CN212467172U - System for separating silicon tetrachloride in crude titanium tetrachloride - Google Patents

System for separating silicon tetrachloride in crude titanium tetrachloride Download PDF

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Publication number
CN212467172U
CN212467172U CN202020599544.5U CN202020599544U CN212467172U CN 212467172 U CN212467172 U CN 212467172U CN 202020599544 U CN202020599544 U CN 202020599544U CN 212467172 U CN212467172 U CN 212467172U
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silicon
tetrachloride
titanium tetrachloride
liquid
separation tower
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姬丽丽
周媛
常智敏
司亚超
季俊红
史广普
侯俊臣
程志
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Henan Billions Advanced Material Co Ltd
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Henan Billions Advanced Material Co Ltd
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Abstract

The utility model discloses a system for separating silicon tetrachloride in crude titanium tetrachloride, which comprises an evaporator, a rectifying tower, a separating tower, a silicon cooler and a heat exchanger; the separation tower is used for spraying, cooling and separating the crude titanium tetrachloride gas from the rectifying tower into refined titanium tetrachloride liquid and silicon tetrachloride gas; the silicon cooler is used for cooling the silicon tetrachloride gas from the separation tower, and one part of the cooled silicon tetrachloride liquid flows back to the separation tower and is used for spraying and separating crude titanium tetrachloride gas; the heat exchanger is used for cooling the fine titanium tetrachloride liquid from the separation tower, and one part of the cooled fine titanium tetrachloride liquid flows back to the separation tower for spraying and separating the crude titanium tetrachloride gas. The utility model discloses only utilize the difference of silicon tetrachloride and titanium tetrachloride boiling point, make silicon tetrachloride and titanium tetrachloride obtain effective separation, solved the pollution problem of silicon tetrachloride in the titanium tetrachloride production to certain economic benefits has been taken into account.

Description

System for separating silicon tetrachloride in crude titanium tetrachloride
Technical Field
The utility model belongs to the technical field of chemical production, concretely relates to system for silicon tetrachloride in thick titanium tetrachloride of separation.
Background
The titanium tetrachloride production raw material contains impurities such as Ca, Mg, Fe, V, Si and the like, after the reaction in the chlorination furnace, part of the impurities are remained in a bed layer, and the other part of the impurities enter the next process along with the generated titanium tetrachloride. Some high boiling point metal chlorides such as AlCl are refined to remove vanadium3And MgCl2Iso and converted VOCl2The titanium tetrachloride is left at the bottom of the evaporator and the rectifying tower and is removed through discharged liquid, and the titanium tetrachloride enters the condensing tower along with a part of silicon tetrachloride with lower boiling point through an outlet at the top of the rectifying tower and is cooled along with the titanium tetrachloride in the condensation process, and the silicon tetrachloride is easy to volatilize to form acid gas, so that resources are wasted, and the environmental pollution is also caused.
In the production process of titanium sponge, high-quality titanium tetrachloride must be used to ensure the purity of the product, and the titanium tetrachloride without silicon removal has high silicon content and is difficult to meet the production requirement, so technical improvement is needed to improve the product quality and widen the product line.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a system for separating silicon tetrachloride in thick titanium tetrachloride for solving the deficiency of the prior art.
The purpose of the utility model is realized by the following technical scheme:
a system for separating silicon tetrachloride in crude titanium tetrachloride comprises an evaporator and a rectifying tower connected with the evaporator, wherein the rectifying tower is used for generating crude titanium tetrachloride gas containing silicon tetrachloride, and also comprises a separation tower, a silicon cooler and a heat exchanger;
the separation tower is connected with the rectifying tower and is used for spraying, cooling and separating the crude titanium tetrachloride gas from the rectifying tower into refined titanium tetrachloride liquid and silicon tetrachloride gas;
the silicon cooler is connected with the separation tower and is used for cooling the silicon tetrachloride gas from the separation tower, and one part of the cooled silicon tetrachloride liquid flows back to the separation tower and is used for spraying and separating crude titanium tetrachloride gas;
the heat exchanger is connected with the separation tower and is used for cooling the fine titanium tetrachloride liquid from the separation tower, and one part of the cooled fine titanium tetrachloride liquid flows back to the separation tower and is used for spraying and separating crude titanium tetrachloride gas.
