CN212504027U - Device for preparing titanium tetrachloride - Google Patents
Device for preparing titanium tetrachloride Download PDFInfo
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- CN212504027U CN212504027U CN202021442159.6U CN202021442159U CN212504027U CN 212504027 U CN212504027 U CN 212504027U CN 202021442159 U CN202021442159 U CN 202021442159U CN 212504027 U CN212504027 U CN 212504027U
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Abstract
A device for preparing titanium tetrachloride is a cylindrical boiling bed, and consists of a boiling section for carrying out main reaction on high-calcium-magnesium high-titanium slag, petroleum coke and chlorine, a transition section for relieving the rising speed of furnace gas, an expansion section for carrying out dilute phase chlorination in the free settling process of dust in the furnace gas and a molten salt section for storing and preserving heat of high-boiling-point chloride in a liquid phase mode, wherein a heating carrier interface at the top end of the molten salt section at the bottommost part is directly communicated with the boiling section at the upper part of the heating carrier interface; the top end of the boiling section is led into the transition section at the upper part of the boiling section through a cone angle of 60 degrees; the expanding section is directly communicated with the upper part of the transition section from the top of the transition section; from the expansion section into the furnace top to the furnace gas outlet. The device can overcome the harsh requirements of the existing device on the content of calcium and magnesium impurities in the high-titanium slag, and is a device suitable for preparing titanium tetrachloride by adopting the high-calcium and high-magnesium high-titanium slag.
Description
Technical Field
The utility model relates to a titanium white powder and titanium sponge industrial production field, concretely relates to device of preparation titanium tetrachloride.
Background
The titanium resource of China is very rich, the reserve is at the head of the world and accounts for 48 percent of the total reserve which is proved in the world, ilmenite accounts for 98 percent of the total reserve of the titanium resource of China, and rutile only accounts for 2 percent.
Ilmenite is subjected to mineral separation to obtain titanium concentrate, and the titanium concentrate is smelted and reduced by an electric furnace, so that titanium dioxide and iron in the titanium concentrate are separated to obtain a high-content titanium dioxide concentrate called high-titanium slag.
The high titanium slag is a main raw material for industrially producing titanium tetrachloride, titanium dioxide and titanium sponge products, 90 percent of ilmenite in China can only produce high-calcium-magnesium high titanium slag products containing calcium oxide and magnesium oxide with the total amount of about 8.5 percent, and the titanium ore which can produce titanium slag products with lower calcium-magnesium oxide content only accounts for a little part.
The boiling chlorination is the main method for industrially producing titanium tetrachloride in China at present, and the high titanium slag suitable for the boiling chlorination production is also obtained by mixing and smelting domestic ores and imported ores.
The process is to perform chlorination reaction on the mixture of high titanium slag and petroleum coke in a fluidized state with chlorine in a fluidized bed furnace, and is a traditional process applied to the production of titanium tetrachloride by a fluidization technology. Because the solid phase and the gas phase are in violent relative motion, the mass transfer and the heat transfer are good, and the production is greatly strengthened. The main disadvantages of this process are: the impurity oxides in the high titanium slag can be chloridized in a boiling chlorination furnace at 800-1000 ℃ to generate corresponding chlorides, CO and CO2And the like. Among these chlorides, those having a boiling point lower than the chlorination temperature, such as FeCl3(sublimation gas), ALCl3(sublimation gas), SiSi4And CO, CO2The gases are mixed with TiCi4Volatilizing the titanium tetrachloride and the titanium tetrachloride to escape from the chlorination furnace, and performing subsequent cooling, dust collection, leaching, settling and filtering treatment to obtain liquid-phase titanium tetrachloride; and chlorides having a boiling point above the chlorination temperature, e.g. CaCl2、MgCl2、FeCl2And MnCl2Etc. with unreacted TiO2And C powder and the like are left in the furnace to form slag. With the progress of chlorination reaction, more and more generated slag is accumulated at the lower part of the fluidized bed furnace, which not only occupies the effective working space of the fluidized bed section, increases the resistance of chlorine gas to destroy the distribution state of chlorine gas, and seriously worsens the production conditions of fluidized bed chlorination, thus forcing us to discharge slag under the conditions of stopping chlorine and stopping material, but also the higher the content of calcium and magnesium oxides in the high titanium slag is, the shorter the slag discharge period is, the higher the slag discharge frequency is, the more the slag discharge process is, the influence on the continuity of chlorination production is undoubtedly caused, and the production can be seriously stopped. In view of the situation, the existing boiling chlorination production process is suitable for high titaniumThe total amount of impurities such as calcium oxide and magnesium oxide in the slag product has strict limiting requirements, the total amount of the impurities such as calcium oxide and magnesium oxide cannot be greater than 1% initially, the demand for high titanium slag is rapidly increased with the increase of the production capacity of titanium tetrachloride in China later, the supply amount of the high titanium slag product capable of meeting the quality requirement is seriously insufficient, the quality limitation on the high titanium slag is forced to be relaxed, the total amount of the calcium oxide and the magnesium oxide is relaxed to be not greater than 2.6%, and even the high titanium slag is obtained by mixing and smelting imported ores and domestic ores.
