CN115806314B - Preparation method of vanadium oxychloride - Google Patents
Preparation method of vanadium oxychloride Download PDFInfo
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- CN115806314B CN115806314B CN202211549753.9A CN202211549753A CN115806314B CN 115806314 B CN115806314 B CN 115806314B CN 202211549753 A CN202211549753 A CN 202211549753A CN 115806314 B CN115806314 B CN 115806314B
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Abstract
The invention discloses a preparation method of vanadium oxychloride, and relates to the technical field of fine chemical engineering. The method has the advantages that the trimethyl chlorosilane and the vanadium pentoxide are used as raw materials for reaction to prepare the vanadium oxychloride, the yield of the vanadium oxychloride product can be improved by precisely controlling the molar ratio and the reaction temperature of the raw materials, the reaction condition is mild, and the energy consumption is low; no toxic gas (chlorine) is adopted, and no toxic gas is generated, so that the harm of highly corrosive and highly toxic gas to human body and environment is avoided.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a preparation method of vanadium oxychloride.
Background
Vanadium, an important metal element, has been widely used in various fields due to its many excellent properties. Currently, about 85% of vanadium in the world is applied to the steel industry, and the remaining about 15% is mainly applied to industries such as aeronautical alloy, vanadium battery, chemical industry, catalyst, etc. The vanadium oxychloride is mainly used as a solvent and a catalyst for olefin polymerization, and can also be used for synthesizing vanadium organic compounds. The catalyst is used as a catalyst or a pre-catalyst in the reaction of preparing ethylene propylene rubber (ethylene propylene diene monomer, EPDM).
At present, the preparation method of vanadium oxychloride mainly comprises the following four methods:
(1) Preparing vanadium oxychloride by reacting thionyl chloride with vanadium pentoxide;
(2) Reacting vanadium pentoxide with chlorine gas at 600 ℃;
(3) Mixing vanadium pentoxide with carbon, and introducing chlorine gas to prepare vanadium oxychloride at the reaction temperature of 200-400 ℃;
(4) Grinding a vanadium source (such as vanadium phosphate) and then roasting with a chlorine source (such as sodium chloride) at a high temperature of 600-800 ℃ to prepare the vanadium oxychloride.
The method (1) adopts thionyl chloride, also contains extremely toxic substances, and generates a large amount of toxic gas sulfur dioxide in the reaction, thereby easily producing extremely toxic hazard to human bodies and the environment. The methods (2) to (4) need to adopt high-temperature or ultra-high-temperature conditions, have high energy consumption and severe reaction conditions, and all need to use the chlorine gas with extremely toxic substances as raw materials.
Therefore, the existing method has the defects of high energy consumption, harsh reaction conditions, environmental friendliness and the like in different degrees.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a preparation method of vanadium oxychloride, which aims to avoid the use of toxic raw materials and reduce the reaction energy consumption on the premise of improving the yield.
The invention is realized in the following way:
in a first aspect, the present invention provides a method for preparing vanadium oxychloride, comprising: the trimethylchlorosilane reacts with the vanadium pentoxide, the mole ratio of the trimethylchlorosilane to the vanadium pentoxide is 5.5-7.0:1, and the reaction temperature is 50-57 ℃.
In an alternative embodiment, the molar ratio of trimethylchlorosilane to vanadium pentoxide is from 5.8 to 6.5:1.
In an alternative embodiment, the reaction temperature is controlled to be 54℃to 57 ℃.
In an alternative embodiment, the reaction time is from 6 hours to 8 hours.
In an alternative embodiment, the reaction time is from 6.5h to 7.5h.
In an alternative embodiment, vanadium pentoxide is added to trimethylchlorosilane, and the reaction is carried out by heating to a reaction temperature.
In an alternative embodiment, after the reaction is completed, separation and purification are performed by distillation.
In an alternative embodiment, after the reaction is finished, the mixture is continuously heated, subjected to normal pressure distillation and condensation, and the fractions at different temperatures are collected to respectively obtain hexamethyldisiloxane and vanadium oxychloride.
In an alternative embodiment, the fraction between 95 ℃ and 105 ℃ is collected to obtain hexamethyldisiloxane.
In an alternative embodiment, the fraction between 115 ℃ and 125 ℃ is collected to obtain vanadium oxychloride.
