CN113247947A - Method for removing vanadium from crude titanium tetrachloride - Google Patents
Method for removing vanadium from crude titanium tetrachloride Download PDFInfo
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- CN113247947A CN113247947A CN202110639021.8A CN202110639021A CN113247947A CN 113247947 A CN113247947 A CN 113247947A CN 202110639021 A CN202110639021 A CN 202110639021A CN 113247947 A CN113247947 A CN 113247947A
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- titanium tetrachloride
- vanadium
- crude titanium
- slurry
- refined
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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 107
- 238000000034 method Methods 0.000 title claims abstract description 42
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 33
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 60
- 239000002002 slurry Substances 0.000 claims abstract description 54
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000203 mixture Substances 0.000 claims abstract description 49
- 239000001257 hydrogen Substances 0.000 claims abstract description 48
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 48
- 239000012535 impurity Substances 0.000 claims abstract description 31
- 238000005507 spraying Methods 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 238000005086 pumping Methods 0.000 claims abstract description 10
- 238000003860 storage Methods 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- 230000008020 evaporation Effects 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims description 6
- VZVLQKOGWNLVAC-UHFFFAOYSA-J tetrachlorotitanium vanadium Chemical compound [V].Cl[Ti](Cl)(Cl)Cl VZVLQKOGWNLVAC-UHFFFAOYSA-J 0.000 claims description 6
- 239000007787 solid Substances 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000004140 cleaning Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000007670 refining Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 235000010215 titanium dioxide Nutrition 0.000 description 3
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
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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 relates to a method for removing vanadium from crude titanium tetrachloride, which comprises the following steps: pumping the crude titanium tetrachloride liquid in the crude titanium tetrachloride storage tank into a mixing pipe, and introducing hydrogen into the mixing pipe to obtain a gas-liquid mixture; inputting the gas-liquid mixture into a superheater, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry; and spraying the mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, then spraying the mixture into a rectifying tower for rectification, condensing titanium tetrachloride steam at the tower top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the tower bottom of the rectifying tower into a slurry tank. By the method, the solid content in the refined slurry can be reduced, the replacement and cleaning frequency of the superheater can be reduced, the stable operation period of the superheater can be prolonged, and the production efficiency of a refined vanadium removal system can be improved; can reduce the impurity content in the refined titanium tetrachloride and the refined tailings, is convenient for high-value utilization of products and reduces the production cost.
Description
Technical Field
The invention belongs to the field of titanium tetrachloride refining, and more particularly relates to a method for removing vanadium from crude titanium tetrachloride.
Background
The titanium white produced by the chlorination process is a mainstream process for producing the titanium white in China gradually due to environmental protection and excellent product quality. The refined titanium tetrachloride is an important intermediate raw material for producing titanium white chloride or titanium sponge, and the refined vanadium removal process of the crude titanium tetrachloride is to produce refined tetrachloroThe key link of titanium transformation. At present, the refining vanadium-removing process of crude titanium tetrachloride mainly comprises a copper wire vanadium-removing method, an aluminum powder vanadium-removing method, a hydrogen sulfide vanadium-removing method and an organic matter vanadium-removing method. The method for removing vanadium from the copper wire has the defects that the regeneration washing operation of the failed copper wire is troublesome, the labor intensity is high, the condition is poor, the pollution of copper-containing wastewater is generated, the vanadium is not convenient to recover, the vanadium removal cost is high, and the production is discontinuous; the method for removing vanadium from aluminum powder has the defects that the used superfine active aluminum powder is expensive and has explosibility; the method for removing vanadium from hydrogen sulfide has the defects that the hydrogen sulfide has high toxicity, stink and explosiveness, and the labor condition is severe; the method for removing vanadium from organic matters has the defect that the organic matters are in VOCl3And TiCl4And a large amount of viscous solids are generated under the catalytic action, so that the superheater is easy to block, the superheater needs to be frequently replaced, and the continuous and stable operation of the refining system is influenced.
Therefore, how to remove vanadium impurities in the crude titanium tetrachloride with low cost and high efficiency and ensure the long-period stable operation of a refining system becomes a problem which needs to be solved urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to remove vanadium impurities in crude titanium tetrachloride with low cost and high efficiency and ensure the long-period stable operation of a refining system.