The existing boiling chlorination process and equipment in China have the following defects:
the titanium resource in China is mainly characterized by high-calcium magnesium oxide, and the existing high-titanium slag raw material conforming to the traditional boiling chlorination for producing titanium tetrachloride is mostly prepared by mixing and smelting domestic ores and imported ores.
Secondly, in the existing boiling chlorination technology and equipment, calcium oxide and magnesium oxide react to form high-boiling-point chlorides such as calcium chloride and magnesium chloride in the process, and the high-boiling-point chlorides are retained at the bottom of the furnace body and mixed with other chlorides and unreacted oxides, so that the chlorination reaction cannot be continuously carried out;
thirdly, the high boiling point chloride remained at the bottom of the furnace is mixed with the unreacted furnace burden, so that the loss of the furnace burden is caused, and the effective utilization rate of the furnace burden is reduced;
fourthly, the high boiling point chloride mixed with the furnace burden can not be recycled due to poor quality, and becomes harmful solid waste residue, thereby causing the waste of valuable materials and environmental pollution.
Disclosure of Invention
The utility model aims at providing a device for preparing titanium tetrachloride by combining the defects of the existing boiling chlorination technical equipment based on the current situation of titanium resources in China, and improving the technical equipment level and technical economic indexes of titanium tetrachloride production in China.
In order to achieve the above object, the utility model provides a following technical scheme:
the device for preparing titanium tetrachloride is a cylindrical boiling bed, and consists of a boiling section (b) for carrying out main reaction on high-calcium-magnesium high-titanium slag, petroleum coke and chlorine, a transition section (c) for relieving the ascending speed of furnace gas, an expansion section (d) for carrying out dilute phase chlorination in the free settling process of dust in the furnace gas and a molten salt section (a) for storing and preserving heat of high-boiling-point chloride in a liquid phase form: the top heating carrier interface of the bottommost molten salt section (a) is directly communicated with the boiling section (b) positioned at the upper part of the top heating carrier interface; a transition section (c) which leads from the top end of the boiling section (b) to the upper part of the boiling section through a cone angle of 60 degrees; the expanding section is directly communicated with the upper part of the transition section (c) from the top part of the transition section; from the expansion section (d) into the furnace top to the furnace gas outlet of the furnace top; the upper part of the boiling section (b), the middle part of the expanding section (d) and the lower part of the furnace top are respectively provided with a plurality of groups of cooling water inlet pipes (2) and cooling water outlet pipes (8) corresponding to the cooling water inlet pipes according to the temperature drop requirement; the furnace top is also provided with a slurry spraying port (1), a titanium tetrachloride nozzle (6) and a furnace gas outlet pipe (7); the middle lower part of the boiling section (b) is provided with a feed inlet (3); the bottom of the fused salt section (a) is provided with a fused salt discharge port (10), the upper surface part is provided with a chlorine distributor (4), the lower part is provided with a heating electrode (5), the whole space is internally provided with a heating carrier (14), and the upper part of the heating carrier (14) is provided with a fault slag discharge port (9); 3 heating electrodes are arranged on the same circumferential plane of the heating electrode (5) and form an included angle of 120 degrees with each other; the chlorine feeding distributor (4) is positioned at the upper part of the heating carrier (14); the molten salt discharge port (10) is positioned at the bottom of the molten salt section.
