KR101919970B1 - Manufacturing apparatus of titanium tetrachloride - Google Patents

Abstract

Ores containing iron and titanium; Goat; And a carbon source to produce a first product containing iron chloride and a precipitate containing titanium; The precipitate connected to the first reaction unit and moved from the first reaction unit; Goat; And a carbon source to produce a second product containing titanium tetrachloride; A first condenser connected to the first reaction unit and condensing the first product moved from the first reaction unit; And a second condenser connected to the second reaction unit and condensing the second product moved from the second reaction unit.

Description

TECHNICAL FIELD [0001] The present invention relates to a titanium tetrachloride (TiCl4)

The present invention relates to an apparatus for producing titanium tetrachloride using an ore containing iron and titanium.

The conventional apparatus for producing titanium tetrachloride (TiCl ₄ ) is characterized in that the ore such as aluminum (FeTiO ₃ ) is partially reduced with a carbon source or the like and leached into dilute sulfuric acid. First, the ore is charged into a rotary kiln together with a carbon source, and the Fe ₂ O ₃ contained in the ore is partially reduced with FeO at 800 ° C to 950 ° C. In this process, CO and CO ₂ gases are generated.

The partially reduced ore is slowly cooled to prevent reoxidation, then the unreacted carbon source is separated and the ore without Fe ₂ O ₃ is sent to the leaching process.

In the leaching step, the spent sulfuric acid generated in the process of producing high purity titanium dioxide (TiO2) by the sulfuric acid method is leached into regenerated dilute sulfuric acid by the use of ammonia as follows.

TiO ₂ · FeO + H ₂ SO ₄ = FeSO ₄ + TiO ₂ + H ₂ O -

Therefore, in the conventional method as described above, since titanium tetrachloride has to be prepared from titanium dioxide after extracting high purity titanium dioxide from ores such as ilmenite, the process by the production apparatus is complicated and the process time is long.

It should be understood that the foregoing description of the background art is merely for the purpose of promoting an understanding of the background of the present invention and is not to be construed as an admission that the prior art is known to those skilled in the art.

KR 2001-0021618

Provided is a titanium tetrachloride producing apparatus capable of obtaining iron chloride and titanium tetrachloride from vapor ore containing iron and titanium and obtaining high purity iron chloride and titanium tetrachloride through selective chlorination reaction.

According to an aspect of the present invention, there is provided an apparatus for producing titanium tetrachloride, comprising: a ore containing iron and titanium; Goat; And a carbon source to produce a first product containing iron chloride and a precipitate containing titanium; A first reaction part connected to the first reaction part, and the sediment and chlorine moved from the first reaction part; And a carbon source to produce a second product containing titanium tetrachloride; A first condenser connected to the first reaction unit and condensing the first product moved from the first reaction unit; And a second condenser connected to the second reaction unit and condensing the second product moved from the second reaction unit.

And an exhaust unit connected to the first reaction unit for activating the ore containing iron and titanium and activating the ore to be charged into the first reaction unit.

Wherein the roasting chamber is provided with a roasting chamber in which the ore is activated, and the roasting chamber is maintained at a temperature of 800 ° C to 1100 ° C; A hopper for supplying the ore to the roasting space through a charging path connected to the roasting body; A gas supply connected to a lower portion of the roasting body and supplying an inert gas to the roasting space; And a reservoir connected to a lower portion of the roasting body and discharging activated ore in the roasting space to store the ore.

A filter connected to the roasting body for discharging the gas out of the generated water generated by the activation of the ore and filtering the solids; And a supply path connecting one end to the filter and the other end communicating with the charging path so that the filtered solid material is supplied to the roasting space along the charging path.

Wherein the first reaction unit includes an activated ore supplied with activated ores from the discharge unit; Goat; A first reaction body provided with an inner space through which a reaction of the carbon source and the carbon source is performed; And a first temperature controller disposed outside the first reaction body and maintaining the temperature of the internal space at 800 ° C to 1100 ° C.

Wherein the first reaction unit connects the reservoir and the first reaction body, and receives ore activated ore from the reservoir and supplies activated ores to the internal space; A first gas supply unit connected to a lower portion of the first reaction body and supplying chlorine or an inert gas to the internal space; And a first carbon source supplier connected to an upper portion of the first reaction body and supplying a carbon source to the inner space.

The first reaction unit may include a first supply path for communicating the first gas supply unit and the internal space; And a first control valve installed on the first supply path and interrupting the entry and exit of chlorine or an inert gas.

The first condenser is connected to the upper portion of the first reaction body and the first condensation space formed therein for condensing the first product may be maintained at 20 ° C to 250 ° C.