In order to solve the technical problems, the invention adopts the following technical scheme:
according to one aspect of the invention, a method for removing vanadium from crude titanium tetrachloride is provided, which comprises the following steps:
1) pumping the crude titanium tetrachloride liquid in the crude titanium tetrachloride storage tank into a mixing pipe, and introducing hydrogen into the mixing pipe to obtain a gas-liquid mixture of the crude titanium tetrachloride liquid and the hydrogen;
2) inputting the gas-liquid mixture into a superheater, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry;
3) and spraying the mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, then spraying the mixture into a rectifying tower for rectification, condensing titanium tetrachloride steam at the tower top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the tower bottom of the rectifying tower into a slurry tank.
In one embodiment of the invention, the mixing tube in step 1) is provided with a control valve.
In one embodiment of the invention, the feeding rate of the crude titanium tetrachloride liquid in step 1) is 6000-10000 kg/h.
In one embodiment of the invention, the impurities in the crude titanium tetrachloride liquid in step 2) comprise VOCl3Said VOCl3The content of (B) is 0.5-2%.
In one embodiment of the invention, the hydrogen gas has a purity of 99.999%.
In one embodiment of the invention, the flow rate of hydrogen in step 1) is controlled by a mass flow meter.
In one embodiment of the invention, hydrogen and VOCl3The molar ratio of (1-10) to (1).
In an embodiment of the invention, the step 2) further comprises controlling the temperature of the outlet of the superheater tube side to be 150-160 ℃ and the pressure to be 0.3-0.4 MPa.
In one embodiment of the invention, the step 3) further comprises controlling the top pressure of the rectifying tower not to exceed 15kPa, and the top temperature is 137-140 ℃.
Further in accordance with the present disclosure, there is provided a crude titanium tetrachloride vanadium removal system configured to perform the crude titanium tetrachloride vanadium removal method as described above.
By adopting the technical scheme, compared with the prior art, the invention has the following advantages:
the invention uses hydrogen to replace organic substances to remove VOCl in the crude titanium tetrachloride on the basis of the existing organic substance refining vanadium removal process3Conversion of vanadium-containing impurities into VOCl2Or VCl3And waiting for the low-valent chloride of vanadium, further refining the vanadium-removing slurry, and separating the vanadium-removing slurry from the refined titanium tetrachloride. The invention reduces the solid content in the refined slurry, reduces the replacement and cleaning frequency of the superheater, increases the stable operation period of the superheater and improves the production efficiency of the refined vanadium removal system; the invention reduces the impurity content in the refined titanium tetrachloride and the refined tailings, is convenient for high-value utilization of products and reduces the production costThe method is as follows.
Detailed Description
It should be understood that the embodiments of the invention shown in the exemplary embodiments are illustrative only. Although only a few embodiments of the present invention have been described in detail above, those skilled in the art will readily appreciate that many modifications are possible without materially departing from the teachings of the present subject matter. Accordingly, all such modifications are intended to be included within the scope of this invention. Other substitutions, modifications, changes and omissions may be made in the design, operating conditions and parameters and the like of the following exemplary embodiments without departing from the spirit of the present invention.
The invention provides a method for removing vanadium from crude titanium tetrachloride, which comprises the following steps:
1) pumping the crude titanium tetrachloride liquid in the crude titanium tetrachloride storage tank into a mixing pipe, and introducing hydrogen into the mixing pipe to obtain a gas-liquid mixture of the crude titanium tetrachloride liquid and the hydrogen;
2) inputting the gas-liquid mixture into a superheater, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry;
3) and spraying the mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, then spraying the mixture into a rectifying tower for rectification, condensing titanium tetrachloride steam at the tower top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the tower bottom of the rectifying tower into a slurry tank.
In the technical scheme, a control valve is arranged on the mixing pipe in the step 1).
In the technical scheme, the feeding rate of the crude titanium tetrachloride liquid in the step 1) is 6000-10000 kg/h.