The device for preparing titanium tetrachloride is characterized in that a heating carrier is filled in a working space of a molten salt section, and the material of the heating carrier simultaneously satisfies the following conditions: (1) does not chemically react with chlorine. (2) Does not pollute the materials. (3) And (4) proper specific resistance. (4) Suitable strength. (5) Good filtering performance on chloride molten salt; the heating carrier is in a form that is convenient for realizing the air flow distribution effect expected by adjusting the bulk density of different areas; sufficient porosity is required between the heating carriers to ensure that the high boiling point chloride has sufficient storage space; the lower part of the heating carrier is uniformly provided with 3 heating electrodes along the circumferential direction, and the 3 heating electrodes penetrate through the furnace shell and extend into the hearth to be contacted with the heating carrier; the upper part of the heating carrier is provided with a chlorine-introducing distributor, and the chlorine-introducing distributor penetrates through the furnace shell and the refractory material lining and extends into the hearth to be distributed on the upper part of the heating carrier; the bottom of the fused salt section is provided with a fused salt discharge port, and the fused salt discharge port penetrates through the refractory lining and the furnace shell from the side part of the bottom surface of the hearth and extends out of the furnace through the runner; the fault slag discharging port penetrates through the refractory lining and the furnace shell from the upper surface side wall of the heating carrier and extends out of the furnace through the runner, and the boiling section is right above the molten salt section; a feeder is arranged at the middle upper part of the boiling section, and the feeder horizontally penetrates through the furnace shell and the refractory lining from the outside of the furnace and extends into the furnace; the furnace top cover is arranged above the expansion section, a furnace gas outlet, a slurry spraying port and a titanium tetrachloride nozzle are arranged on the furnace top cover, and the furnace gas outlet is connected with a dust collection cooler at the downstream of the device.
Preferably, the heating carrier is high-quality carbon blocks with various forms.
Preferably, the heating electrode is a metal-high-quality graphite combined electrode with a water cooling device, and a thermocouple is longitudinally inserted into the electrode from outside to inside to the depth of the refractory lining of the electrode.
Preferably, the chlorine distributor is a special steel-ceramic combined pipe fitting and is arranged on the surface of the upper part of the molten salt section.
Preferably, the heating electrode penetrates through the furnace shell and the refractory material lining and extends into the hearth, and the part extending into the hearth is communicated with the heating carrier.
Preferably, the molten salt discharge port extends out of the furnace through a launder from the side wall of the bottom surface of the hearth through the refractory lining and the furnace shell.
Preferably, the fault slag discharge port penetrates through the refractory material lining and the furnace shell from the side wall of the upper surface of the heating carrier to extend out of the furnace through a launder.
Compared with the prior art, the beneficial effects of the utility model are as follows:
the utility model discloses a carry out innovative design optimization to current boiling chlorination furnace device, formed overall structure and more reasonable new technology and device of function, through the fused salt section that the design has specific function, including setting up heating carrier, heating electrode, leading to chlorine distributor and fused salt discharge port, possessed even chlorine air current distribution and preheat, fused salt purification, heat preservation, storage and controllable emission function, solved the usable problem that is fit for the titanium resource characteristics (high calcium magnesium high titanium sediment) raw materials of china; the high-boiling-point chloride smoothly enters the molten salt section from the boiling section in a molten state, so that the adverse effect on the continuous stability of the production caused by the retention and accumulation of the high-boiling-point chloride at the lower part of the boiling section is avoided, and the continuous stable operation of the production of preparing titanium tetrachloride by using the high-calcium-magnesium high-titanium slag through boiling chlorination is realized; the thermodynamic and kinetic conditions of the unreacted furnace charge falling into the bottom of the fluidized bed (the upper surface of the heating carrier) for chlorination reaction are enhanced, and the utilization rate of raw materials is improved; improves the quality of the high-boiling-point chlorine salt so that the high-boiling-point chlorine salt becomes a useful material.
Drawings
Fig. 1 is a schematic structural diagram of the device of the present invention.
In the figure: a fused salt section, a boiling section b, a transition section c, an expansion section d, a slurry spraying port 1, a cooling water inlet pipe 2, a charging port 3, a chlorine distributor 4, a heating electrode 5, a titanium tetrachloride nozzle 6, a furnace gas outlet pipe 7, a cooling water outlet pipe 8, a fault slag discharge port 9, a fused salt discharge port 10, a refractory lining of the expansion section 11, a refractory lining of the boiling section 12, a refractory lining of the fused salt section 13 and a heating carrier 14.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Referring to the attached drawings, the device for preparing titanium tetrachloride comprises a molten salt section a, wherein a heating carrier 14 filled in the whole working space is arranged, and in order to meet the comprehensive performance of the heating carrier, the heating carrier is a high-quality carbon block.
The size of the working space of the molten salt section and the gaps among the heating carriers determine the capacity of the molten salt, and the capacity needs to be determined according to the capacity of the device and the characteristics of raw materials.
When the heating carrier carbon block 14 is filled, the heating carrier carbon block is closely contacted with the working surface of the heating electrode 5, so that the heating electrode 5 and the heating carrier 14 are ensured to work normally.
The heating electrode 5 is a water-cooling metal-graphite electrode with excellent performance.
