CN112299474A - Method for refining titanium tetrachloride and removing vanadium - Google Patents
Method for refining titanium tetrachloride and removing vanadium Download PDFInfo
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- CN112299474A CN112299474A CN202011265077.3A CN202011265077A CN112299474A CN 112299474 A CN112299474 A CN 112299474A CN 202011265077 A CN202011265077 A CN 202011265077A CN 112299474 A CN112299474 A CN 112299474A
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- Prior art keywords
- titanium tetrachloride
- vanadium
- liquid
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- solid
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 30
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000007670 refining Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000007710 freezing Methods 0.000 claims abstract description 24
- 230000008014 freezing Effects 0.000 claims abstract description 24
- ZHXZNKNQUHUIGN-UHFFFAOYSA-N chloro hypochlorite;vanadium Chemical compound [V].ClOCl ZHXZNKNQUHUIGN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012267 brine Substances 0.000 claims abstract description 19
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 19
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 4
- 238000005265 energy consumption Methods 0.000 abstract description 10
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 4
- 238000012824 chemical production Methods 0.000 abstract description 2
- VZVLQKOGWNLVAC-UHFFFAOYSA-J tetrachlorotitanium vanadium Chemical compound [V].Cl[Ti](Cl)(Cl)Cl VZVLQKOGWNLVAC-UHFFFAOYSA-J 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 150000003682 vanadium compounds Chemical class 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- JBIQAPKSNFTACH-UHFFFAOYSA-K vanadium oxytrichloride Chemical compound Cl[V](Cl)(Cl)=O JBIQAPKSNFTACH-UHFFFAOYSA-K 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of chemical production, and particularly relates to a method for refining titanium tetrachloride and removing vanadium. Solves the problems that impurities are introduced into the titanium tetrachloride vanadium removal process and the energy consumption is higher in the prior art. The invention reduces the temperature of the rectified titanium tetrachloride to be below the melting point of the titanium tetrachloride and above the melting point of the vanadium oxychloride, and then realizes the vanadium removal of the titanium tetrachloride through solid-liquid separation. Then the solid titanium tetrachloride is heated and liquefied through the heat exchanger and is conveyed to the refined titanium tetrachloride tank, the temperature of brine at the other end of the heat exchanger is reduced simultaneously to prepare frozen brine, and the frozen brine is conveyed to a chlorination workshop to be used for cooling crude titanium tetrachloride gas, so that comprehensive utilization of energy is realized, and energy consumption is reduced. The invention improves the purity of titanium tetrachloride, realizes the recycling of energy, reduces energy consumption, overcomes the technical bias and ensures that the freezing vanadium removal process has practical value in industry. The method is suitable for removing the vanadium-containing compound in the titanium tetrachloride.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a method for refining titanium tetrachloride and removing vanadium.
Background
Titanium tetrachloride is the most important intermediate product for producing titanium dioxide by a chlorination process and producing sponge titanium by a Kloer process. The downstream products of titanium sponge and titanium dioxide have strict requirements on the content of vanadium in titanium tetrachloride, so that the removal of vanadium from crude titanium tetrachloride is an important process for refining titanium tetrachloride. Since the boiling point of titanium tetrachloride is 136.4 ℃ which is different from the boiling point of 127.2 ℃ of vanadium oxytrichloride which is the main component of vanadium in titanium tetrachloride by less than 10 ℃, the separation is difficult to realize by the rectification technology.
In the prior art, the mature vanadium removal process comprises the steps of removing vanadium from colored aluminum powder, removing vanadium from copper wires, removing vanadium from hydrogen sulfide, removing vanadium from organic matters and the like, wherein the vanadium removal mechanism is that the boiling point of a vanadium compound is changed, the difference between the boiling points of the vanadium compound and titanium tetrachloride is increased, and the vanadium compound is removed by rectification. However, in these methods, vanadium is removed by other media, and impurities are inevitably introduced. The other vanadium removing process is vanadium removing by a freezing method, but the freezing method has high energy consumption and no practical value in industry, so that the development of the low-energy-consumption freezing vanadium removing method is needed.
Disclosure of Invention
Aiming at the problems that impurities are introduced into a titanium tetrachloride vanadium removal process in the prior art and the energy consumption is high, the invention provides a method for refining and removing vanadium from titanium tetrachloride, which aims to solve the following problems: the energy consumption in the vanadium removal process is reduced, the introduction of impurities is prevented, and the purity of the titanium tetrachloride is improved.