In the technical scheme, the impurities in the crude titanium tetrachloride liquid in the step 2) comprise VOCl3Said VOCl3The content of (B) is 0.5-2%.
In the technical scheme, the purity of the hydrogen is 99.999%.
In the technical scheme, the flow rate of the hydrogen in the step 1) is controlled by a mass flow meter.
In the above technical scheme, in order to achieve the best vanadium removal effect, hydrogen and VOCl3The molar ratio of (1-10) to (1).
In the technical scheme, in order to ensure the quality and the yield of the refined titanium tetrachloride, the step 2) also comprises controlling the temperature of an outlet of a tube side of the superheater to be 150-160 ℃ and the pressure to be 0.3-0.4 MPa; the step 3) also comprises the step of controlling the pressure at the top of the rectifying tower not to exceed 15kPa, and the temperature at the top of the rectifying tower is 137-140 ℃.
In addition, the invention also provides a crude titanium tetrachloride vanadium removal system which is configured to execute the crude titanium tetrachloride vanadium removal method.
The invention uses hydrogen to replace organic substances to remove VOCl in the crude titanium tetrachloride on the basis of the existing organic substance refining vanadium removal process3Conversion of vanadium-containing impurities into VOCl2Or VCl3And the low-valent chloride of vanadium is further separated from the refined titanium tetrachloride, so that the amount of the produced refined slurry is reduced, the impurity content in the refined titanium tetrachloride and the refined tailings is reduced, the high-value utilization of products is facilitated, and the production cost is reduced.
After the treatment by the method, VOCl in the refined titanium tetrachloride3The content can be reduced to below 0.0007 percent, and the solid content in the refined slurry can be controlled to below 100 g/L.
The present invention is further illustrated by the following specific examples, which, however, do not limit the scope of the invention.
Example 1:
pumping the crude titanium tetrachloride liquid in a crude titanium tetrachloride storage tank into a mixing pipe, controlling the feeding rate of the crude titanium tetrachloride liquid to be 8000kg/h, simultaneously introducing hydrogen with the purity of 99.999% into the mixing pipe, controlling the flow rate of the hydrogen through a mass flow meter, and setting the flow rate of the hydrogen to be 10.5Nm3H, thereby obtaining a gas-liquid mixture of crude titanium tetrachloride liquid and hydrogen; inputting the gas-liquid mixture into a superheater for heating, controlling the temperature of a tube side outlet of the superheater to be 155 ℃ and the pressure to be 0.35MPa, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry; spraying the obtained mixture containing vanadium-removing mud into a flash tank for flash evaporationRemoving high boiling point impurities, spraying into a rectifying tower for rectification, controlling the top pressure of the rectifying tower to be 15kPa, the temperature at the top of the rectifying tower to be 137 ℃, condensing titanium tetrachloride vapor at the top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of a flash tank and the bottom of the rectifying tower into a slurry tank.
The VOCl in the fine titanium tetrachloride product obtained by the method3The content is 0.0007 percent, and the solid content in the refined slurry is 65.4 g/L.
Example 2:
pumping the crude titanium tetrachloride liquid in a crude titanium tetrachloride storage tank into a mixing pipe, controlling the feeding rate of the crude titanium tetrachloride liquid to be 8000kg/h, simultaneously introducing hydrogen with the purity of 99.999% into the mixing pipe, controlling the flow rate of the hydrogen through a mass flow meter, and setting the flow rate of the hydrogen to be 53.5Nm3H, thereby obtaining a gas-liquid mixture of crude titanium tetrachloride liquid and hydrogen; inputting the gas-liquid mixture into a superheater for heating, controlling the temperature of a tube side outlet of the superheater to be 155 ℃ and the pressure to be 0.35MPa, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry; and spraying the obtained mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, spraying the mixture into a rectifying tower for rectification, controlling the top pressure of the rectifying tower to be 15kPa, controlling the temperature at the top of the rectifying tower to be 137 ℃, condensing titanium tetrachloride steam at the top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the bottom of the rectifying tower into a slurry tank.
The VOCl in the fine titanium tetrachloride product obtained by the method3The content is 0.0003 percent, and the solid content in the refined slurry is 68.5 g/L.
