CN116282139A - Molten salt chlorination furnace cooling method - Google Patents
Molten salt chlorination furnace cooling method Download PDFInfo
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- CN116282139A CN116282139A CN202310143785.7A CN202310143785A CN116282139A CN 116282139 A CN116282139 A CN 116282139A CN 202310143785 A CN202310143785 A CN 202310143785A CN 116282139 A CN116282139 A CN 116282139A
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- chlorination furnace
- titanium tetrachloride
- temperature
- spraying
- furnace
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- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 102
- 150000003839 salts Chemical class 0.000 title claims abstract description 34
- 238000001816 cooling Methods 0.000 title claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 63
- 238000005507 spraying Methods 0.000 claims abstract description 57
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000007921 spray Substances 0.000 claims description 40
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000002893 slag Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 abstract description 6
- 230000003116 impacting effect Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Images
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
-
- 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 discloses a cooling method of a fused salt chlorination furnace, which comprises the following steps that 1) during the chlorination production, the temperature in the chlorination furnace is 750+/-15 ℃, the temperature at the top of the chlorination furnace is 350+/-50 ℃, the fused salt chlorination furnace carries out slurry returning spraying, the medium of the slurry returning spraying is titanium tetrachloride liquid, and the viscosity of the titanium tetrachloride liquid is 3 multiplied by 10 ‑3 Pa·s~10×10 ‑3 Pa.s, wherein the temperature of the titanium tetrachloride liquid is 0-25 ℃; according to the invention, the temperature, viscosity, spraying position and state of the sprayed titanium tetrachloride solution are controlled, so that the cooling efficiency of the chlorination furnace is improved, and the material waste is reduced.
Description
Technical Field
The invention relates to the technical field of inorganic chemical industry, in particular to a cooling method of a molten salt chlorination furnace.
Background
TiCl 4 Is used for producing titanium sponge, titanium white and nano TiO 2 Is also the most basic material in the titanium related industry. In TiCl 4 In the production process, molten salt chlorination plays an indispensable important role, and the principle is that high titanium slag is reacted with chlorine gas mainly through sodium chloride as a medium, and petroleum coke is used for providing a reducing atmosphere during the period to convert oxides in the high titanium slag into chlorides, and the products are mainly titanium tetrachloride and comprise AlCl 3 、FeCl 3 Etc. In the chlorination production process, the middle temperature of the chlorination furnace is maintained at 350+/-5 ℃, the top temperature is controlled at 450+/-50 ℃, in the current molten salt chlorination process, slurry generated by direct condensation is returned to the chlorination furnace to control the temperature of the chlorination furnace, although the slurry can be used as a catalyst for leading reaction to a certain extent, the method can lead to excessive circulation of titanium tetrachloride in a system, and the frequency of salt of the chlorination furnace is increased due to higher solid content in the returned slurry, so that part of materials are discharged out of the chlorination furnace without reaction, and the material is wasted.
Disclosure of Invention
In order to overcome the defects, the invention provides a molten salt chlorination furnace cooling method to solve the problems in the background technology.
The technical scheme of the invention is as follows:
a molten salt chlorination furnace cooling method comprises the following steps:
1) During chlorination production, the temperature in the chlorination furnace is 750+/-15 ℃, the temperature at the top of the furnace is 350+/-50 ℃, the molten salt chlorination furnace performs slurry returning spraying, the medium of the slurry returning spraying is titanium tetrachloride liquid, and the viscosity of the titanium tetrachloride liquid is 3 multiplied by 10 -3 Pa·s~10×10 -3 Pa.s, the fourThe temperature of the titanium chloride liquid is 0-25 ℃;
2) When the temperature in the chlorination furnace in the step 1) is less than 730 ℃, reducing the spraying amount of the sprayed titanium tetrachloride liquid or stopping the slurry returning spraying, and when the temperature is firstly waited to rise to 730-735 ℃, recovering the spraying amount of the sprayed titanium tetrachloride or starting the slurry returning spraying;
3) When the temperature in the chlorination furnace in the step 1) is more than 770 ℃, the spraying amount of the sprayed titanium tetrachloride solution is increased; after the maximum slurry returning spray quantity is started, the temperature of the chlorination furnace is more than 770 ℃, the feeding of the processing material into the chlorination furnace is stopped, the temperature is reduced, and after the normal temperature is recovered, the feeding of the processing material into the chlorination furnace is started.
As a preferable technical scheme, the titanium tetrachloride solution comprises crude titanium tetrachloride.
As the preferable technical scheme, a top spraying device is arranged at the top in the chlorination furnace, a top pulp returning spray head of the top spraying device is positioned at the center of the top in the chlorination furnace, and a nozzle opening of the top pulp returning spray head is lower than a furnace gas outlet of the chlorination furnace by 20 cm.