Preferably, the rectifying tower is also connected with a condensing tower.
Preferably, a crude titanium tetrachloride liquid reflux opening is formed in the bottom of the rectifying tower, and the crude titanium tetrachloride liquid reflux opening is connected with the evaporator.
Preferably, the system further comprises a steam scrubber connected with the separation tower and used for receiving and scrubbing the silicon tetrachloride gas from the separation tower.
Preferably, the silicon cooling system further comprises a silicon storage intermediate tank, wherein one end of the silicon storage intermediate tank is connected with the silicon cooler, the other end of the silicon storage intermediate tank is connected with the separation tower, and the silicon storage intermediate tank is used for storing silicon tetrachloride liquid from the silicon cooler and discharging a part of the silicon tetrachloride liquid to the separation tower to be used as spraying liquid; the silicon storage intermediate tank is also provided with a breathing port, and the breathing port is connected with the steam washer.
Preferably, the device also comprises a titanium storage intermediate tank, wherein one end of the titanium storage intermediate tank is connected with the separation tower, the other end of the titanium storage intermediate tank is connected with the heat exchanger, and the titanium storage intermediate tank is used for storing the refined titanium tetrachloride liquid from the separation tower and discharging a part of the refined silicon tetrachloride liquid to the heat exchanger.
Preferably, still include silicon tetrachloride liquid delivery pump, silicon tetrachloride liquid delivery pump the inlet end with store up the silicon tundish and connect, the exit end divide into two branches, a branch road with the knockout tower is connected, another branch road with store up the silicon tundish top and connect.
Preferably, the system also comprises a refined titanium tetrachloride liquid delivery pump, wherein the inlet end of the refined titanium tetrachloride liquid delivery pump is connected with the titanium storage intermediate tank, the outlet end of the refined titanium tetrachloride liquid delivery pump is divided into two branches, one branch is connected with the heat exchanger, and the other branch is connected with the top of the titanium storage intermediate tank.
Preferably, the silicon tetrachloride spray liquid enters from the top of the separation tower, and the titanium tetrachloride spray liquid enters from the middle of the separation tower.
Preferably, the steam scrubber device further comprises a steam scrubber pump, wherein an inlet end of the steam scrubber pump is connected with the bottom of the steam scrubber, and an outlet end of the steam scrubber pump is connected with the top of the steam scrubber and is used for spraying and refluxing the steam scrubber.
The utility model provides a system for silicon tetrachloride only utilizes the difference of silicon tetrachloride and titanium tetrachloride boiling point in the thick titanium tetrachloride of separation, makes silicon tetrachloride and titanium tetrachloride obtain effective separation, has solved the pollution problem of silicon tetrachloride in the titanium tetrachloride production to certain economic benefits has been taken into account.
Drawings
FIG. 1 is a schematic structural diagram of a system for separating silicon tetrachloride from crude titanium tetrachloride according to the present invention;
fig. 2 is a schematic structural diagram of a system for separating silicon tetrachloride in crude titanium tetrachloride according to one preferred embodiment of the present invention.
Detailed Description
The utility model provides a system for silicon tetrachloride in separation thick titanium tetrachloride, as shown in figure 1, including evaporimeter 1 and the rectifying column 2 of being connected with the evaporimeter, thick titanium tetrachloride gas outlet 21 is established at rectifying column 2 top, the evaporimeter is used for making thick titanium tetrachloride vaporization, then the titanium tetrachloride of vaporization gets into the rectifying column and gets rid of impurity such as metal chloride, and the thick titanium tetrachloride gas that includes silicon tetrachloride is discharged from thick titanium tetrachloride gas outlet 21, generally gets into the condensing tower among the prior art and makes silicon tetrachloride and thick titanium tetrachloride gas together cool off.