Example 3:
pumping the crude titanium tetrachloride liquid in a crude titanium tetrachloride storage tank into a mixing pipe, controlling the feeding rate of the crude titanium tetrachloride liquid to be 6000kg/h, simultaneously introducing hydrogen with the purity of 99.999% into the mixing pipe, controlling the flow rate of the hydrogen through a mass flow meter, and setting the flow rate of the hydrogen to be 39.0Nm3H, thereby obtaining a gas-liquid mixture of crude titanium tetrachloride liquid and hydrogen; inputting the gas-liquid mixture into a superheater for heating, controlling the outlet temperature of the superheater tube side at 150 ℃, the pressure at 0.3MPa, and reacting hydrogen and crude tetrachloroReacting impurities in the titanium liquid to obtain a mixture containing vanadium-removed mud; and spraying the obtained mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, spraying the mixture into a rectifying tower for rectification, controlling the top pressure of the rectifying tower to be 10kPa, controlling the temperature at the top of the rectifying tower to be 140 ℃, condensing titanium tetrachloride steam at the top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the bottom of the rectifying tower into a slurry tank.
The VOCl in the fine titanium tetrachloride product obtained by the method3The content is 0.0002 percent, and the solid content in the refined slurry is 61.4 g/L.
Example 4:
pumping the crude titanium tetrachloride liquid in a crude titanium tetrachloride storage tank into a mixing pipe, controlling the feeding rate of the crude titanium tetrachloride liquid to be 10000kg/h, simultaneously introducing hydrogen with the purity of 99.999 percent into the mixing pipe, controlling the flow of the hydrogen through a mass flow meter, and setting the flow of the hydrogen to be 50.0Nm3H, thereby obtaining a gas-liquid mixture of crude titanium tetrachloride liquid and hydrogen; inputting the gas-liquid mixture into a superheater for heating, controlling the temperature of a tube side outlet of the superheater to be 160 ℃, and controlling the pressure to be 0.4MPa, wherein hydrogen reacts with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry; and spraying the obtained mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, spraying the mixture into a rectifying tower for rectification, controlling the top pressure of the rectifying tower to be 8kPa, controlling the temperature of the top of the rectifying tower to be 138 ℃, condensing titanium tetrachloride steam at the top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the bottom of the rectifying tower into a slurry tank.
The VOCl in the fine titanium tetrachloride product obtained by the method3The content is 0.0004 percent, and the solid content in the refined slurry is 52.3 g/L.
Example 5:
pumping the crude titanium tetrachloride liquid in a crude titanium tetrachloride storage tank into a mixing pipe, controlling the feeding rate of the crude titanium tetrachloride liquid to be 8000kg/h, simultaneously introducing hydrogen with the purity of 99.999 percent into the mixing pipe, controlling the flow rate of the hydrogen through a mass flow meter, and setting the flow rate of the hydrogen to be 25.5Nm3H, thereby obtaining a gas-liquid mixture of the crude titanium tetrachloride liquid and the hydrogenAn agent; inputting the gas-liquid mixture into a superheater for heating, controlling the temperature of a tube side outlet of the superheater to be 156 ℃ and the pressure to be 0.36MPa, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry; and spraying the obtained mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, spraying the mixture into a rectifying tower for rectification, controlling the top pressure of the rectifying tower to be 10kPa, controlling the temperature at the top of the rectifying tower to be 140 ℃, condensing titanium tetrachloride steam at the top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the bottom of the rectifying tower into a slurry tank.
The VOCl in the fine titanium tetrachloride product obtained by the method3The content is 0.0006 percent, and the solid content in the refined slurry is 60.8 g/L.
