KR20020023867A - Continuous manufacturing apparatus and method of titanium by exchange type - Google Patents

Abstract

PURPOSE: Continuous titanium manufacturing apparatus and method are provided in which a titanium reduction proceeding reduction device and a reduction terminated reduction device are continuously recovered from or charged into a reaction furnace so that a series of processes for manufacturing titanium are continuously repeated. CONSTITUTION: The continuous manufacturing apparatus of titanium by exchange type comprises a reduction device(100) in which raw materials of titanium, reducing agents and reaction salts are mixed for proceeding reduction; a cooling device(130) which is adhered onto the outer circumferential surface of the reduction device so as to primarily cool the reduction terminated reduction device in a reaction furnace(110); and a crane device(400) capable of taking out the primarily cooled reduction device from the reaction furnace, and continuously putting a separately prepared reduction device(300) into the reaction furnace. The continuous manufacturing method of titanium by exchange type comprises a reduction step of reducing titanium by exhausting oxygen in a reduction device, and heating the raw materials, reducing agents and reaction salts to an appropriate temperature for a certain period of time; a first cooling step of cooling the reduction device so as to recover titanium produced through reduction after terminating the reduction; and a continuous exchange step of taking out the cooled reduction device from the reaction furnace using a crane after the first cooling step, and then continuously putting a separate reduction device into the reaction furnace.

Description

Continuous manufacturing apparatus and method of titanium by exchange type

The present invention relates to an apparatus and method for continuously producing titanium by an exchange type, and in particular, it is possible to continuously recover and load a reduction reaction apparatus in which a reduction reaction of titanium proceeds and a reduction reaction apparatus in which a predetermined reduction reaction is completed from a reactor. Thus, the present invention relates to a titanium continuous production apparatus and method for continuously repeating a series of processes for producing titanium.

In general, titanium is a metal material widely used in aircraft materials, chemical industries requiring corrosion and medical and biomaterials because of its high specific strength and excellent chemical corrosion resistance as well as excellent biocompatibility. However, since titanium is widely used in this manufacturing process, it takes a lot of manufacturing time for a single process, and the power consumption is high because the temperature of the reactor is increased and cooled at every production. There was a problem of this deterioration. A conventional embodiment thereof is shown in FIG. 1.

1 is a configuration diagram illustrating a conventional titanium manufacturing apparatus and method.

Conventional titanium production was made using the Kroll method, which is a kind of metal thermal reduction method by physical contact between raw materials and a reducing agent.

An approximate manufacturing process for this is to charge and mix raw materials, reducing agents and reaction salts in the reaction vessel 9 provided in the reduction reaction apparatus 8 and maintain the vacuum with the vacuum pump 6 while 2) After the gas is introduced, oxygen inside the reduction reaction apparatus 8 is discharged to the gas outlet 7, heated to 700 to 1000 ° C. with the heating element 1, and then subjected to a reduction process for several hours. After this, the power of the reactor was shut off to cool the temperature of the reduction reaction apparatus to room temperature in the reactor to prepare a method in which titanium, which is fixed in the reaction vessel 9, was dissolved and recovered from the reaction salt or the reducing agent.

However, such a titanium manufacturing process takes a long time for the reduction reaction apparatus to cool to room temperature after the reduction reaction is completed, and the life of the heating element is not only shortened as the power of the reactor must be supplied and cut off every time. There is a problem that the productivity and work efficiency is low, and the production cost is high, such as a long time is required when the required temperature is increased and cooled.

