CN104003444A - Method for preparing vanadium oxydichloride - Google Patents
Method for preparing vanadium oxydichloride Download PDFInfo
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- CN104003444A CN104003444A CN201410268646.8A CN201410268646A CN104003444A CN 104003444 A CN104003444 A CN 104003444A CN 201410268646 A CN201410268646 A CN 201410268646A CN 104003444 A CN104003444 A CN 104003444A
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- dichloro vanadyl
- vanadium
- preparing
- vanadyl
- chlorine
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Abstract
The invention discloses a method for preparing vanadium oxydichloride. The method for preparing the vanadium oxydichloride comprises the steps that vanadium trioxide with the particular size smaller than 0.074 mm is heated at high temperature in chlorine, and vanadium oxydichloride gas obtained through the reaction is condensed, so that the vanadium oxydichloride is obtained. According to the method for preparing the vanadium oxydichloride, the vanadium oxydichloride is directly prepared through the chlorine and the vanadium trioxide, and the vanadium yield reaches over 90wt%. The method is simple and easy to master, requirements for equipment are low, operation is convenient, the application range is wide, cost is low, environmental friendliness is achieved, and pollution is avoided.
Description
Technical field
The invention belongs to the fine chemical technology field that vanadium is produced, more particularly, relate to a kind of method of preparing dichloro vanadyl.
Background technology
Vanadium is a kind of important metal, has many premium propertiess, is widely used in every field.Approximately have in the world the vanadium of 85wt% to be applied to steel industry, all the other about 15wt% are mainly used in the industries such as aerometal, vanadium cell, chemical industry, catalyzer.Dichloro vanadyl has very important effect in organic chemical industry, can be used as the catalyzer of producing c_2-oxygen compound.
In inorganic chemistry book series, set forth a kind of method of preparing dichloro vanadyl, in the pipe of a sealing, at 400 ℃, used zinc powder reduction VOCl
3, can obtain VOCl
2.Also can make reductive agent with hydrogen, comparatively effectively preparation method makes V
2o
5, VCl
3and VOCl
3press following formula 1 reaction:
V
2o
5+ 3VCl
3+ VOCl
3→ 6VOCl
2---formula 1
But this reaction is chronic, pass through 4-5 days, and VCl
3and VOCl
3be difficult to prepare, the industrial application of this method hardly may.
Existing more Introduction of Literatures vanadium oxytrichloride in industrial application, but the preparation method who relates to dichloro vanadyl does not almost have.
Therefore, need to provide a kind of dichloro vanadyl preparation method that can be applied to industrial mass production.
Summary of the invention
For the deficiencies in the prior art, one or more during the present invention is intended to solve the problems of the technologies described above.
The object of the present invention is to provide a kind of reaction process simply, easily to control and be easy to the dichloro vanadyl preparation method of large industrial-scale production
To achieve these goals, the invention provides a kind of method of preparing dichloro vanadyl, be that vanadous oxide below 0.074mm carries out heat in chlorine, then the dichloro vanadyl condensation of gas that reaction is obtained obtains dichloro vanadyl by granularity.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, the purity of described vanadous oxide is greater than 99wt%.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, the moisture content of described vanadous oxide is lower than 0.1wt%.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, described chlorine is analytical pure chlorine.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, described heat is carried out in encloses container.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, the temperature of described heat is 400～600 ℃.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, the time of described heat is 60～300min.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, the temperature of described condensation is 0～20 ℃.
According to an embodiment who prepares the method for dichloro vanadyl of the present invention, the time of described condensation is 2～10h.
The present invention adopts vanadous oxide and chlorine as raw material production dichloro vanadyl, and reaction process simply and is easily controlled, and environmental protection and be easy to large industrial-scale production has high economic benefit and social benefit.
Embodiment
Hereinafter, the method for preparing dichloro vanadyl of the present invention will be described in detail.
Thinking of the present invention is the vanadous oxide of certain particle size to heat in chlorine, after reaction for some time, obtains dichloro vanadyl.