Wherein the first condensing portion includes a first condensing body having the first condensing space therein; And a first ejector connected to an upper portion of the first condensing main body and discharging exhaust gas containing unreacted chlorine out of the first product to the outside.

The first condenser includes a condensing duct connecting the first reaction body and the first condensation body; And a temperature controller disposed on the outer side of the condensing furnace to maintain the temperature inside the condensing furnace at 700 ° C to 800 ° C.

Wherein the second reacting portion is supplied with the precipitate from the first reaction portion, the precipitate; Goat; And a carbon source in the reaction space; And a second temperature controller disposed outside the second reaction body and maintaining the temperature of the reaction space at 800 ° C to 1100 ° C.

The second reaction unit connects the first reaction body and the second reaction body, and the movement path moves the precipitate to the reaction space. A second gas supply unit connected to a lower portion of the second reaction unit and supplying chlorine or an inert gas into the reaction space; And a second carbon source supplier connected to an upper portion of the second reaction body and supplying a carbon source to the reaction space.

The second reaction unit includes a second supply path for communicating the second gas supply unit and the reaction space; And a second control valve installed on the second supply path for controlling the entry and exit of chlorine or an inert gas.

The second condensing portion is connected to the upper portion of the second reaction body, and the second condensing space formed therein for condensing the second product may be maintained at 20 ° C or lower.

Wherein the second condensing portion includes a second condensing body having the second condensing space therein; And a second ejector connected to an upper portion of the second condensing main body and discharging exhaust gas containing unreacted chlorine out of the second product to the outside.

And a purifier connected to the second condenser and configured to purify the condensed second product.

According to the apparatus for producing titanium tetrachloride as described above, iron chloride and titanium tetrachloride can be obtained by selectively chlorinating iron ore ores containing titanium and subsequently sequentially condense the generated gaseous iron chloride and titanium tetrachloride, thereby obtaining high purity iron chloride and titanium tetrachloride It is possible to do.

1 is a view showing an apparatus for producing titanium tetrachloride according to an embodiment of the present invention.
FIG. 2 is a view showing a refining unit according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings.

1, an apparatus for producing titanium tetrachloride according to an embodiment of the present invention will be described.

The apparatus for producing titanium tetrachloride according to one embodiment of the present invention includes a first reaction unit 100, a second reaction unit 200, a first condensation unit 300, and a second condensation unit 400.

In the first reaction part 100, the reaction between the iron and the titanium-containing ores charged into the inside and the chlorine and the carbon source supplied to the inside may generate the first product containing iron chloride and the precipitate containing titanium.

An ore containing iron and titanium may be charged in the first reaction unit 100 and a space may be provided therein. The ores containing iron and titanium may be iron (Fe) in the form of iron oxide (FeO) and titanium (Ti) in the form of titanium oxide (TiO ₂ ). As the ore, rutile containing titanium, and anatase may be used. Preferably, a low cost Ilmenite ore can be used.

The first reaction unit 100 may be maintained at a temperature of 800 ° C. or higher so that the reaction of chlorine (Cl ₂ ) and carbon source supplied to the inside of the ore as described above can be performed. Specifically, carbon sources such as Cokes, Charcoal and the like can be used and become a source of carbon (C). Ore containing iron and titanium can be activated at temperatures above 800 ° C and can be expressed as FeTiO ₃ .

Activation of ore may mean the removal of unnecessary components from the ore and the state in which iron oxide or titanium oxide can react well with chlorine and carbon sources.

The first chlorination reaction in which the iron oxides of the following formulas (1) and (2) react preferentially with chlorine due to the reaction of ore with chlorine and carbon source in the first reaction section 100 can be performed first. The affinity between iron and chlorine is higher than the affinity between titanium and chlorine, so that the iron chloride reaction takes priority.

The first chlorination reaction as shown in the following formulas (1) and (2) can be performed first at a temperature of 800 캜 or more for about 90 minutes. As the amount of ore increases, the flow rate of chlorine supplied can also increase. Preferably, the flow rate of chlorine can be determined to be about 1000 sccm per kg of ore.

FeTiO ₃ + C + Cl ₂ = FeCl ₂ + CO + TiO ₂ - (1)

2FeTiO ₃ + 2C + 3Cl ₂ = 2FeCl ₃ + 2CO + 2TiO ₂ - (2)

Due to the first chlorination reaction, a gaseous first product containing iron chloride such as FeCl ₂ and FeCl ₃ can be produced. Carbon monoxide (CO) and unreacted chlorine may be further included.

Further, due to the chloride reaction 1 can be a precipitate of a solid phase that contains a titanium oxide such as TiO ₂ produced. An unreacted carbon source and the like may be further included.