Accordingly, an object of the present invention is to devise to solve the above-mentioned drawbacks, and after the reduction reaction is completed, to increase the cooling rate of the reduction reaction apparatus and to cool the outer surface of the reduction reaction apparatus for continuous operation. Was selected to complete the primary cooling, and to recover the reduction reaction apparatus after the primary cooling to a predetermined temperature to the outside by using a crane that can be rotated up, down and rotated to cool to room temperature. . In addition, after the reduction reactor is recovered to the outside of the reactor, a series of titanium manufacturing processes can be carried out continuously by inserting a separate reduction reactor prepared in a preliminary zone into the reactor in order to eliminate the empty time occurring inside the reactor. As a result, the time required for the manufacturing process can be drastically shortened, and the time required for the temperature rise and cooling of the reduction reaction device can be reduced by not supplying and shutting off the heat source supply device of the reactor, and a series of titanium is produced. The purpose of this is to continuously manufacture the titanium by repeating the process.

1 is a configuration diagram for explaining a device and method for manufacturing titanium in the prior art

Figure 2 is a block diagram for explaining the titanium continuous production apparatus by an exchange type according to the present invention

Figure 3 is a detailed view for explaining the titanium continuous production apparatus and method according to the present invention

Figure 4 is a block diagram for explaining the titanium continuous manufacturing method according to the present invention

※ Description of the main parts of the drawings

100: reduction reactor 101: gas inlet

102: locking means 103: cover

104: raw material loading entrance 106: reducing agent entrance

107: vacuum pump 108: gas outlet

110: reaction vessel 120: crane hook

130: 1st cooling unit 140: Agitator

200: reactor 202: groove

210: power supply 220: heating element

230: temperature control device 300: separate reduction reaction device

400: crane 410: crane hanger

500; reduction reaction step 510: charging step

520: oxygen release step 530: heating step

540: titanium production step 600: 1st cooling step

610: refrigerant injection step 620: temperature drop step

700: continuous exchange step 710: recovery reaction unit recovery step

720: secondary cooling stage 730: reduction reactor replacement stage

In order to achieve the above object, the continuous production apparatus of titanium according to the present invention is a reduction reaction apparatus for producing titanium, a cooling apparatus capable of cooling the reduction reaction apparatus, charging, recovering and recovering the reduction reaction apparatus from the reactor. It is achieved as a continuous production apparatus of titanium by an exchange type comprising a crane device manufactured to enable the up, down, rotation of the reduced reaction device and a separate reduction reaction device required for the continuous production process.

The continuous production method of titanium according to the exchange of the present invention is a reduction reaction step in which titanium is produced by the interaction of the reducing agent, the raw material and the reaction salt in the reduction reaction device, cooling the reduction reaction device after the completion of the reduction reaction step 1 It is achieved by a continuous process for producing titanium by a series of exchanges including a primary cooling step, a continuous exchange step of recovering the primary cooled reduction reactor from the reactor and charging a separate reduction reactor into the reactor continuously.

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

Accompanying drawings, Figure 2 is a block diagram illustrating a continuous exchange titanium production apparatus according to the present invention.

The continuous production apparatus of titanium according to the present invention according to the drawings is a reduction reaction apparatus 100 and a reduction reaction apparatus in which a reduction reaction is completed by mixing titanium raw materials, a reducing agent and a reaction salt and proceeding a reduction reaction. Cooling device 130 attached to the outer circumferential surface of the reduction reaction apparatus 100 and the primary cooled reduction reaction apparatus 100 from the reactor 200 to primarily cool the 100 in the reactor 200. It is composed of a crane device 400 that can be pulled out and put separately prepared reduction reaction device 300 into the reactor 200 continuously.

The reduction reaction apparatus 100 is provided with a ring 120 on the outer circumferential surface that can hang the crane hook 410 at the time of recovery and charging of the reduction reaction apparatus 100.

The cooling device 130 is provided with a control valve for transferring liquid and gaseous refrigerant such as water or alcohol for cooling, and quantitatively controlling the amount of the transferred refrigerant.

The crane device 400 is provided with a device capable of hanging the crane hanger 410 on the ring 120 attached to the outer peripheral surface of the reduction reaction device when charging and recovery of the reduction reaction device 100, and rotates up, down, A device is provided which can freely exercise.

Accompanying drawings, Figure 3 is a detailed view for explaining a continuous manufacturing apparatus of titanium according to the present invention.