The invention has the following beneficial effects: the method has the advantages that the trimethyl chlorosilane and the vanadium pentoxide are used as raw materials for reaction to prepare the vanadium oxychloride, the yield of the vanadium oxychloride product can be improved by precisely controlling the molar ratio and the reaction temperature of the raw materials, the reaction condition is mild, and the energy consumption is low; no toxic gas (chlorine) is adopted, and no toxic gas is generated, so that the harm of highly corrosive and highly toxic gas to human body and environment is avoided.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The embodiment of the invention provides a preparation method of vanadium oxychloride, which comprises the following steps: the reaction principle of the trimethylchlorosilane and vanadium pentoxide is as follows:
in the reaction process, oxygen in the vanadium pentoxide is combined with silicon in the trimethylchlorosilane to form a silicon-oxygen bond, so that more stable hexamethyldisiloxane is generated, and vanadium oxychloride is generated.
In order to further improve the yield of the product, the inventor optimizes the conditions of the consumption of the reaction raw materials, the reaction temperature, the reaction time and the like:
when the raw materials are mixed, the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is controlled to be 5.5-7.0:1, preferably 5.8-6.5:1, and more preferably 6.0:1. The inventor finds that under other optimal conditions, if the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is 4.5-5.4:1, the vanadium pentoxide is not completely reacted, the yield is 75-85%, and the yield is lower; when the molar ratio is greater than 7.0, the yield can be higher than 90%, but the trimethylchlorosilane is greatly excessive, so that raw materials are wasted, the cost is increased, and the optimal molar ratio is 5.5-7.0:1.
Specifically, the molar ratio of trimethylchlorosilane to vanadium pentoxide may be 5.5:1, 5.8:1, 6.0:1, 6.5:1, 7.0:1, or any value between the above adjacent values.
The reaction temperature of the preparation reaction is 50℃to 57℃and preferably 54℃to 57℃and more preferably 55 ℃. Under other optimal conditions, if the reaction temperature is 35-45 ℃, the vanadium pentoxide is not completely reacted, the yield is 70-85%, and the yield is low; since the boiling point of trimethylchlorosilane is 57 ℃, the optimum reaction temperature should not exceed 57 ℃.
Specifically, the reaction temperature may be 50 ℃, 51 ℃, 52 ℃, 53 ℃, 54 ℃, 55 ℃, 56 ℃, 57 ℃ or any value between the above adjacent values.
The reaction time of the preparation reaction is 6 to 8 hours, preferably 6.5 to 7.5 hours, more preferably 7 hours. Under other optimal conditions, if the reaction time is 3-5 h, the vanadium pentoxide is incompletely reacted, the yield is 65-80%, and the yield is lower; if the reaction time is more than 8 hours, the yield can be higher than 90% and basically unchanged, but the extension of the reaction time can cause unnecessary energy consumption and waste, thereby increasing the cost. Therefore, the optimal reaction time ranges from 6h to 8h.
Specifically, the reaction time may be 6.0h, 6.5h, 7.0h, 7.5h, 8.0h, etc., or may be any value between the above adjacent values.
In the actual operation process, vanadium pentoxide is added into trimethylchlorosilane, the mixture is heated to the reaction temperature for reaction, and after the reaction is finished, separation and purification are carried out in a distillation mode to obtain hexamethyldisiloxane and vanadium oxychloride products.
And further, after the reaction is finished, continuously heating, performing normal pressure distillation, condensing, and collecting fractions at different temperatures to respectively obtain hexamethyldisiloxane and vanadium oxychloride. Specifically, collecting the fraction at the temperature of 95-105 ℃ to obtain hexamethyldisiloxane, and collecting the fraction at the temperature of 115-125 ℃ to obtain vanadium oxychloride.
Specifically, the atmospheric distillation is to conduct distillation at 1 atmosphere without additional pressurization.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The embodiment provides a preparation method of vanadium oxychloride, which comprises the following steps:
controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 5.5:1, adding 100.0g of vanadium pentoxide into 328.5g of trimethylchlorosilane, stirring, heating to 40 ℃, reacting for 5 hours at 40 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 229.2g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 173.5g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 91.0 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.3%, total vanadium: 29.4%.
Example 2
The embodiment provides a preparation method of vanadium oxychloride, which comprises the following steps:
controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 6.0:1, adding 100.0g of vanadium pentoxide into 358.3g of trimethylchlorosilane, stirring, heating to 50 ℃, reacting for 5 hours at 50 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 232.5g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 180.3g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 94.6 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.4%, total vanadium: 29.5%.