The system for separating silicon tetrachloride in crude titanium tetrachloride provided by the utility model comprises a separation tower 3, a silicon cooler 4 and a heat exchanger 5 besides an evaporator 1 and a rectifying tower 2; a crude titanium tetrachloride gas inlet 31, a silicon tetrachloride gas outlet 32, a first refined titanium tetrachloride liquid outlet 33, a silicon tetrachloride spray liquid inlet 34 and a titanium tetrachloride spray liquid inlet 35 are arranged on the separation tower 3; a silicon tetrachloride gas inlet 41, a first silicon tetrachloride liquid outlet 42 and a circulating cooling medium inlet and outlet are formed in the silicon cooler 4; the heat exchanger 5 is provided with a first refined titanium tetrachloride liquid inlet 51, a second refined titanium tetrachloride liquid outlet 52 and a circulating cooling medium inlet and outlet.
A crude titanium tetrachloride gas inlet 31 of the separation tower 3 is connected with a crude titanium tetrachloride gas outlet 21 of the rectifying tower 2 and is used for receiving crude titanium chloride gas containing silicon tetrachloride and discharged from the top of the rectifying tower; a silicon tetrachloride gas outlet 32 is connected with a silicon tetrachloride gas inlet 41 of the silicon cooler 4, a first refined titanium tetrachloride liquid outlet 33 is connected with a first refined titanium tetrachloride liquid inlet 51 of the heat exchanger 5, a silicon tetrachloride spraying liquid inlet 34 is connected with a first silicon tetrachloride liquid outlet 42 of the silicon cooler 4, and a titanium tetrachloride spraying liquid inlet 35 is connected with a second refined titanium tetrachloride liquid outlet 52 of the heat exchanger 5; the separation tower 3 is used for spraying and cooling the crude titanium tetrachloride gas from the rectifying tower 2 to separate the crude titanium tetrachloride gas into fine titanium tetrachloride liquid and silicon tetrachloride gas, the fine titanium tetrachloride liquid is discharged from a first fine titanium tetrachloride liquid outlet 33 and is conveyed to the heat exchanger 5 through a first fine titanium tetrachloride liquid inlet 51, and the silicon tetrachloride gas is discharged from a silicon tetrachloride gas outlet 32 and is conveyed to the silicon cooler 4 through a silicon tetrachloride gas inlet 41.
The silicon cooler 4 is used for cooling the silicon tetrachloride gas from the separation tower 3, the cooled silicon tetrachloride liquid is discharged, one part of the cooled silicon tetrachloride liquid flows back to the separation tower 3 through the silicon tetrachloride spraying liquid inlet 34 and is used for spraying and separating crude titanium tetrachloride gas, and the other part of the cooled silicon tetrachloride liquid can be collected and stored.
The heat exchanger 5 is used for cooling the fine titanium tetrachloride liquid from the separation tower 3, the cooled fine titanium tetrachloride liquid is discharged, one part of the fine titanium tetrachloride liquid flows back to the separation tower 3 through the titanium tetrachloride spray liquid inlet 35 for spraying and separating the crude titanium tetrachloride gas, and the other part of the fine titanium tetrachloride liquid can be collected and stored.
As can be understood by those skilled in the art, the system for separating silicon tetrachloride from crude titanium tetrachloride provided by the invention further comprises a plurality of connecting pipelines and control valves which are conventionally arranged so as to flow and control materials among various components of the system.
In practical use, the crude titanium tetrachloride is vaporized in the evaporator 1 and then enters the rectifying tower 2 to remove impurities such as metal chlorides, the crude titanium tetrachloride after impurity removal enters the separating tower 3 along with the discharge of the silicon tetrachloride with lower boiling point, in the separating tower 3, the crude titanium tetrachloride is cooled by spraying the silicon tetrachloride liquid from the silicon cooler 4 and the titanium tetrachloride liquid from the heat exchanger 5, the titanium tetrachloride gas with higher boiling point is condensed into liquid and is discharged to the titanium tetrachloride heat exchanger through the separating tower, the silicon tetrachloride with lower boiling point is not condensed and still remains as gas and is discharged to the silicon cooler, so that the silicon tetrachloride in the crude titanium tetrachloride can be effectively separated and removed, the silicon tetrachloride gas and the condensed refined titanium tetrachloride liquid are respectively cooled by the heat exchange of the silicon cooler and the heat exchanger, one part can be collected by extraction, and the other part flows back to the separating tower, the spray liquid is used in the separation tower to realize the continuous operation of the system. The whole system does not use additional chemical substances, and only utilizes the difference of the boiling points of the silicon tetrachloride and the titanium tetrachloride to effectively separate the silicon tetrachloride and the titanium tetrachloride, thereby solving the problem of pollution of the silicon tetrachloride in the production of the titanium tetrachloride and giving consideration to certain economic benefits. Moreover, the utility model discloses the refined titanium tetrachloride who obtains is once refined through the rectifying column, and the knockout tower secondary is refined, and purity obtains improving, and product quality also obtains improving.