The continuous production apparatus of titanium according to the present invention according to the drawings is a reaction vessel so that the reduction reaction can be carried out by the physical means of the vacuum means, the raw material and the reducing agent and the reaction salt to prevent the oxidation of titanium combined with oxygen A heat generating means for heating the 110 to an appropriate temperature, and a cooling device 130 attached to the outer circumferential surface of the reduction reaction device so as to realize cooling of the reduction reaction device 100 after the reduction reaction is completed. .

The vacuum means consists of a reduction reaction apparatus 100 and a vacuum pump 107 for generating a vacuum in the reduction reaction apparatus 100. The reduction reaction apparatus 100 includes a reaction vessel 110 capable of containing raw materials, a reducing agent, and a reaction salt therein, and an inert gas inlet for discharging oxygen by injecting argon gas, which is an inert gas ( 101 and an outlet 109, and a cover 103 at the top. This cover 103 is provided with clamping locking means 102 in order to prevent the cover 103 from being opened and closed by vacuum pressure.

On the other hand, the heating means is composed of a reactor 200, and a temperature control device 230 for controlling the temperature generated by the heating element 220 for generating heat using the resistance of the heating wire. The upper part of the reactor 200 is provided with a recess 202 into which the reduction reaction apparatus 100 is inserted, and the heating part 220 is provided at the wall of the recess 202 to generate heat using the resistance of the heating wire. In order to control the temperature generated by the heating element 220, the temperature control device 230 is provided on the side wall surface of the reactor 200. A power switch 210 is provided below the temperature control device.

In addition, the cooling device 130 is provided on the outer circumferential surface of the reduction reaction apparatus 100 for cooling the manufactured titanium.

4 is a block diagram for elucidating a method for continuously manufacturing titanium by an exchange type according to the present invention.

In the continuous production method of titanium according to the present invention according to the drawings, the oxygen is discharged in the reaction vessel, and a reduction reaction step and reduction reaction in which titanium is reduced by heating raw materials, a reducing agent and a reaction salt to a predetermined temperature for a predetermined time. In order to recover the titanium produced through the primary cooling step for the primary cooling of the reduction reaction apparatus and the primary cooled reduction reaction apparatus is recovered from the reactor by a crane, and another reduction reaction apparatus is continuously added to the reactor. Charging consists of a continuous exchange step.

The reduction reaction step 500 is a charging step 510 for charging raw materials, a reducing agent, a reaction salt, and the like into the reaction vessel 110 in the reduction reaction device 100, and discharging oxygen existing in the reduction reaction device 100. In order to discharge the oxygen by continuously introducing an inert gas into the reduction reaction apparatus 100 in order to discharge and the reduction reaction apparatus 100 so that the reduction reaction may occur by physical contact in the molten state Heating step (530) for heating and the reduction reaction is completed is made of a titanium generating step 540 to produce titanium.

The primary cooling step 600 is a step of primarily cooling the reduction reaction apparatus 100 to recover the titanium produced in the reduction reaction step 500, in the cooling apparatus tube 130 attached to the outer circumferential surface of the reduction reaction apparatus. It consists of a temperature drop step 620 to lower the temperature of the reactor 200 by using the refrigerant injection step 610 for injecting the refrigerant and the temperature control device 230 for controlling the heat generating means of the reactor 200.

In the continuous exchange step 700, the reduction reaction device recovery step 710 for recovering the primary cooled reduction reaction device 100 to the outside of the reactor 200 using the crane 400, and the reduction reaction device recovered outside. Reduction reaction apparatus 300 is completed by the second cooling step 720 to cool the room temperature to room temperature by air cooling and the oxygen discharge step 520 of the reduction reaction step 500 in a separate reduction reaction device 300 ) Is newly charged into the reactor (200) and consists of a reduction reaction unit exchange step (730) to continuously perform a series of manufacturing processes.