The second reaction part 200 is connected to the first reaction part 100. The reaction between the precipitate transferred from the first reaction part 100 and the chlorine and the carbon source supplied to the inside of the reaction part 100 is performed to form a second product containing titanium tetrachloride Can be generated.

The secondary chlorination reaction in which the titanium oxide of the following formulas (3) and (4) reacts with chlorine due to the reaction of the chlorides and the carbon source with the solid precipitate transferred from the first reaction section 100 after the first chlorination reaction Lt; / RTI >

TiO ₂ + C + 2Cl ₂ = TiCl ₄ + CO ₂ - (3)

TiO ₂ + 2C + 2Cl ₂ = TiCl ₄ + 2CO ????? (4)

The second chlorination reaction may produce a second product comprising titanium tetrachloride (TiCl ₄ ). Carbon monoxide, carbon dioxide (CO ₂ ) and unreacted chlorine may be further included.

The inside of the second reaction part 200 may preferably be maintained at 800 ° C or higher so that the second product containing titanium tetrachloride formed from the chloride of the liquid is converted into the vapor phase.

The first condenser 300 is connected to the first reaction unit 100 and the first product moved from the first reaction unit 100 can be condensed.

Preferably, in the case of the first condensing part 300, an internal space communicating with the space inside the first reaction part 100 may be provided. The space inside the first condenser 300 may be maintained at a temperature of 20 to 250 ° C. Accordingly, it is possible to condense the gaseous first product containing the iron chloride transferred from the first reaction section 100 into a solid phase. The iron chloride such as FeCl ₂ collected in the first condenser 300 may be used as a separate resource.

The second condensing part 400 is connected to the reaction part, and the second product moved from the reaction part can be condensed.

Preferably, in the case of the second condensing part 400, an internal space communicating with the space inside the second reaction part 200 may be provided. The space inside the second condenser 400 can be maintained at a temperature of 20 ° C or lower. Accordingly, it is possible to condense the gaseous second product containing titanium tetrachloride, which has been moved from the second reaction section 200, into a liquid phase.

The apparatus for producing titanium tetrachloride according to an embodiment of the present invention may further include a burning unit 500.

The casting part 500 may be connected to the first reaction part 100 so that activated ore is charged into the first reaction part 100 by activating or activating iron or titanium-containing ore charged in the casting part 500.

Preferably, the ore having the space inside the burning part 500 and the ore containing iron and titanium may be charged before the first reaction part 100 is charged. An inert gas such as nitrogen (N ₂ ) may be injected into the interior of the substrate 500 and the space inside the substrate 500 may be maintained at a temperature of 800 ° C or higher. As a result, the ore can be activated by air roasting.

The burner 500 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may include a roasting body 510, a hopper 530, a gas supplier 540, and a reservoir 550.

The roasting body 510 is provided with a roasting space 511 in which activation of ore is performed, and the temperature of the roasting space 511 can be maintained at 800 ° C to 1100 ° C.

In order to activate the ore, a temperature of 800 DEG C or more is required as an effective temperature. If the temperature is higher than 1100 ° C, cohesion may occur between the powders when the ore is present in powder form.

The ore and the carbon source are laminated from the lower part of the roasting space 511 of the roasting body 510 and the inert gas can be supplied to the lower part of the roasting body 510. Activation of the ore in the roasting space 511 can thus be achieved.

A temperature can be formed so that the ore charged in the roasting space 511 of the roasting body 510 can be activated. Such temperature may be 800 ° C to 1100 ° C.

The hopper 530 can provide ore to the roasting space 511 through the charging path 520 connected to the roasting body 510.

The hopper 530 is connected to the roasting body 510 through the charging passage 520 and can provide ore to the roasting space 511. [ The charging path 520 communicates the space inside the hopper 530 with the roasting space 511, and the ore can be moved. The ore containing iron and titanium may be loaded from the hopper 530 into the roasting body 510 and laminated from the bottom of the roasting space 511.

The gas supplier 540 is connected to the lower portion of the roasting body 510 and can supply the inert gas to the roasting space 511.

An inert gas may be blown into the roasting space 511 through the gas supplier 540 to roast the ores. An inert gas at a temperature of 800 ° C to 1100 ° C at which activation of the ore is preferably carried out may be introduced.

The reservoir 550 is connected to the lower portion of the roasting body 510, and the ore activated in the roasting space 511 may be discharged and stored.

The reservoir 550 is connected to the roasting body 510 so that the ore activated in the roasting space 511 can be moved to a space inside the reservoir 550 and stored. Preferably, the activated ore, which has been stored in connection with the first reaction part 100, may be supplied to the first reaction part 100.

