution is 1:1.

[0043] 3. Under the condition of continuous stirring, rapidly raise the temperature of the reaction system to 80°C, the heating rate is 7°C / min, and react for 20min until the reaction system is in the form of slurry.

[0044] 4. The obtained sample was dried in a blast drying oven at a drying temperature of 60° C. and a drying time of 8 hours until the sample turned into a yellow powder with a water content of less than 5% wt.

[0045] 5. After drying, use a powder machine to pulverize the sample, pass the pulverized sample through a sieve of more than 200 mesh, and place i...

Embodiment 2

[0055] 1. Put vanadium source V 2 o 5 After grinding, it is ground with aluminum chloride so that the molar ratio of vanadium to chloride is 1:1.

[0056] 2. Place the obtained sample in a tube furnace, use an inert non-oxidizing atmosphere to replace the atmosphere in the tube, and roast it under the conditions of an inert non-oxidizing atmosphere (nitrogen, argon). The roasting temperature is 600 ° C, and the roasting time is 40 minutes. The tailpipe distillate is the target product vanadyl trichloride.

Embodiment 3

[0058] 1. Grind the vanadium source APV and mix it with magnesium chloride, and grind and mix evenly so that the molar ratio of vanadium to chloride is 3:4.

[0059] 2. Place the obtained sample in a tube furnace, use an inert non-oxidizing atmosphere to replace the atmosphere in the tube, and roast it under the conditions of an inert non-oxidizing atmosphere (nitrogen, argon). The roasting temperature is 700 ° C, and the roasting time is 30 minutes. The tailpipe distillate is the target product vanadyl trichloride.

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Abstract

The invention provides a preparation method of vanadium oxytrichloride, which comprises the following steps: mixing and grinding a vanadium source and a chlorine source in a molar ratio of 3: 2, placing the mixture in a roasting furnace, roasting the mixture in a non-oxidizing atmosphere at a roasting temperature of 400-900 DEG C for 10-120 minutes, and collecting distillate, namely vanadium oxytrichloride, wherein the vanadium source is one or more of ammonium metavanadate, ammonium polyvanadate, vanadium pentoxide, VONH4HPO4, VPO4, VOPO4, (VO2)3PO4, (VO)4P2O7, (VO)2P2O7, VOSiO3, (VO2)2SiO3 and (VO2)4SiO4. According to the preparation method of the vanadium oxychloride, no toxic and harmful substances are generated, and harm of high-corrosivity and high-toxicity chlorine to human bodies and the environment is avoided.

Description

technical field [0001] The invention relates to material technology, in particular to a preparation method of vanadyl trichloride. Background technique [0002] Vanadium oxychloride VOCl 3 It is an important chemical raw material, it can be used as a catalyst for the copolymerization of ethylene-propylene rubber and ethylene-cyclopentadiene, it is also a solvent for various organic compounds, and it can also be used for the synthesis of vanadium organic compounds. [0003] The preparation of vanadium oxychloride mainly adopts following three methods at present: [0004] Method 1: use vanadium pentoxide to react with chlorine, and keep the ambient temperature at 600°C during the reaction; [0005] Method 2: Mix vanadium pentoxide with carbon. When the ambient temperature is 200-400°C, carbon will act as a deoxidizer, just like carbon deoxidizes TiCl in the Kroll method. 2 Convert to TiCl 4 same, first generate V 2 o 3 , and then pass chlorine gas to produce VOCl 3 ; ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
CPCC01G31/00
Inventor 王璐丁琳杨洪尚俊龙崔健
Owner DALIAN RONGKE ENERGY STORAGE GRP CO LTD
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