An embodiment of the present invention will be described in detail with reference to FIGS. 2, 3 and 4.

Titanium oxide (generally TiO ₂ ) as a raw material in the reaction vessel 110 at room temperature, magnesium (Mg) having a strong oxidizing power as a reducing agent and sodium chloride (NaCl), potassium chloride (KCl), lithium chloride (LiCl) as a reaction salt Mix and so on. At this time, depending on the operating conditions, titanium tetrachloride (TiCl ₄ ) as a raw material can be used as a reducing agent with a metal having excellent oxidation power, such as calcium (Ca), potassium (K), sodium (Na), generally known from titanium manufacturers As shown in the actual operation site, at the charging step 510 or the heating step 530 through the raw material charge 104 and the reducing agent charge 105 at the same time or separately depending on the operating conditions, the raw material, reducing agent and reaction salts. In the reaction vessel 110 may be charged. Meanwhile, when the samples are loaded into the reaction vessel 110, the reaction vessel 110 is charged to the reduction reaction apparatus 100 and 10-3 torr (torr) is used by the vacuum pump 107 attached to the reduction reaction apparatus 100. After the vacuum is formed, a series of operations for blowing and discharging argon gas, which is an inert gas, up to 760 torr is performed five times to minimize the amount of dissolved oxygen present in the reduction reaction apparatus 100, and Keep the gas running. In addition, when the reaction temperature is raised to 700 to 1000 ° C. while completely dissolving the raw materials, the reducing agent and the reaction salts in the reaction vessel 110, the agitation is performed using the stirrer 140 to dissolve the reaction vessel 110. In), the following reaction occurs.

MX + R = M + RX

Here, MX represents a raw material and R represents a reducing agent. Therefore, when titanium oxide is used as a reducing agent and magnesium is used as a raw material, the reduction reaction is as follows.

TiO ₂ + 2Mg → Ti + 2MgO ①

If titanium oxide is used as a raw material and calcium is used as a reducing agent, the reduction reaction is as follows.

TiO ₂ + 2Ca → Ti + 2CaO ②

If titanium tetrachloride is used as a raw material and magnesium is used as a reducing agent, the reduction reaction is as follows.

TiCl ₄ + 2Mg → Ti + 2MgCl 2 ③

When titanium tetrachloride is used as a raw material and sodium is used as a reducing agent, the reduction reaction is as follows.

TiCl ₄ + 4Na → Ti + 4NaCl ④

On the other hand, the recovery of titanium precipitated in the reaction vessel 110 after the predetermined process is completed to adjust the temperature controller 230 provided in the reactor 200 to 300 ~ 400 ℃, in order to increase the cooling rate Refrigerant flows through the cooling device tube 130 attached to the outer peripheral surface of the reduction reaction device. In this case, the refrigerant used may be any material effective for the refrigerant including water or alcohol, but water is mainly used in general operation. Meanwhile, when the temperature of the reduction reaction device 100 reaches 300 to 400 ° C., the crane hook 410 is connected to the ring 120 provided on the outer circumferential surface of the reduction reaction device using a crane 400 installed outside to react. Take out the reduction reaction apparatus 100 from the furnace 200 to the outside to perform the cooling from the outside to room temperature. In addition, the continuous reduction of the operation by carrying out the series of manufacturing process mentioned above by charging a new reduction reactor 300 containing the raw material, reducing agent and the reaction salt to the reactor 200 for the continuous manufacturing of the process. The manufacturing process can proceed continuously without.

Therefore, the present invention can shorten the operating time by cooling the reduction reaction device from the outside, and by continuously inserting a separate reduction reaction device into the reactor, continuous operation is possible to increase the production process and work efficiency to increase productivity. Can

As described above, the continuous production apparatus and method of titanium according to the present invention

It takes about 20 hours or more to cool the reduction reaction device from the reactor to room temperature in a general operation site, but it can be cooled in about 5 hours when the method of the present invention is applied, which significantly shortens the time of the manufacturing process. Not only does not supply and shut off the heat source supply device, but also reduce the time required for the temperature rise and cooling of the reduction reaction device, and it is possible to continuously manufacture the titanium manufacturing process. There is an advantage to be improved.