According to exemplary embodiment of the present invention, the described method of preparing dichloro vanadyl is specially: by granularity, be that vanadous oxide below 0.074mm carries out heat in chlorine, then the dichloro vanadyl condensation of gas that reaction is obtained obtains dichloro vanadyl.
Wherein, adding granularity is that tri-chlorination two vanadium below 0.074mm are in order to increase the contact surface of tri-chlorination two vanadium and chlorine, thereby improves reactivity and reaction efficiency.According to exemplary embodiment of the present invention, the purity of vanadous oxide is greater than 99wt%, and is preferably dried to guarantee that moisture content in vanadous oxide is lower than 0.1wt% vanadous oxide being entered to stokehold.If the purity of vanadous oxide is not high, affect yield and the purity of final dichloro vanadyl; If moisture is too high in vanadous oxide, affect speed of response and reaction efficiency.In addition, chlorine is preferably analytical pure chlorine, same yield and purity in order to ensure reaction product.
When carrying out heat, vanadous oxide and chlorine occur as shown in the formula 2 react:
V
2o
3+ Cl
2=VOCl
2+ O
2---formula 2
In order to ensure carrying out smoothly of above-mentioned reaction, should make above-mentioned heat carry out in encloses container, do not allow entering of foreign gas.
According to exemplary embodiment of the present invention, the temperature of heat is 400～600 ℃, and the time of heat is 60～300min.Experiment shows, the temperature range of 400～600 ℃ is the optimum temperature range of chlorination reaction, if the too low meeting of temperature causes speed of reaction very slow, if excess Temperature can cause the waste of the energy.In addition,, if too short meeting heat-up time causes vanadium yield lower, if the oversize waste that can cause chlorine heat-up time, the time of controlling heat is that 60～300min can either guarantee that sufficient reacting carries out, and also can guarantee vanadium yield.
Because the temperature in encloses container is higher, the product obtaining after reaction finishes is dichloro vanadyl gas, so need to carry out condensation to obtain dichloro vanadyl liquid to dichloro vanadyl gas.Particularly, the temperature of condensation is 0～20 ℃, and the time of condensation is 2～10h, but as long as the final dichloro vanadyl that obtains liquid state the invention is not restricted to this.In addition, can also comprise the step of condensing crystal after condensation, to obtain the solid phase prod of dichloro vanadyl, the present invention is also not limited to this.
Below in conjunction with concrete example, further illustrate the present invention.
Example 1:
Vanadous oxide is crushed to below 0.074mm, gets 100g vanadous oxide and in chlorine, be heated to 400 ℃, be 300min heat-up time, obtains dichloro vanadyl gas after reaction.
By gained dichloro vanadyl gas condensation 10h at 20 ℃, obtain dichloro vanadyl liquid.
After testing, the content of vanadium in gained dichloro vanadyl is 36.8wt%, and purity is 99.5wt%.
Example 2:
Vanadous oxide is crushed to below 0.074mm, gets 100g vanadous oxide and in chlorine, be heated to 600 ℃, be 60min heat-up time, obtains dichloro vanadyl gas after reaction.
By gained dichloro vanadyl gas condensation 5h at 10 ℃, obtain dichloro vanadyl liquid.
After testing, the content of vanadium in gained dichloro vanadyl is 36.85wt%, and purity is 99.8wt%.
Example 3:
Vanadous oxide is crushed to below 0.074mm, gets 100g vanadous oxide and in chlorine, be heated to 500 ℃, be 200min heat-up time, obtains dichloro vanadyl gas after reaction.
By gained dichloro vanadyl gas condensation 2h at 0 ℃, obtain dichloro vanadyl liquid.
After testing, the content of vanadium in gained dichloro vanadyl is 36.9wt%, and purity is 99.9wt%.
In sum, the present invention adopts chlorine and vanadous oxide directly to prepare dichloro vanadyl, more than vanadium yield reaches 90wt%.That the present invention is simple and easy to is low, easy to operate by, equipment requirements, wide accommodation, cost are low, environmental friendliness and pollution-free.