As a preferable technical scheme, the top slurry returning spray nozzle sprays titanium tetrachloride liquid in a circular state to be separated.
As the preferable technical scheme, a middle spraying device is arranged in the center of the chlorination furnace, a middle pulp returning spray head of the middle spraying device is positioned at 1-2m above a feed inlet of the chlorination furnace, the middle pulp returning spray heads are four middle pulp returning spray heads, and the four middle pulp returning spray heads are oppositely arranged in the chlorination furnace.
As the preferable technical scheme, the middle slurry returning spray nozzle sprays titanium tetrachloride liquid to be separated in a fan-shaped state.
As a preferable technical scheme, the processing material in the step 3) is one or more of high titanium slag and sodium chloride.
The molten salt chlorination furnace cooling method comprises the following steps that 1) during chlorination production, the temperature in the chlorination furnace is 750+/-15 ℃, the temperature at the top of the chlorination furnace is 350+/-50 ℃, the molten salt chlorination furnace performs slurry returning spraying, and a medium of the slurry returning spraying is titanium tetrachloride liquid and titanium tetrachlorideViscosity of liquid 3X 10 -3 Pa·s~10×10 -3 Pa.s, wherein the temperature of the titanium tetrachloride liquid is 0-25 ℃; 2) When the temperature in the chlorination furnace in the step 1) is less than 730 ℃, reducing the spraying amount of the sprayed titanium tetrachloride liquid or stopping the slurry returning spraying, and when the temperature is firstly waited to rise to 730-735 ℃, recovering the spraying amount of the sprayed titanium tetrachloride or starting the slurry returning spraying; 3) When the temperature in the chlorination furnace in the step 1) is more than 770 ℃, the spraying amount of the sprayed titanium tetrachloride solution is increased; after the maximum slurry returning spray quantity is started, the temperature of the chlorination furnace is more than 770 ℃, the feeding of the processing material into the chlorination furnace is stopped, the temperature is reduced, and after the normal temperature is recovered, the feeding of the processing material into the chlorination furnace is started.
The invention has the advantages that:
according to the invention, the temperature, viscosity, spraying position and state of the sprayed titanium tetrachloride solution are controlled, so that the cooling efficiency of the chlorination furnace is improved, and the material waste is reduced.
1. The low-temperature titanium tetrachloride liquid is sprayed, so that the furnace temperature control effect is improved, and the production control difficulty is reduced;
2. the returned titanium tetrachloride solution has low viscosity and does not contain solid impurities, so that the material waste caused by salt discharge is reduced, and the material chlorination efficiency is improved;
3. the position and the spraying state of the spray head are improved, and the spraying efficiency is improved;
4. iron chloride is reduced to return to the molten salt furnace, and the height of molten salt foam slag is reduced;
drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a schematic diagram of a spray head structure of a top spray device and a middle spray device in an embodiment of the invention;
wherein: 1-a middle pulp returning spray head; 2-a nozzle of a middle pulp return nozzle; 3-a liquid dispersion plate of the middle pulp return nozzle; 4-top slurry returning nozzle; 5-nozzles of the top slurry return nozzle; 6-a liquid dispersion plate of the top slurry returning spray head.
Detailed Description
In order to overcome the defects, the invention provides a molten salt chlorination furnace cooling method for solving the problems in the background technology.
A molten salt chlorination furnace cooling method comprises the following steps:
1) During chlorination production, the temperature in the chlorination furnace is 750+/-15 ℃, the temperature at the top of the furnace is 350+/-50 ℃, the molten salt chlorination furnace performs slurry returning spraying, the medium of the slurry returning spraying is titanium tetrachloride liquid, and the viscosity of the titanium tetrachloride liquid is 3 multiplied by 10 -3 Pa·s~10×10 -3 Pa.s, wherein the temperature of the titanium tetrachloride liquid is 0-25 ℃;
2) When the temperature in the chlorination furnace in the step 1) is less than 730 ℃, reducing the spraying amount of the sprayed titanium tetrachloride liquid or stopping the slurry returning spraying, and when the temperature is firstly waited to rise to 730-735 ℃, recovering the spraying amount of the sprayed titanium tetrachloride or starting the slurry returning spraying;
3) When the temperature in the chlorination furnace in the step 1) is more than 770 ℃, the spraying amount of the sprayed titanium tetrachloride solution is increased; after the maximum slurry returning spray quantity is started, the temperature of the chlorination furnace is more than 770 ℃, the feeding of the processing material into the chlorination furnace is stopped, the temperature is reduced, and after the normal temperature is recovered, the feeding of the processing material into the chlorination furnace is started.
The titanium tetrachloride solution includes crude titanium tetrachloride.