The separation column 3 preferably uses a float valve column, and has high tray efficiency and high production capacity.
As one of preferred embodiments, as shown in FIG. 1, a T-shaped pipe is provided at the crude titanium tetrachloride gas outlet of a rectifying column 2, and comprises two branches, one branch is connected with a separation column 3, and the other branch is connected with a condensing column, and the T-shaped pipe is operated in parallel with a refining system in the prior art. The flow of the crude titanium tetrachloride gas entering the condensing tower and the separating tower can be controlled by adjusting the control valve, and different grades of fine titanium tetrachloride can be produced according to actual requirements.
As one of the preferred embodiments, as shown in fig. 1, the bottom of the rectifying tower 2 is further provided with a crude titanium tetrachloride liquid reflux port 22, and the crude titanium tetrachloride liquid reflux port 22 is connected to the evaporator 1. Crude titanium tetrachloride liquid which is generated in the rectifying tower 2 and contains some impurities flows back to the evaporator 1 for further evaporation, and the separation efficiency of titanium tetrachloride and silicon tetrachloride is improved.
As one of the preferred embodiments, as shown in FIG. 1, the system for separating silicon tetrachloride from crude titanium tetrachloride provided by the present invention further comprises a steam scrubber 7 connected to the silicon tetrachloride gas outlet 32 of the separation column 3. When the silicon cooler 4 needs to be overhauled, the steam scrubber can be opened, the non-condensable silicon tetrachloride gas generated in the separation tower 3 can be directly conveyed to directly enter the steam scrubber 7 for treatment, and meanwhile, the negative pressure of the separation tower can be kept, so that the crude titanium tetrachloride gas can enter the separation tower from the top of the rectifying tower 2, and another important guarantee is provided for the continuous operation of the system. Of course, it is also possible to open the control valves at the top of the separation column 3 to the silicon cooler 4 and the vapor scrubber 7 simultaneously, and to supply the non-condensable gas to the silicon cooler 4 and the vapor scrubber 7 simultaneously.
As one of the preferred embodiments, as shown in fig. 2, the system for separating silicon tetrachloride in crude titanium tetrachloride provided by the present invention further includes a silicon storage intermediate tank 6, the silicon storage intermediate tank 6 is provided with a silicon tetrachloride liquid inlet 61, a second silicon tetrachloride liquid outlet 62 and a breathing port 63, the silicon tetrachloride liquid inlet 61 is connected to the first silicon tetrachloride liquid outlet 42 of the silicon cooler 4, the second silicon tetrachloride liquid outlet 62 is connected to the silicon tetrachloride spray liquid inlet 34 of the separation tower 3, the breathing port 63 is connected to the vapor scrubber 7, and the silicon tetrachloride gas volatilized in the tank is sent to the vapor scrubber 7 for absorption. Through setting up silicon storage intermediate tank 6, made things convenient for collection, storage and the spraying backward flow of silicon tetrachloride liquid. Preferably, in order to facilitate the transportation of the silicon tetrachloride liquid, the system further comprises a silicon tetrachloride liquid transportation pump 64, the inlet end of the silicon tetrachloride liquid transportation pump 64 is connected with the second silicon tetrachloride liquid outlet 62 of the silicon storage intermediate tank 6, the outlet end is divided into two branches, one branch is connected with the silicon tetrachloride spraying liquid inlet 34 of the separation tower 3, the other branch is connected with the top of the silicon storage intermediate tank 6 and used for the backflow of the silicon tetrachloride liquid, and the purpose of setting the other branch is to protect the silicon tetrachloride liquid transportation pump 64 itself and must set backflow to stabilize the pump outlet pressure.