The discharging portion 500 of the titanium tetrachloride producing apparatus according to an embodiment of the present invention may further include a filter 560 and a furnace 570.

The filter 560 is connected to the roasting body 510 and is capable of filtering the generated material as the ore is activated by roasting. By filtering the product, gases such as nitrogen and oxygen (O ₂ ) and solids can be separated and the gas can be discharged to the outside. The solids can contain iron and titanium as well as ore.

The supplying path 570 may be connected to the filter 560 at one end and may communicate with the charging path 520 at the other end so that the filtered solids are supplied to the roasting space 511 along the charging path 520.

The solids filtered from the filter 560 can be introduced into the charging path 520 along the providing path 570. The solids may be provided to the roasting space 511 from the charging path 520 where the provision of ore is made.

The first reaction part 100 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may include a first reaction body 110 and a first temperature controller 120.

The first reaction body 110 may be provided with an activated ore from the exhaust part 500 and an internal space 111 through which the activated ore and the carbon and the carbon source are reacted.

The activated ore and the carbon source are laminated from the lower part of the inner space 111 of the first reaction body 110 and the chlorine can be supplied to the lower part of the first reaction body 110. Accordingly, the reaction of chlorine and carbon source with the activated ore in the inner space 111 can be achieved.

The first temperature regulator 120 is disposed outside the first reaction body 110 and can maintain the temperature of the internal space 111 at 800 ° C to 1100 ° C.

In order for the reaction of iron oxide and chlorine and carbon source of ore to be performed, an effective temperature of 800 ° C or more is required. When the temperature is higher than 1100 ° C, when the ore or carbon source is present in the form of powder, coagulation phenomena may occur between powders, which may result in ineffective fluidization.

The first temperature regulator 120 may form a temperature at which the reaction of the activated ore charged in the inner space 111 with the chlorine and the carbon source occurs. Such temperature may be 800 ° C to 1100 ° C.

The first reaction part 100 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may include an ore feeder 130, a first gas feeder 140, and a first carbon source feeder 150.

The ore feeder 130 may connect the first reaction body 110 with the reservoir 550 and may supply activated ores to the internal space 111 by receiving activated ores from the reservoir 550.

The activated ore stored in the reservoir 550 can be transferred to the inner space 111 of the first reaction body 110 through the ore feeder 130. [ The activated ore may be loaded into the first reaction body 110 and laminated from the bottom of the internal space 111.

The first gas feeder 140 is connected to the lower portion of one reaction body and can supply chlorine or an inert gas to the inner space 111.

The first gas supply unit 140 may supply chlorine from the lower portion of the first reaction body 110 to the inner space 111 to allow the first chlorination reaction between iron and chlorine in the ores. Meanwhile, the first gas supplying unit 140 may inject an inert gas such as nitrogen into the inner space 111. The first product in the gaseous phase can be moved to the first condenser 300 by being blown from the bottom of the first reaction body 110.

The first carbon source supply 150 is connected to the upper portion of the first reaction body 110 and can supply the carbon source to the inner space 111.

The first carbon source feeder 150 may charge the carbon source carbon source from the upper portion of the first reaction body 110 to the inner space 111 to allow oxygen present in the ore to react with carbon.

The first reaction part 100 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may further include a first supply path 160 and a first control valve 170.

The first supply passage 160 can communicate the first gas supply unit 140 and the inner space 111. The first gas supply unit 140 and the first reaction unit 110 are connected to each other through the first supply channel 160 so that chlorine or an inert gas can be introduced into the inner space 111 along the first supply channel 160 have.

The first control valve 170 is installed on the first supply path 160 and can interrupt the entry and exit of chlorine or inert gas.

The first chlorination reaction can be induced by controlling the flow rate of chlorine through opening and closing of the first control valve 170 provided on the first supply path 160. Further, the flow rate of the inert gas may be controlled to induce the movement of the first product to the first condenser 300.

The first condenser 300 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention is connected to the upper portion of the first reaction body 110 and includes a first condensation space 311 formed therein for condensing the first product, Lt; RTI ID = 0.0 > 20 C < / RTI >

The first product generated from the first reaction body 110 can be transferred to the first condensation part 300. The first condensing space 311 may be provided in the first condensing part 300 and the first condensing space 311 may communicate with the inner space 111. [

The gaseous iron in the gaseous phase contained in the first product may be changed to a liquid phase at a temperature of about 250 ° C or lower and may change to a solid phase at 20 ° C to 250 ° C.

Temperatures at which the iron chloride can be maintained in the solid phase may be sufficient.