The top in the chlorination furnace is provided with a top spraying device, a top slurry returning spray head of the top spraying device is positioned in the center of the top in the chlorination furnace, and a nozzle opening of the top slurry returning spray head is 20 centimeters lower than a furnace gas outlet of the chlorination furnace.
The top slurry returning spray head sprays titanium tetrachloride liquid and is separated in a circular state.
The center in the chlorination furnace is provided with a middle spraying device, a middle pulp returning spray head of the middle spraying device is positioned at a position 1-2m above a feed inlet of the chlorination furnace, the middle pulp returning spray heads are four middle pulp returning spray heads, and the four middle pulp returning spray heads are oppositely arranged in the chlorination furnace.
The middle slurry returning spray nozzle sprays titanium tetrachloride liquid and is separated in a fan-shaped state.
The processing material in the step 3) is one or more of high titanium slag and sodium chloride.
The invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
Example 1:
during chlorination production, the temperature of the chlorination furnace is 750+/-15 ℃, the temperature of the top of the chlorination furnace is 350+/-50 ℃, the slurry returning medium is leached slurry, the viscosity of the leached slurry is 5+/-1 Pa.s, the slurry temperature is 80 ℃, and the flow of the middle slurry returning pump is 10m 3 And/h, the flow of the top slurry return pump is 5m 3 And (3) the spraying position is positioned at the middle part of the furnace top and the chlorination furnace, the furnace top is sprayed in the middle of the furnace body, the nozzle opening is 20 centimeters lower than the furnace gas outlet, the spraying position at the middle part of the furnace body is positioned at 1-2m above the feeding inlet and is arranged at four positive positions of the furnace body, two pairs of spraying nozzles are arranged in the use period, the slurry returning nozzle at the top uniformly diffuses after the slurry is impacted, the middle slurry returning nozzle uniformly diffuses in a fan shape after the slurry is impacted, the normal operation of the chlorination furnace is kept, and the discharge amount of waste molten salt is 35-40t.
Example 2:
during chlorination production, the temperature of the chlorination furnace is 750+/-15 ℃, the temperature of the top of the chlorination furnace is 350+/-50 ℃, at this time, the slurry returning medium is crude titanium tetrachloride, and the viscosity of the titanium tetrachloride is 3+/-1 multiplied by 10 -3 Pa.s, temperature 20 ℃, at this time, the flow rate of the middle pulp return pump is 3m 3 And/h, the flow of the top slurry return pump is 1m 3 And (3) the spraying position is positioned at the middle of the furnace top and the chlorination furnace, the furnace top is sprayed in the middle of the furnace body, the nozzle opening is 20 centimeters lower than the furnace gas outlet, the spraying position at the middle of the furnace body is positioned at 1-2m above the feeding opening, the spraying position is arranged at four positive orientations of the furnace body, two pairs of spraying nozzles are arranged in the use period, the top slurry returning nozzle uniformly diffuses the titanium tetrachloride after impacting, the middle slurry returning nozzle uniformly diffuses in a fan shape after impacting, the chlorination furnace is kept to normally operate, and the waste molten salt discharge amount is 30-35t.
A slurry return pump mounted in a rinsing circulation tank of the chlorination furnace is cut off, and a slurry return pump is mounted in a crude titanium collecting tank to supply titanium tetrachloride solution.
Example 3:
during chlorination production, the temperature of the chlorination furnace is 750+/-15 ℃, the temperature of the top of the chlorination furnace is 350+/-50 ℃, at this time, the slurry returning medium is crude titanium tetrachloride, and the viscosity of the titanium tetrachloride is 10+/-1 multiplied by 10 -3 Pa.s, temperature 20 ℃, at this time, the flow rate of the middle pulp return pump is 3.5m 3 And/h, the flow of the top slurry return pump is 1m 3 And (3) the spraying position is positioned at the middle of the furnace top and the chlorination furnace, the furnace top is sprayed in the middle of the furnace body, the nozzle opening is 20 centimeters lower than the furnace gas outlet, the spraying position at the middle of the furnace body is positioned at 1-2m above the feeding opening, the spraying position is arranged at four positive orientations of the furnace body, two pairs of spraying nozzles are arranged in the use period, the top slurry returning nozzle uniformly diffuses the titanium tetrachloride after impacting, the middle slurry returning nozzle uniformly diffuses in a fan shape after impacting, the chlorination furnace is kept to normally operate, and the waste molten salt discharge amount is 30-35t.
A slurry return pump mounted in a rinsing circulation tank of the chlorination furnace is cut off, and a slurry return pump is mounted in a crude titanium collecting tank to supply titanium tetrachloride solution.