As one preferred embodiment, as shown in fig. 2, the system for separating silicon tetrachloride from crude titanium tetrachloride provided by the present invention further includes a titanium storage intermediate tank 8, wherein the titanium storage intermediate tank 8 is provided with a second refined titanium tetrachloride liquid inlet 81 and a third refined titanium tetrachloride liquid outlet 82, the second refined titanium tetrachloride liquid inlet 81 is connected to the first refined titanium tetrachloride liquid outlet 33 of the separation tower 3, and the third refined titanium tetrachloride liquid outlet 82 is connected to the first refined titanium tetrachloride liquid inlet 51 of the heat exchanger 5. By arranging the titanium storage intermediate tank 8, the collection, storage and spraying reflux of the refined titanium tetrachloride liquid are facilitated. Further preferably, in order to facilitate the transportation of the refined titanium tetrachloride liquid, the system further comprises a refined titanium tetrachloride liquid transportation pump 83, the inlet end of the refined titanium tetrachloride liquid transportation pump 83 is connected with a third refined titanium tetrachloride liquid outlet 82 of the titanium storage intermediate tank 8, the outlet end is divided into two branches, one branch is connected with the first refined titanium tetrachloride liquid inlet 51 of the heat exchanger 5, the other branch is connected with the top of the titanium storage intermediate tank 8 and used for the reflux of the refined titanium tetrachloride liquid, and the purpose of arranging the other branch is that the reflux must be arranged to stabilize the outlet pressure of the pump for the protection of the refined titanium tetrachloride liquid transportation pump 83 itself. Preferably, the titanium storage intermediate tank 8 is further connected with a liquid supplementing pipeline 84, and titanium tetrachloride can be supplemented into the titanium storage intermediate tank 8 through the liquid supplementing pipeline 84 when necessary.
As one preferred embodiment, as shown in FIGS. 1-2, a silicon tetrachloride spray liquid inlet 34 of the separation tower 3 is positioned at the top of the separation tower 3, and a titanium tetrachloride spray liquid inlet 35 is positioned at the middle of the separation tower 3. The silicon tetrachloride spraying liquid inlet 34 and the titanium tetrachloride spraying liquid inlet 35 are positioned in different areas of the separation tower, namely, the crude titanium tetrachloride gas is sprayed and cooled from different areas of the separation tower, so that the heat exchange efficiency can be improved, and the silicon tetrachloride in the refined titanium tetrachloride is reduced to a lower level.
As one of the preferred embodiments, as shown in fig. 1-2, the system for separating silicon tetrachloride from crude titanium tetrachloride provided by the present invention further comprises a steam scrubber pump 71, wherein the inlet end of the steam scrubber pump 71 is connected to the bottom of the steam scrubber 7, and the outlet end of the steam scrubber pump 71 is connected to the top of the steam scrubber 7, for self-spraying and back-flowing of the steam scrubber. By providing a steam scrubber pump 71, repeated spraying of the washing liquid is available. The washed gas can be merged into the deslagging treatment pipeline in the prior art through a steam washer fan 72 for subsequent treatment.
As one preferred embodiment, as shown in figures 1-2, a sewage discharge port 36 connected with an evaporator is arranged at the bottom in the separation tower 3, and polluted titanium tetrachloride generated by secondary refining in the separation tower can be continuously or discontinuously discharged to the evaporator 1 through the sewage discharge port at the bottom so as to keep the quality of separated silicon tetrachloride.