The first condensing space 311 is maintained at 20 ° C to 250 ° C so that at least chloride chloride such as FeCl ₂ and FeCl ₃ can be condensed to a solid phase among the first products in the gaseous phase. Therefore, in the first condensing space 311, the condensed iron chloride can be collected.

The first condenser 300 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may include a first condenser body 310 and a first extractor 320.

The first condensing body 310 may have a first condensing space 311 therein. Accordingly, the condensation of the first product in the first condensing space 311 can be achieved.

The first ejector 320 is connected to the upper portion of the first condensing body 310, and unnecessary gas including unreacted chlorine in the first product can be discharged to the outside.

The first product of the vapor phase may further contain unreacted chlorine, carbon monoxide and the like in addition to the ferric chloride. The unreacted chlorine and carbon monoxide including the carbon monoxide can be discharged to the outside by the first discharger 320 connected to the upper part of the first condensing main body 310.

The first reaction part 100 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may further include a condensation furnace 330 and a temperature holder 340.

The condensing furnace 330 can connect the first reaction body 110 and the first condensation body 310. The inner space 111 and the first condensing space 311 can communicate with each other by the condensing passage 330. Thereby allowing the first product to move from the first reaction body 110 to the first condensation body 310 along the condensation furnace 330.

The temperature maintainer 340 is disposed outside the condensing furnace 330 and can maintain the temperature inside the condensing furnace 330 at 700 ° C to 800 ° C.

The temperature inside the condensing furnace 330 is maintained at 700 to 800 占 폚 through the temperature holder 340 to move the first product to the first condensing part 300 while the first product is maintained in the vapor phase via the condensing furnace 330 Can be maintained. The first product is moved to the first condensing space 311 while maintaining the gaseous state.

The temperature at which the iron chloride in the first product can maintain the gaseous phase may be sufficient.

The second reaction part 200 of the titanium tetrachloride production system according to an embodiment of the present invention may include a second reaction body 210 and a second temperature regulator 220.

The second reaction body 210 may be provided with a reaction space 211 through which the precipitate is supplied from the first reaction part 100 and the reaction between the precipitate and the carbon source is performed.

The deposition of the precipitate is performed from the lower part of the reaction space 211 of the second reaction body 210 and the supply of chlorine to the lower part of the second reaction body 210 can be performed. Accordingly, the reaction of the precipitate with the chlorine and the carbon source can be performed in the reaction space 211.

The second temperature regulator 220 is disposed outside the second reaction body 210 and can maintain the temperature of the reaction space 211 at 800 ° C to 1100 ° C.

A temperature of 800 DEG C or more is required as an effective temperature for the reaction of titanium oxide, chlorine and carbon source of the precipitate. When the temperature is higher than 1100 ° C, when the ore or carbon source is present in the form of powder, coagulation phenomena may occur between powders, which may result in ineffective fluidization. In addition, TiCl ₄ produced in the liquid phase can be changed into gas phase and can be moved smoothly by blowing an inert gas or the like.

The second temperature regulator 220 can form a temperature at which the reaction of the chlorine and the carbon source with the precipitate charged in the reaction space 211 occurs. Such temperature may be 800 ° C to 1100 ° C.

The second reaction unit 200 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may further include a moving path 230, a second gas feeder 240, and a second carbon source feeder 250.

The transfer path 230 connects the first reaction body 110 and the second reaction body 210, and the precipitate can be transferred to the reaction space 211.

Preferably, a discharge port is formed in the lower part of the first reaction body 110, a discharge port is formed in the second reaction body 210, and the transfer path 230 can connect the discharge port and the discharge port. In addition, a height difference may be formed between the discharge port and the discharge port so that the sediment can move to the reaction space 211 along the transfer path 230 by its own weight. That is, the discharge port can be formed at a position higher than the charging port, and the transfer path 230 can linearly connect the discharging port and the charging port.

The second gas supply unit 240 is connected to the lower portion of the second reaction unit 210 and may supply chlorine or an inert gas to the reaction space 211.

The second gas supply unit 240 may supply chlorine from the lower part of the second reaction body 210 to the reaction space 211 to cause the second chlorination reaction of titanium and chlorine in the precipitate. On the other hand, the second gas supply unit 240 can introduce an inert gas such as nitrogen into the inner space 111. The second product in the gaseous phase can be moved to the second condenser 400 by being blown from the bottom of the second reaction body 210.

The second reaction part 200 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may further include a second supply path 260 and a second control valve 270.

The second supply passage 260 can communicate the second gas supply unit 240 and the reaction space 211. The second gas supply unit 240 and the second reaction unit 210 are connected through the second supply channel 260 so that chlorine or inert gas can be introduced into the reaction space 211 along the second supply channel 260 have.