Example comparison:
from the practical production situation, the lower the viscosity of the titanium tetrachloride is, the smaller the slurry returning amount is, the salt discharging amount is reduced, the content of titanium dioxide and coke in discharged molten salt is also reduced, and the example can fully explain that in the molten salt chlorination production process, metal substances such as iron, aluminum and the like brought in ore are enough to catalyze the chlorination reaction, the leaching slurry is used for controlling the temperature of the furnace returning, the control difficulty of the chlorination furnace is increased, the slag amount of the molten salt is increased, the raw material consumption is increased, and the temperature of the titanium tetrachloride returning slurry is controlled by using the titanium tetrachloride, so that the control of the production is more facilitated.
The foregoing has shown and described the basic principles, main features and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The cooling method of the molten salt chlorination furnace is characterized by comprising the following steps of:
1) During chlorination production, the temperature in the chlorination furnace is 750+/-15 ℃, the temperature at the top of the furnace is 350+/-50 ℃, the molten salt chlorination furnace performs slurry returning spraying, the medium of the slurry returning spraying is titanium tetrachloride liquid, and the viscosity of the titanium tetrachloride liquid is 3 multiplied by 10 -3 Pa·s~10×10 -3 Pa.s, wherein the temperature of the titanium tetrachloride liquid is 0-25 ℃;
2) When the temperature in the chlorination furnace in the step 1) is less than 730 ℃, reducing the spraying amount of the sprayed titanium tetrachloride liquid or stopping the slurry returning spraying, and when the temperature is firstly waited to rise to 730-735 ℃, recovering the spraying amount of the sprayed titanium tetrachloride or starting the slurry returning spraying;
3) When the temperature in the chlorination furnace in the step 1) is more than 770 ℃, the spraying amount of the sprayed titanium tetrachloride solution is increased; after the maximum slurry returning spray quantity is started, the temperature of the chlorination furnace is more than 770 ℃, the feeding of the processing material into the chlorination furnace is stopped, the temperature is reduced, and after the normal temperature is recovered, the feeding of the processing material into the chlorination furnace is started.
2. The molten salt chlorination furnace cooling method of claim 1, wherein: the titanium tetrachloride solution includes crude titanium tetrachloride.
3. The molten salt chlorination furnace cooling method of claim 1, wherein: the top in the chlorination furnace is provided with a top spraying device, a top slurry returning spray head of the top spraying device is positioned in the center of the top in the chlorination furnace, and a nozzle opening of the top slurry returning spray head is 20 centimeters lower than a furnace gas outlet of the chlorination furnace.
4. The molten salt chlorination furnace cooling method of claim 1, wherein: the top slurry returning spray head sprays titanium tetrachloride liquid and is separated in a circular state.
5. The molten salt chlorination furnace cooling method of claim 4, wherein: the center in the chlorination furnace is provided with a middle spraying device, a middle pulp returning spray head of the middle spraying device is positioned at a position 1-2m above a feed inlet of the chlorination furnace, the middle pulp returning spray heads are four middle pulp returning spray heads, and the four middle pulp returning spray heads are oppositely arranged in the chlorination furnace.
6. The molten salt chlorination furnace cooling method of claim 5, wherein: the middle slurry returning spray nozzle sprays titanium tetrachloride liquid and is separated in a fan-shaped state.
7. The molten salt chlorination furnace cooling method of claim 1, wherein: the processing material in the step 3) is one or more of high titanium slag and sodium chloride.
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CN202310143785.7A CN116282139A (en) | 2023-02-21 | 2023-02-21 | Molten salt chlorination furnace cooling method |
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---|---|---|---|---|
FR1115115A (en) * | 1954-11-26 | 1956-04-19 | Thann Fab Prod Chem | Improvements in the preparation of titanium tetrachloride |
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CN201501799U (en) * | 2009-08-18 | 2010-06-09 | 锦州钛业有限公司 | Spray atomizer of fused salt chlorinating furnace |
CN103626224A (en) * | 2013-11-25 | 2014-03-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Fused salt chlorination furnace for producing titanium tetrachloride |
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CN211770341U (en) * | 2019-12-11 | 2020-10-27 | 河南龙兴钛业科技股份有限公司 | Automatic furnace returning system for titanium tetrachloride slurry |
CN213202390U (en) * | 2020-06-23 | 2021-05-14 | 云南国钛金属股份有限公司 | Titanium tetrachloride slurry spray gun |
CN215063715U (en) * | 2021-06-29 | 2021-12-07 | 攀钢集团攀枝花钛材有限公司 | Flue gas cooling device at spray furnace top of fused salt chlorination furnace |
-
2023
- 2023-02-21 CN CN202310143785.7A patent/CN116282139A/en active Pending
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CN215063715U (en) * | 2021-06-29 | 2021-12-07 | 攀钢集团攀枝花钛材有限公司 | Flue gas cooling device at spray furnace top of fused salt chlorination furnace |
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Title |
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