While the preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the appended claims be interpreted as including the preferred embodiment and all such alterations and modifications as fall within the scope of the invention. It will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (10)

1. A system for separating silicon tetrachloride in crude titanium tetrachloride comprises an evaporator and a rectifying tower connected with the evaporator, wherein the rectifying tower is used for generating crude titanium tetrachloride gas containing silicon tetrachloride and is characterized by also comprising a separation tower, a silicon cooler and a heat exchanger;
the separation tower is connected with the rectifying tower and is used for spraying, cooling and separating the crude titanium tetrachloride gas from the rectifying tower into refined titanium tetrachloride liquid and silicon tetrachloride gas;
the silicon cooler is connected with the separation tower and is used for cooling the silicon tetrachloride gas from the separation tower, and one part of the cooled silicon tetrachloride liquid flows back to the separation tower and is used for spraying and separating crude titanium tetrachloride gas;
the heat exchanger is connected with the separation tower and is used for cooling the fine titanium tetrachloride liquid from the separation tower, and one part of the cooled fine titanium tetrachloride liquid flows back to the separation tower and is used for spraying and separating the crude titanium tetrachloride gas.
2. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 1, wherein,
the rectifying tower is also connected with a condensing tower.
3. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 1, wherein,
and a crude titanium tetrachloride liquid reflux opening is formed in the bottom of the rectifying tower and is connected with the evaporator.
4. The system for separating silicon tetrachloride from crude titanium tetrachloride according to any one of claims 1 to 3, wherein,
the system also comprises a steam scrubber which is connected with the separation tower and is used for receiving and scrubbing the silicon tetrachloride gas from the separation tower.
5. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 4, wherein,
the silicon storage intermediate tank is connected with the silicon cooler at one end and connected with the separation tower at the other end, and is used for storing silicon tetrachloride liquid from the silicon cooler and discharging a part of the silicon tetrachloride liquid to the separation tower to be used as spraying liquid; the silicon storage intermediate tank is also provided with a breathing port, and the breathing port is connected with the steam washer.
6. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 1, wherein,
the device also comprises a titanium storage intermediate tank, wherein one end of the titanium storage intermediate tank is connected with the separation tower, the other end of the titanium storage intermediate tank is connected with the heat exchanger, and the titanium storage intermediate tank is used for storing the refined titanium tetrachloride liquid from the separation tower and discharging a part of the refined silicon tetra-titanate liquid to the heat exchanger.
7. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 5, wherein,
still include silicon tetrachloride liquid delivery pump, silicon tetrachloride liquid delivery pump the inlet end with store up the silicon tundish and connect, the exit end divide into two branches, a branch with the knockout tower is connected, another branch with store up the silicon tundish top and connect.
8. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 6, wherein,
the titanium storage device is characterized by further comprising a refined titanium tetrachloride liquid delivery pump, wherein the inlet end of the refined titanium tetrachloride liquid delivery pump is connected with the titanium storage intermediate tank, the outlet end of the refined titanium tetrachloride liquid delivery pump is divided into two branches, one branch is connected with the heat exchanger, and the other branch is connected with the top of the titanium storage intermediate tank.
9. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 1, wherein,
the separation tower is provided with a silicon tetrachloride spraying liquid inlet and a titanium tetrachloride spraying liquid inlet, the silicon tetrachloride spraying liquid inlet is positioned at the top of the separation tower, and the titanium tetrachloride spraying liquid inlet is positioned in the middle of the separation tower.
10. The system for separating silicon tetrachloride from crude titanium tetrachloride according to claim 4, wherein,
the steam scrubber device is characterized by further comprising a steam scrubber pump, wherein the inlet end of the steam scrubber pump is connected with the bottom of the steam scrubber, and the outlet end of the steam scrubber pump is connected with the top of the steam scrubber and used for spraying and refluxing of the steam scrubber.
CN202020599544.5U 2020-04-21 2020-04-21 System for separating silicon tetrachloride in crude titanium tetrachloride Active CN212467172U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114832417A (en) * 2022-04-21 2022-08-02 洛阳双瑞万基钛业有限公司 System for recovering titanium tetrachloride in refined low-boiling-point distillate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114832417A (en) * 2022-04-21 2022-08-02 洛阳双瑞万基钛业有限公司 System for recovering titanium tetrachloride in refined low-boiling-point distillate
CN114832417B (en) * 2022-04-21 2024-02-02 洛阳双瑞万基钛业有限公司 Titanium tetrachloride recovery system in refined low boiling point distillate

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