The second control valve 270 is installed on the second supply path 260 and can interrupt the entry and exit of chlorine or inert gas.

The second chlorination reaction can be induced by controlling the flow rate of chlorine through opening and closing of the second control valve 270 provided on the second supply path 260. In addition, the flow rate of the inert gas may be controlled to induce movement of the second product to the second condenser 400.

The second condenser 400 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention is connected to the upper portion of the second reaction body 210 and includes a second condensation space 411 formed therein for condensing the second product, Lt; RTI ID = 0.0 > 20 C < / RTI >

The second product generated from the second reaction body 210 can be moved to the second condensation part 400. A second condensation space 411 may be provided in the second condensing unit 400 and a second condensation space 411 may communicate with the reaction space 211.

The gaseous titanium tetrachloride contained in the second product may be changed into a liquid state at 20 ° C or lower.

The temperature at which the titanium tetrachloride can maintain the liquid phase may suffice.

The second condensation space 411 is maintained at 20 ° C or lower so that at least titanium tetrachloride can be condensed into a liquid phase in the second product of the gaseous phase. Therefore, in the second condensing space 411, the titanium tetrachloride condensed in the liquid phase can be collected.

The second condenser 400 of the apparatus for producing titanium tetrachloride according to an embodiment of the present invention may include a second condenser body 410 and a second extractor 420.

The second condensing body 410 may be provided with a second condensing space 411 therein. Condensation of the second product in the second condensation space 411 can thus be achieved.

The second ejector 420 is connected to the upper portion of the second condensing body 410, and unnecessary gas including unreacted chlorine can be discharged to the outside from the second product.

The second product of the vapor phase may further contain unreacted chlorine, carbon monoxide and carbon dioxide in addition to titanium tetrachloride. The unreacted gas including unreacted chlorine, carbon monoxide, and carbon dioxide except titanium tetrachloride can be discharged to the outside by the second ejector 420 connected to the upper part of the second condensing main body 410.

Referring to FIG. 2, an apparatus for producing titanium tetrachloride according to an embodiment of the present invention may further include a purification unit 600.

The purification unit 600 is connected to the second condenser 400, and the condensed second product can be purified. Accordingly, it may be possible to obtain titanium tetrachloride of high purity.

And may be connected to the second condensing body 410, which constitutes the second condensing part 400. The liquid second product condensed from the second condensation body 410 is moved to the purification section 600 and the second product can be vaporized again by application of high temperature heat. As the second product in the gaseous phase passes through the multi-stage vapor column, impurities are removed and ultimately high purity titanium tetrachloride can be obtained.

The operation of the titanium tetrachloride production apparatus according to one embodiment of the present invention will be described with reference to FIGS. 1 and 2. FIG.

Ore containing iron and titanium can be charged into the roasting space 511 of the roasting body 510 through the hopper 530. [ The inert gas can be blown into the roasting space 511 through the gas supplier 540 to roast the ore. The ore can be activated in an atmosphere in which the temperature of the roasting space 511 is maintained at 800 ° C to 1100 ° C.

The generated matter generated by the activation of the ore can be moved from the roasting space 511 to the filter 560. In the filter 560, the product is separated into gas and solid, and the gas can be discharged to the outside. The solids may be discharged through the furnace 570 and provided to the roasting space 511 again along the charging path 520.

On the other hand, the ore activated in the roasting body 510 can be moved to the reservoir 550. The activated ore stored in the reservoir 550 may be supplied to the first reaction body 110 through the ore feeder 130.

In addition, chlorine may be supplied to the inner space 111 of the first reaction body 110 through the first gas feeder 140 and the carbon source may be supplied through the first carbon source feeder 150.

The reaction of ore, chlorine and carbon source can be carried out at a temperature of 800 ° C to 1100 ° C for about 90 minutes. The primary iron chloride reaction in which the iron oxide of ore reacts with chlorine and carbon sources as shown in the above formulas (1) and (2) to produce a first product containing iron chloride can proceed.

As the inert gas is blown from the first gas feeder 140, the gaseous first product can be moved to the first condenser 300. The precipitate containing titanium oxide may remain in the inner space 111 in a solid state.

The first product may be moved into the first condensing space 311 of the first condensing body 310. The temperature of the first condensing space 311 may be maintained at 20 to 250 ° C. At 20 ° C to 250 ° C, at least the first product, iron chloride, can condense to a solid phase.

The precipitate remaining in the inner space 111 of the first reaction body 110 may be moved to the reaction space 211 of the second reaction body 210 along the transfer path 230. In addition, chlorine may be supplied to the reaction space 211 of the second reaction body 210 through the second gas supply unit 240, and a carbon source may be supplied through the second carbon source supply 250.