Claims (9)

In the titanium manufacturing apparatus A reduction reaction device in which the raw material of titanium, a reducing agent, a reaction salt, etc. are mixed and charged to advance a reduction reaction; A cooling device attached to an outer circumferential surface of the reduction reaction device for primarily cooling the reduction reaction device in which the reduction reaction is completed; And And a crane device capable of taking out the primary cooled reduction reaction device from the reactor and continuously inserting the separately prepared reduction reaction device into the reactor. The method of claim 1, wherein the reduction reaction device is provided with a ring on the outer circumferential surface of the crane hook when recovering and loading the reduction reaction device, and the reaction vessel and vacuum pressure to charge the raw material, reducing agent and the reaction salt An adjustable vacuum pump and a continuous production apparatus of titanium by exchange type, characterized in that the gas inlet and outlet for discharging the oxygen introduced into the vacuum chamber to the outside. The apparatus of claim 1, wherein the cooling device is attached to an outer circumferential surface of the reduction reaction device to transfer a liquid and gaseous refrigerant such as water or alcohol, and has a control valve that can quantitatively control the amount of refrigerant transferred. Continuous production apparatus of titanium by an exchange type. The crane device according to claim 1, wherein the crane device can hang the crane hook on the hook attached to the outer circumferential surface of the reduction device so that the cooled reduction device can be pulled out of the reactor and the separately prepared reduction device can be continuously inserted into the reactor. A continuous production apparatus of titanium according to the exchange type, characterized in that the device is provided, and the top and bottom are rotatable. 5. The method of claim 4, wherein the number of separate reduction reactors includes one or more separate reduction reactors in order to enable continuous operation while eliminating the white space occurring in the reactor when the reduction reactor is recovered from the reactor. Continuous production apparatus of titanium by exchange type characterized in that it comprises. In the titanium manufacturing method A reduction reaction step of discharging oxygen in the reduction reaction apparatus and heating the raw materials, the reducing agent, and the reaction salt to an appropriate temperature for a predetermined time to reduce titanium; After the reduction reaction is completed, the first cooling step of cooling the reduction reaction apparatus to recover the titanium produced through the reduction reaction; And After the first cooling step, a continuous method of producing titanium by a continuous exchange step of taking out the cooled reduction reaction apparatus from the reactor by the crane and the continuous reduction step of inserting a separate reduction reactor in the reactor continuously. The method of claim 5, wherein the reduction step is a charging step of charging the raw material, the reducing agent and the reaction salt in the reaction vessel in the reduction reaction apparatus, and active gas inside the reduction reaction apparatus to discharge the oxygen present in the vacuum vessel The oxygen discharge step to discharge oxygen by continuously inputting and the heating step of heating the reduction reaction device so that the reduction reaction can occur by physical contact in the molten state, and the titanium production step in which the titanium is produced by the completion of the reduction reaction. Continuous production method of titanium by the exchange, characterized in that consisting of. The method of claim 5, wherein the first cooling step is a step of cooling a reduction reaction device to recover titanium produced in the reduction reaction step, and a refrigerant injection step of injecting a refrigerant into a cooling device tube attached to an outer circumferential surface of the reaction device. Method of continuously manufacturing titanium by an exchange type, characterized in that consisting of a temperature drop step of lowering the temperature of the reactor using a temperature control device for controlling the heating means of the furnace. The method of claim 5, wherein the continuous exchange step is a recovery step of recovering the primary cooled reduction reaction unit to the outside of the reactor using a crane and secondary cooling to cool the reduction reaction unit recovered outside to room temperature by air cooling And a replacement step of continuously charging a new reduction reactor to the reactor to perform a series of manufacturing processes.