Example 3
The embodiment provides a preparation method of vanadium oxychloride, which comprises the following steps:
controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 7.0:1, adding 100.0g of vanadium pentoxide into 418.1g of trimethylchlorosilane, stirring, heating to 40 ℃, reacting for 5 hours at 40 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 233.6g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 178.3g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 93.6 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.6%, total vanadium: 29.7%.
Example 4
The embodiment provides a preparation method of vanadium oxychloride, which comprises the following steps:
controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 6.0:1, adding 100.0g of vanadium pentoxide into 358.3g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 5 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 234.2g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 181.1g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 95.0 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.7%, total vanadium: 29.8%.
Example 5
The embodiment provides a preparation method of vanadium oxychloride, which comprises the following steps:
controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 6.0:1, adding 100.0g of vanadium pentoxide into 358.3g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 8 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 235.4g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 183.3g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 96.2 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.9%, total vanadium: 29.5%.
Example 6
The only difference from example 5 is that: the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is controlled to be 7.0:1.
The embodiment provides a preparation method of vanadium oxychloride, which comprises the following steps:
controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 7.0:1, adding 100.0g of vanadium pentoxide into 418.1g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 8 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 235.8g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 182.8g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 95.9%.
Boiling point of the product: 126-127 ℃, chlorine content: 61.7%, total vanadium: 29.4%.
Example 7
The only difference from example 5 is that: the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is controlled to be 5.5:1.
Controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 5.5:1, adding 100.0g of vanadium pentoxide into 328.4g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 8 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 212.3g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 158.9g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 83.4 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.6%, total vanadium: 29.6%.
Example 8
The only difference from example 5 is that: the reaction temperature was 50 ℃.
Controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 6.0:1, adding 100.0g of vanadium pentoxide into 358.3g of trimethylchlorosilane, stirring, heating to 50 ℃, reacting for 8 hours at 50 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 233.8g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 169.3g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 88.8%.
Boiling point of the product: 126-127 ℃, chlorine content: 61.2%, total vanadium: 29.4%.
Comparative example 1
The only difference from example 5 is that: the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is controlled to be 8.0:1.
Controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 8.0:1, adding 100.0g of vanadium pentoxide into 477.7g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 8 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 236.4g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 183.1g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 96.1 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.5%, total vanadium: 29.6%.
Comparative example 2
The only difference from example 5 is that: the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is controlled to be 5:1.
Controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 5.0:1, adding 100.0g of vanadium pentoxide into 298.6g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 8 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 196.8g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 149.9g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 78.7 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.1%, total vanadium: 29.3%.
Comparative example 3
The only difference from example 5 is that: the reaction temperature was 40 ℃.
Controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 6.0:1, adding 100.0g of vanadium pentoxide into 358.3g of trimethylchlorosilane, stirring, heating to 40 ℃, reacting for 8 hours at 40 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 202.3g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 160.8g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 84.4 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.3%, total vanadium: 29.5%.
Comparative example 4
The only difference from example 5 is that: the reaction time was 4h.
Controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 6.0:1, adding 100.0g of vanadium pentoxide into 358.3g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 4 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 210.4g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 165.2g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 86.7 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.3%, total vanadium: 29.8%.
Comparative example 5
The only difference from example 5 is that: the reaction time was 10h.
Controlling the molar ratio of trimethylchlorosilane to vanadium pentoxide to be 6.0:1, adding 100.0g of vanadium pentoxide into 358.3g of trimethylchlorosilane, stirring, heating to 57 ℃, reacting for 10 hours at 57 ℃, continuing heating to heat after the reaction is finished, distilling and condensing at normal pressure, collecting fractions between 95 and 105 ℃ to obtain 236.2g of hexamethyldisiloxane, collecting fractions between 115 and 125 ℃ to obtain 183.6g of vanadium oxychloride liquid, wherein the vanadium oxychloride yield is 96.3 percent.
Boiling point of the product: 126-127 ℃, chlorine content: 61.3%, total vanadium: 29.5%.
It can be seen that comparative example 5 significantly prolonged the reaction time and the yield was substantially the same as example 5.
Comparative example 6
The only difference from example 5 is that: trimethylchlorosilane is replaced with an equimolar amount of tert-butyl chloride.