The reaction of the precipitate, chlorine and carbon source can be effected at a temperature of 800 ° C to 1100 ° C. The titanium chloride of the precipitate may be reacted with chlorine and the carbon source as shown in the above formulas (3) and (4) to proceed the second chlorination reaction in which a second product containing titanium tetrachloride is produced.

As the inert gas is blown from the second gas feeder 240, the gaseous second product can be moved to the second condenser 400.

The second product may be moved to the second condensation space 411 of the second condensation body 410. The temperature of the second condensation space 411 can be maintained at 20 ° C or lower. The titanium tetrachloride of at least the second product can be condensed into a liquid phase at a temperature of 20 DEG C or lower.

The liquid second product is transferred from the second condensing body 410 to the refining section 600 and is again vaporized, and then, through the multi-stage refining column, high purity titanium tetrachloride can be obtained.

Hereinafter, effects of the selective chlorination reaction according to the present invention will be described with reference to Experimental Examples and Comparative Examples. These experimental examples are only for illustrating the present invention, and the present invention is not limited thereto.

Experimental Example

The ore, chlorine and carbon source containing iron and titanium were fed in the first reaction part maintained at a temperature of 950 ° C and reacted for about 90 minutes.

Then, the first product and the precipitate produced by the reaction were respectively collected and examined for their constituents. The components of the first product and the precipitate are shown in Table 1 below.

The precipitate, chlorine and carbon source were fed to the second reaction part maintained at a temperature of 950 캜 and reacted for about 60 minutes.

The second product produced by the reaction was then collected and the components were investigated. The components of the second product are shown in Table 2 below.

Component (wt%) Al ₂ O ₃ SiO ₂ TiO ₂ Cr ₂ O ₃ MnO Fe ₂ O ₃ FeCl ₂ The first product - - - - 1.81 - 98.19 precipitate 1.30 5.99 86.89 1.38 - 4.44 -

Component (ppm) Li Be Mg Al P Ca V Cr Mn Fe Co Ni Ti The second product One One 10 40 2 4 1000 20 10 400 One 90 Remainder

In Table 1, it can be seen that most of the components are composed of FeCl ₂ as the first product. Further, it can be seen that most of the components are made of TiO ₂ as a precipitate. The iron component of the ore except Fe ₂ O ₃ through the precipitate component was mostly separated by FeCl ₂ reaction with chlorine.

Table 2 shows the remaining chlorides by discharging all chlorine and the like by purge of nitrogen gas. It can be seen that most of them are made of titanium tetrachloride, which is Ti chloride, except metal chlorides which are treated as impurities. It can be confirmed that no iron component was present in the second product except for a small amount of Fe chloride.

The iron chloride and titanium tetrachloride obtained per kg of ore were 1.03 kg and 1.22 kg, respectively. Each of which is separately collected in the first condenser and the second condenser.

Comparative Example

The ore, chlorine, and carbon source containing iron and titanium were fed to an arbitrary space maintained at a temperature of 950 ° C and reacted for about 30 minutes.

The product was then collected by the reaction and the components were investigated. The components of the product are shown in Tables 3 and 4 below.

Component (wt%) CaO FeCl ₃ TiO ₂ FeO _x MgO Al ₂ O ₃ product 0.4 54.4 24.7 19.3 1.1 1.1

Component (ppm) Li Be Mg Al P Ca V Cr Mn Fe Co Ni Ti product One One 160 120 6 One 1890 34 3 6700 One 3 Remainder

Table 3 shows the product by reaction, and the components of the residue are shown separately in Table 4.

Unlike the experimental example in which the reaction of chlorite and carbon source with the precipitate composed mostly of TiO ₂ was possible by reacting the ore with chlorine and carbon source without separately distinguishing the first chlorination reaction and the second chlorination reaction, It is not the produced components.

Compared with the experimental example, the amount of collected iron chloride and titanium tetrachloride was small. Further, unlike the experimental example in which iron chloride and titanium tetrachloride can be obtained in a separated state and the production process can be shortened, chloride and titanium tetrachloride are not separately collected in the comparative example.

While the present invention has been particularly shown and described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the following claims It will be apparent to those of ordinary skill in the art.