The technical scheme adopted by the invention is as follows:
a method for refining and removing vanadium from titanium tetrachloride comprises the following steps:
s1, reducing the temperature of the rectified titanium tetrachloride to be lower than the melting point of the titanium tetrachloride and higher than the melting point of the vanadium oxychloride to obtain solid refined titanium tetrachloride and liquid vanadium oxychloride;
s2: separating solid titanium tetrachloride from liquid vanadium oxychloride by a solid-liquid separation method;
s3: the solid fine titanium tetrachloride is heated and liquefied by a heat exchanger with heat exchange liquid filled inside to obtain liquid pure titanium tetrachloride,
meanwhile, the temperature of the heat exchange liquid is reduced to obtain the frozen heat exchange liquid;
s4: and conveying the frozen heat exchange liquid to a chlorination workshop for cooling the crude titanium tetrachloride, raising the temperature of the heat exchange liquid, and conveying the heated heat exchange liquid to a heat exchanger again for heating and liquefying the solid fine titanium tetrachloride.
The melting point of vanadium oxychloride is-78.9 ℃ and the melting point of titanium tetrachloride is-25 ℃ which are different by about 54 ℃, so that the vanadium oxychloride in the titanium tetrachloride can be completely removed by adopting a freezing method and a solid-liquid separation method without introducing other impurities, the frozen titanium tetrachloride is cooled by a heat exchanger, and the cooled heat exchange liquid is used for cooling the crude titanium tetrachloride gas, thereby realizing the recycling of energy, reducing energy consumption, overcoming technical bias and leading the freezing method vanadium removal process to have practical value in industry.
Preferably, the heat exchange liquid in step S3 is brine.
After the preferred scheme is adopted, the melting point of the brine is lower than that of pure water, the brine is not easy to freeze, and the heat exchange liquid can be prevented from being solidified to block the heat exchanger, so that the energy recycling is influenced.
Preferably, the freezing temperature of titanium tetrachloride in step S1 is-25 ℃ to-78 ℃.
The melting point of vanadium oxychloride is-78.9 ℃ and the melting point of titanium tetrachloride is-25 ℃, and by adopting the preferred scheme, the vanadium oxychloride can be in a liquid state, and the titanium tetrachloride can be in a solid state, so that the vanadium oxychloride can be conveniently removed from the titanium tetrachloride.
Preferably, the method of reducing the temperature of titanium tetrachloride in step S1 is spray freezing or pressure-increasing freezing.
After the optimal scheme is adopted, the freezing and solid-liquid separation can be realized at the same time.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the melting point of vanadium oxychloride is-78.9 ℃ and the melting point of titanium tetrachloride is-25 ℃ which are different by about 54 ℃, so that the vanadium oxychloride in the titanium tetrachloride can be completely removed by adopting a freezing method and a solid-liquid separation method without introducing other substances, the purity of the titanium tetrachloride can be improved, the frozen titanium tetrachloride is cooled by a heat exchanger, and the cooled heat exchange liquid is used for cooling the crude titanium tetrachloride, so that the energy recovery and utilization are realized, the energy consumption is reduced, the technical bias is overcome, and the vanadium removal process by the freezing method has a practical value in industry.
2. The melting point of the salt water is lower than that of pure water, the salt water is not easy to freeze, and the heat exchange liquid can be prevented from being solidified to block the heat exchanger, so that the energy recycling is influenced.
3. The freezing temperature is-25 ℃ to-78 ℃, so that the vanadium oxychloride is in a liquid state, and the titanium tetrachloride is in a solid state, and the vanadium oxychloride is conveniently removed from the titanium tetrachloride.
4. Spray freezing or pressure-boosting freezing is adopted, so that solid-liquid separation can be realized while freezing is realized.
Drawings
The invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all the embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present application without making any creative effort, shall fall within the protection scope of the present application.
In the description of the embodiments of the present application, it should be noted that the terms "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships that the products of the present invention are usually placed in when used, and are only used for convenience of description and simplicity of description, but do not indicate or imply that the devices or elements that are referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present application. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
The present invention will be described in detail with reference to fig. 1.