100.0g of vanadium pentoxide is added into 305.4g of tert-butyl chloride by controlling the molar ratio of trimethylchlorosilane to tert-butyl chloride to be 6.0:1, the mixture is stirred and heated to be 51 ℃ (the boiling point of the tert-butyl chloride is 51-52 ℃), the mixture is reacted for 8 hours at the temperature of 51 ℃, normal pressure distillation and condensation are carried out, and finally, only the tert-butyl chloride can be collected without vanadium oxychloride.
In summary, the embodiment of the invention provides a preparation method of vanadium oxychloride, which has the following advantages compared with the prior art:
(1) Is environment-friendly, and avoids the generation of toxic hazard to human body and environment due to high-corrosiveness and high-toxicity chlorine in raw materials and high-toxicity byproduct sulfur dioxide.
(2) The preparation method is simple and convenient to operate, has no harsh conditions such as ultrahigh temperature and the like, and is safer and more reliable.
(3) The preparation yield of the vanadium oxychloride is high and can reach more than 90 percent.
(4) The byproduct hexamethyldisiloxane has high market value and is widely applied to the fields of end sealing agents, cleaning agents, parting agents, organic synthesis intermediates and the like.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for preparing vanadium oxychloride, which is characterized by comprising the following steps: the method comprises the steps of reacting trimethylchlorosilane with vanadium pentoxide, wherein in the reaction process, oxygen in the vanadium pentoxide is combined with silicon in the trimethylchlorosilane to form a silicon-oxygen bond, and generating hexamethyldisiloxane and vanadium oxychloride at the same time;
the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is 5.5-7.0:1, the reaction temperature is 50-57 ℃, and the reaction time is 6-8 hours.
2. The preparation method of claim 1, wherein the molar ratio of the trimethylchlorosilane to the vanadium pentoxide is 5.8-6.5:1.
3. The preparation method according to claim 1, wherein the reaction temperature is controlled to be 54 ℃ to 57 ℃.
4. The preparation method according to claim 1, wherein the reaction time is 6.5h to 7.5h.
5. The preparation method according to claim 1, wherein vanadium pentoxide is added to trimethylchlorosilane, and the reaction is carried out by heating to a reaction temperature.
6. The method according to claim 1, wherein the separation and purification are carried out by distillation after the completion of the reaction.
7. The preparation method according to claim 6, wherein after the reaction is finished, heating is continued to raise the temperature, normal pressure distillation and condensation are performed, and the hexamethyldisiloxane and the vanadium oxychloride are respectively obtained by collecting fractions at different temperatures.
8. The process of claim 7, wherein the fraction between 95 ℃ and 105 ℃ is collected to obtain hexamethyldisiloxane.
9. The method according to claim 7, wherein the vanadium oxychloride is obtained by collecting a fraction at 115-125 ℃.
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| US4448893A (en) * | 1981-07-24 | 1984-05-15 | The Standard Oil Company | Preparation of improved mixed vanadium phosphorus oxide catalyst and their use in oxidation processes |
| CN104016407A (en) * | 2014-06-11 | 2014-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of vanadium oxytrichloride and vanadium oxytrichloride obtained by using preparation method |
| CN110937630A (en) * | 2019-12-20 | 2020-03-31 | 大连博融新材料有限公司 | Preparation method of vanadium oxytrichloride |
| CN112142107A (en) * | 2020-09-29 | 2020-12-29 | 攀钢集团研究院有限公司 | Method for preparing high-purity vanadium oxychloride from vanadium-containing refined tailings |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| IT1403290B1 (en) * | 2010-12-27 | 2013-10-17 | Polimeri Europa Spa | SOLID COMPONENT OF CATALYST, CATALYST INCLUDING THE SOLID COMPONENT, AND PROCEDURE OF (CO) POLYMERIZATION OF ALPHA-OLEFINES |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4448893A (en) * | 1981-07-24 | 1984-05-15 | The Standard Oil Company | Preparation of improved mixed vanadium phosphorus oxide catalyst and their use in oxidation processes |
| CN104016407A (en) * | 2014-06-11 | 2014-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of vanadium oxytrichloride and vanadium oxytrichloride obtained by using preparation method |
| CN110937630A (en) * | 2019-12-20 | 2020-03-31 | 大连博融新材料有限公司 | Preparation method of vanadium oxytrichloride |
| CN112142107A (en) * | 2020-09-29 | 2020-12-29 | 攀钢集团研究院有限公司 | Method for preparing high-purity vanadium oxychloride from vanadium-containing refined tailings |
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