Example 6:
pumping the crude titanium tetrachloride liquid in a crude titanium tetrachloride storage tank into a mixing pipe, controlling the feeding rate of 9000kg/h, simultaneously introducing hydrogen with the purity of 99.999% into the mixing pipe, controlling the flow of the hydrogen through a mass flow meter, and setting the flow of the hydrogen to be 52.0Nm3H, thereby obtaining a gas-liquid mixture of crude titanium tetrachloride liquid and hydrogen; inputting the gas-liquid mixture into a superheater for heating, controlling the temperature of a tube side outlet of the superheater to be 157 ℃ and the pressure to be 0.34MPa, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry; and spraying the obtained mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, spraying the mixture into a rectifying tower for rectification, controlling the top pressure of the rectifying tower to be 15kPa, controlling the temperature at the top of the rectifying tower to be 137 ℃, condensing titanium tetrachloride steam at the top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the bottom of the rectifying tower into a slurry tank.
The VOCl in the fine titanium tetrachloride product obtained by the method3The content of the slurry was 0.0001%, and the solid content of the refined slurry was 63.8 g/L.
Thus, VOCl was present in the refined titanium tetrachloride products obtained in examples 1 to 63The contents and solids content of the refined slurry are shown in table 1 below:
TABLE 1
As can be seen from Table 1, VOCl in the fine titanium tetrachloride obtained after the treatment by the method of the present invention3The content can be reduced to below 0.0007 percent, and the solid content in the refined slurry can be controlled to below 100 g/L. Therefore, the invention reduces the solid content in the refined slurry, reduces the replacement and cleaning frequency of the superheater, increases the stable operation period of the superheater and improves the production efficiency of the refined vanadium removal system; the invention reduces the impurity content in the refined titanium tetrachloride and the refined tailings, is convenient for high-value utilization of products and reduces the production cost.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention; it is intended that the following claims be interpreted as including all such alterations, modifications, and equivalents as fall within the true spirit and scope of the invention.
Claims (10)
1. A method for removing vanadium from crude titanium tetrachloride is characterized by comprising the following steps:
1) pumping the crude titanium tetrachloride liquid in the crude titanium tetrachloride storage tank into a mixing pipe, and introducing hydrogen into the mixing pipe to obtain a gas-liquid mixture of the crude titanium tetrachloride liquid and the hydrogen;
2) inputting the gas-liquid mixture into a superheater, and reacting hydrogen with impurities in the crude titanium tetrachloride liquid to obtain a mixture containing vanadium-removed slurry;
3) and spraying the mixture containing the vanadium-removing slurry into a flash tank for flash evaporation to remove high-boiling-point impurities, then spraying the mixture into a rectifying tower for rectification, condensing titanium tetrachloride steam at the tower top of the rectifying tower to obtain a refined titanium tetrachloride product, and discharging refined slurry at the bottom of the flash tank and the tower bottom of the rectifying tower into a slurry tank.
2. The method for removing vanadium from crude titanium tetrachloride according to claim 1, wherein a control valve is installed on the mixing tube in step 1).
3. The method for removing vanadium from crude titanium tetrachloride as claimed in claim 1, wherein the feeding rate of the crude titanium tetrachloride liquid in the step 1) is 6000-10000 kg/h.
4. The process for removing vanadium from crude titanium tetrachloride according to claim 1, wherein the impurities in the crude titanium tetrachloride liquid in step 2) comprise VOCl3Said VOCl3The content of (B) is 0.5-2%.
5. The process for removing vanadium from crude titanium tetrachloride according to claim 1, wherein the purity of the hydrogen gas is 99.999%.
6. The method of removing vanadium from crude titanium tetrachloride according to claim 1, wherein the flow rate of the hydrogen gas is controlled by a mass flow meter.
7. The method of removing vanadium from crude titanium tetrachloride according to claim 4, wherein the hydrogen and the VOCl are mixed3The molar ratio of (1-10) to (1).
8. The method for removing vanadium from crude titanium tetrachloride as claimed in claim 1, wherein the step 2) further comprises controlling the temperature of the tube side outlet of the superheater at 150-160 ℃ and the pressure at 0.3-0.4 MPa.
9. The method as claimed in claim 1, wherein the step 3) further comprises controlling the top pressure of the rectifying tower not to exceed 15kPa, and the top temperature is 137-140 ℃.
10. A crude titanium tetrachloride vanadium removal system, wherein the system is configured to perform the crude titanium tetrachloride vanadium removal method of any one of claims 1 to 9 above.
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