A method for refining and removing vanadium from titanium tetrachloride comprises the following steps:
s1, reducing the temperature of the rectified titanium tetrachloride to be lower than the melting point of the titanium tetrachloride and higher than the melting point of the vanadium oxychloride to obtain solid refined titanium tetrachloride and liquid vanadium oxychloride;
s2: solid-liquid separation of solid titanium tetrachloride and liquid vanadium oxychloride is carried out by a filter pressing method;
s3: heating and liquefying the solid fine titanium tetrachloride by using a heat exchanger with brine introduced inside to obtain liquid pure titanium tetrachloride, then conveying the liquid pure titanium tetrachloride to a fine titanium tetrachloride tank for storage, and reducing the temperature of the brine to obtain frozen brine;
s4: and conveying the frozen brine to a chlorination workshop for cooling the crude titanium tetrachloride gas, raising the temperature of the brine, and conveying the heated brine to a heat exchanger again for heating and liquefying the solid fine titanium tetrachloride.
In this example, the freezing temperature of titanium tetrachloride in step S1 was-45 ℃.
In this embodiment, the method of cooling titanium tetrachloride in step S1 is spray freezing.
Example two
A method for refining and removing vanadium from titanium tetrachloride comprises the following steps:
s1, reducing the temperature of the rectified titanium tetrachloride to be lower than the melting point of the titanium tetrachloride and higher than the melting point of the vanadium oxychloride to obtain solid refined titanium tetrachloride and liquid vanadium oxychloride;
s2: solid-liquid separation of solid titanium tetrachloride and liquid vanadium oxychloride is carried out by suction filtration (reduced pressure filtration);
s3: heating and liquefying the solid fine titanium tetrachloride by using a heat exchanger with brine introduced inside to obtain liquid pure titanium tetrachloride, then conveying the liquid pure titanium tetrachloride to a fine titanium tetrachloride tank for storage, and reducing the temperature of the brine to obtain frozen brine;
s4: and conveying the frozen brine to a chlorination workshop for cooling the crude titanium tetrachloride, raising the temperature of the brine, and conveying the heated brine to a heat exchanger again for heating and liquefying the solid fine titanium tetrachloride.
In this example, the freezing temperature of titanium tetrachloride in step S1 was-25 ℃ and the energy consumption was reduced by freezing to this temperature.
In this embodiment, the method of reducing the temperature of titanium tetrachloride in step S1 is pressure-increasing freezing.
The above-mentioned embodiments only express the specific embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.
Claims (4)
1. A method for refining and removing vanadium from titanium tetrachloride is characterized by comprising the following steps:
s1, reducing the temperature of the rectified titanium tetrachloride to be lower than the melting point of the titanium tetrachloride and higher than the melting point of the vanadium oxychloride to obtain solid refined titanium tetrachloride and liquid vanadium oxychloride;
s2: separating solid titanium tetrachloride from liquid vanadium oxychloride by a solid-liquid separation method;
s3: heating and liquefying the solid fine titanium tetrachloride by using a heat exchanger filled with heat exchange liquid to obtain liquid pure titanium tetrachloride, and reducing the temperature of the heat exchange liquid to obtain frozen heat exchange liquid;
s4: and conveying the frozen heat exchange liquid to a chlorination workshop for cooling the crude titanium tetrachloride, raising the temperature of the heat exchange liquid, and conveying the heated heat exchange liquid to a heat exchanger again for heating and liquefying the solid fine titanium tetrachloride.
2. The method for refining and removing vanadium from titanium tetrachloride according to claim 1, wherein the heat exchange liquid in step S3 is brine.
3. The method of claim 1, wherein the freezing temperature of titanium tetrachloride in step S1 is-25 ℃ to-78 ℃.
4. The method for refining and removing vanadium from titanium tetrachloride according to claim 1, wherein the method for reducing the temperature of titanium tetrachloride in step S1 is spray freezing or pressure-increasing freezing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011265077.3A CN112299474A (en) | 2020-11-13 | 2020-11-13 | Method for refining titanium tetrachloride and removing vanadium |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011265077.3A CN112299474A (en) | 2020-11-13 | 2020-11-13 | Method for refining titanium tetrachloride and removing vanadium |
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| CN112299474A true CN112299474A (en) | 2021-02-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113634357A (en) * | 2021-08-23 | 2021-11-12 | 禄丰新立钛业有限公司 | Method for recovering titanium tetrachloride dust collecting slag |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113634357A (en) * | 2021-08-23 | 2021-11-12 | 禄丰新立钛业有限公司 | Method for recovering titanium tetrachloride dust collecting slag |
| CN113634357B (en) * | 2021-08-23 | 2024-02-13 | 云南国钛金属股份有限公司 | Recovery method of titanium tetrachloride dust collection slag |
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Application publication date: 20210202 |