Although above by having described the present invention in conjunction with exemplary embodiment, it will be apparent to those skilled in the art that in the situation that do not depart from the spirit and scope that claim limits, can carry out various modifications and change to exemplary embodiment of the present invention.
Claims (9)
1. a method of preparing dichloro vanadyl, is characterized in that, be that vanadous oxide below 0.074mm carries out heat in chlorine, then the dichloro vanadyl condensation of gas that reaction is obtained obtains dichloro vanadyl by granularity.
2. the method for preparing dichloro vanadyl according to claim 1, is characterized in that, the purity of described vanadous oxide is greater than 99wt%.
3. the method for preparing dichloro vanadyl according to claim 1 and 2, is characterized in that, the moisture content of described vanadous oxide is lower than 0.1wt%.
4. the method for preparing dichloro vanadyl according to claim 1, is characterized in that, described chlorine is analytical pure chlorine.
5. the method for preparing dichloro vanadyl according to claim 1, is characterized in that, described heat is carried out in encloses container.
6. the method for preparing dichloro vanadyl according to claim 1, is characterized in that, the temperature of described heat is 400～600 ℃.
7. the method for preparing dichloro vanadyl according to claim 1, is characterized in that, the time of described heat is 60～300min.
8. the method for preparing dichloro vanadyl according to claim 1, is characterized in that, the temperature of described condensation is 0～20 ℃.
9. the method for preparing dichloro vanadyl according to claim 1, is characterized in that, the time of described condensation is 2～10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410268646.8A CN104003444B (en) | 2014-06-16 | 2014-06-16 | A kind of method preparing dichloro vanadyl |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410268646.8A CN104003444B (en) | 2014-06-16 | 2014-06-16 | A kind of method preparing dichloro vanadyl |
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| Publication Number | Publication Date |
|---|---|
| CN104003444A true CN104003444A (en) | 2014-08-27 |
| CN104003444B CN104003444B (en) | 2015-11-18 |
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114229894A (en) * | 2021-12-13 | 2022-03-25 | 大连博融新材料有限公司 | Preparation method of anhydrous vanadyl dichloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3462288A (en) * | 1966-06-20 | 1969-08-19 | Dow Chemical Co | Aluminum plating process |
| CN101054201A (en) * | 2006-04-10 | 2007-10-17 | 北京有色金属研究总院 | Method for removing vanadium in titanium tetrachloride |
| CN101113495A (en) * | 2006-07-27 | 2008-01-30 | 张荣禄 | Method for extracting iron titanium vanadium from high-titanium iron concentrate |
-
2014
- 2014-06-16 CN CN201410268646.8A patent/CN104003444B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3462288A (en) * | 1966-06-20 | 1969-08-19 | Dow Chemical Co | Aluminum plating process |
| CN101054201A (en) * | 2006-04-10 | 2007-10-17 | 北京有色金属研究总院 | Method for removing vanadium in titanium tetrachloride |
| CN101113495A (en) * | 2006-07-27 | 2008-01-30 | 张荣禄 | Method for extracting iron titanium vanadium from high-titanium iron concentrate |
Non-Patent Citations (2)
| Title |
|---|
| A. HACKERT ET AL.: "Nachweis und thermochemische Charakterisierung des Gasphasenmolekuls VOCl2", 《ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE》, vol. 622, 31 December 1996 (1996-12-31) * |
| 杨绍利: "《钒钛磁铁矿非高炉冶炼技术》", 29 February 2012, 《冶金工业出版社》, article "钒钛磁铁矿非高炉冶炼技术", pages: 35 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114229894A (en) * | 2021-12-13 | 2022-03-25 | 大连博融新材料有限公司 | Preparation method of anhydrous vanadyl dichloride |
| CN114229894B (en) * | 2021-12-13 | 2024-01-23 | 大连融科储能集团股份有限公司 | Preparation method of anhydrous vanadium oxychloride |
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| CN104003444B (en) | 2015-11-18 |
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