100: first reaction part 110: first reaction body
111: internal space 120: first temperature regulator
130: ore feeder 140: first gas feeder
150: first carbon source feeder 160: first carbon source feeder
170: first control valve 200: second reaction part
210: second reaction body 211: reaction space
220: second temperature regulator 230: traveling path
240: second gas feeder 250: second carbon source feeder
260: second supply passage 270: second control valve
300: first condenser 310: first condenser
311: first condensation space 320: first ejector
330: condensing furnace 340: temperature maintaining device
400: second condensing part 410: second condensing body
411: second condensing space 420: second ejector
500: exhaust part 510: roasting body
511: roasting space 520: charging path
530: hopper 540: gas feeder
550: reservoir 560: filter
570: Supplied with 600: Tablet section

Claims (16)

Ores containing iron and titanium; Goat; And a carbon source to produce a first product containing iron chloride and a precipitate containing titanium;
The precipitate connected to the first reaction unit and moved from the first reaction unit; Goat; And a carbon source to produce a second product containing titanium tetrachloride;
A first condenser connected to the first reaction unit and condensing the first product moved from the first reaction unit;
A second condenser connected to the second reaction unit and condensing the second product moved from the second reaction unit; And
And an exhaust unit connected to the first reaction unit so that activated ore is charged into the first reaction unit,
The roasting unit
A roasting body provided with a roasting space for activating the ore;
A hopper for supplying the ore to the roasting space through a charging path connected to the roasting body;
A gas supply connected to a lower portion of the roasting body and supplying an inert gas to the roasting space; And
And a reservoir connected to a lower portion of the roasting body and discharging the activated ore in the roasting space to store. delete The method according to claim 1,
Wherein the roasting body comprises:
Wherein the temperature of the roasting space is maintained at 800 ° C to 1100 ° C. The method of claim 3,
The roasting unit
A filter connected to the roasting body, for discharging the gas out of the generated water generated by the activation of the ore and for filtering solid matter; And
And one end connected to the filter and the other end communicating with the charging path to provide filtered solid matter to the roasting space along the charging path. The method of claim 3,
Wherein the first reaction unit comprises:
An activated ore to which activated ore is supplied from the above-mentioned discharge portion; Goat; A first reaction body provided with an inner space through which a reaction of the carbon source and the carbon source is performed; And
And a first temperature controller disposed outside the first reaction body and maintaining the temperature of the internal space at 800 ° C to 1100 ° C. The method of claim 5,
Wherein the first reaction unit comprises:
An ore feeder connecting the reservoir and the first reaction body and supplying activated ore to the internal space by receiving activated ore from the reservoir;
A first gas supply unit connected to a lower portion of the first reaction body and supplying chlorine or an inert gas to the internal space; And
And a first carbon source supplier connected to an upper portion of the first reaction body and supplying a carbon source to the inner space. The method of claim 6,
Wherein the first reaction unit comprises:
A first supply path communicating the first gas supply unit and the inner space; And
And a first control valve installed on the first supply path and interrupting the entry / exit of chlorine or an inert gas. The method of claim 5,
Wherein the first condenser comprises:
Wherein a first condensing space connected to an upper portion of the first reaction body and formed therein for condensing the first product is maintained at 20 ° C to 250 ° C. The method of claim 8,
Wherein the first condenser comprises:
A first condensing main body having the first condensing space therein; And
And a first discharger connected to an upper portion of the first condensing main body and discharging exhaust gas containing unreacted chlorine to the outside from the first product. The method of claim 9,
Wherein the first condenser comprises:
A condensation path connecting the first reaction body and the first condensation body; And
And a temperature controller disposed on the outside of the condensing furnace to maintain a temperature inside the condensing furnace at 700 ° C to 800 ° C. The method of claim 5,
The second reaction unit includes:
The precipitate is supplied from the first reaction section, and the precipitate; Goat; And a carbon source in the reaction space; And
And a second temperature controller disposed outside the second reaction body and maintaining the temperature of the reaction space at 800 ° C to 1100 ° C. The method of claim 11,
The second reaction unit includes:
A moving path connecting the first reaction body and the second reaction body and moving the precipitate into the reaction space;
A second gas supply unit connected to a lower portion of the second reaction unit and supplying chlorine or an inert gas into the reaction space; And
And a second carbon source supplier connected to an upper portion of the second reaction body and supplying a carbon source to the reaction space. The method of claim 12,
The second reaction unit includes:
A second supply path communicating the second gas supply unit and the reaction space; And
And a second control valve installed on the second supply path for interrupting the entry and exit of chlorine or an inert gas. The method of claim 11,
Wherein the second condenser comprises:
And a second condensation space connected to an upper portion of the second reaction body and formed therein for condensing the second product is maintained at 20 ° C or lower. 15. The method of claim 14,
Wherein the second condenser comprises:
A second condensing main body having the second condensing space therein; And
And a second discharger connected to an upper portion of the second condensing main body and discharging an unnecessary gas containing unreacted chlorine out of the second product to the outside. The method according to claim 1,
And a refining unit connected to the second condensing unit and configured to refine the condensed second product.

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