The upper part of the heating carrier 14 is reasonably arranged, which is beneficial to the chlorination of the unreacted oxides (furnace burden) falling on the surface and the filtration and purification of the molten salt, is beneficial to the further uniform distribution of the chlorine flow, and has the function of a chlorine pre-distributor.
The heating electrode 5 is arranged on the lower portion of the molten salt section, so that molten salt can become an effective conductor, and meanwhile, the electrode is effectively protected by the molten salt.
A plurality of groups of cooling water inlet pipes 2 and corresponding cooling water outlet pipes 8 are arranged in the furnace, so that the temperature reduction requirement of the airflow in the furnace is ensured.
The expansion section refractory lining 11, the boiling section refractory lining 12 and the molten salt section refractory lining 13 ensure that the boiling chlorination furnace can bear the working performance under the environment of high temperature and corrosive medium for a long time.
The chlorine distributor (4) is arranged on the upper surface or a slightly lower part of the molten salt section heating carrier according to the requirement of uniform distribution of chlorine gas flow.
The fault slag discharge port 9 is used for discharging slag when the pressure difference of the furnace is increased to exceed the normal range after the unreacted oxide solid residue layer accumulated on the heating carrier 14 is thickened to a certain degree in the normal production period of the boiling chlorination furnace.
To sum up, this utility model device spouts mud mouth 1, cooling water import pipe 2, feed inlet 3, leads to chlorine distributor 4, heating electrode 5, titanium tetrachloride spout 6, burner gas outlet pipe 7, cooling water outlet pipe 8, trouble row cinder notch 9, fused salt discharge port 10, enlarges the fire-resistant inside lining of section 11, boiling section fire-resistant inside lining 12, the fire-resistant inside lining of fused salt section 13 and the accurate combination of heating carrier 14 through the bell, has formed a preparation titanium tetrachloride's that possesses complete function device. The problem of availability of the raw material of the high-calcium high-magnesium high-titanium slag is solved; the high-boiling-point chloride smoothly enters the molten salt section from the boiling section in a molten state, so that the adverse effect on the continuous stability of the production caused by the retention and accumulation of the high-boiling-point chloride at the lower part of the boiling section is avoided, and the continuous stable operation of the production of preparing titanium tetrachloride by using the high-calcium-magnesium high-titanium slag through boiling chlorination is realized; the thermodynamic and kinetic conditions of the unreacted furnace charge falling into the bottom of the fluidized bed (the upper surface of the heating carrier) for chlorination reaction are enhanced, and the utilization rate of raw materials is improved; improves the quality of the high-boiling-point chlorine salt so that the high-boiling-point chlorine salt becomes a useful material.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The device for preparing titanium tetrachloride is a cylindrical boiling bed, and consists of a boiling section (b) for carrying out main reaction on high-calcium-magnesium high-titanium slag, petroleum coke and chlorine, a transition section (c) for relieving the ascending speed of furnace gas, an expansion section (d) for carrying out dilute phase chlorination in the free settling process of dust in the furnace gas and a molten salt section (a) for storing and preserving heat of high-boiling-point chloride in a liquid phase form, and is characterized in that: the top heating carrier interface of the bottommost molten salt section (a) is directly communicated with the boiling section (b) positioned at the upper part of the top heating carrier interface; a transition section (c) which leads from the top end of the boiling section (b) to the upper part of the boiling section through a cone angle of 60 degrees; the expanding section is directly communicated with the upper part of the transition section (c) from the top part of the transition section; from the expansion section (d) into the furnace top to the furnace gas outlet.
2. The apparatus for producing titanium tetrachloride according to claim 1, wherein: the upper part of the boiling section (b), the middle part of the expanding section (d) and the lower part of the furnace top are respectively provided with a plurality of groups of cooling water inlet pipes (2) and cooling water outlet pipes (8) corresponding to the cooling water inlet pipes according to the temperature drop requirement; the furnace top is also provided with a slurry spraying port (1), a titanium tetrachloride nozzle (6) and a furnace gas outlet pipe (7), the middle lower part of the boiling section (b) is provided with a feed inlet (3), the bottom of the fused salt section (a) is provided with a fused salt discharge port (10), the upper surface or the lower part is provided with a chlorine distributor (4), the lower part is provided with a heating electrode (5), the whole space is internally provided with a heating carrier (14), and the upper part of the heating carrier (14) is provided with a fault slag discharge port (9).
3. The apparatus for producing titanium tetrachloride according to claim 2, wherein: the same circumferential plane of the heating electrodes (5) is provided with 3 heating electrodes which form an included angle of 120 degrees.
4. The apparatus for producing titanium tetrachloride according to claim 2, wherein: the chlorine feeding distributor (4) is positioned at the upper part of the heating carrier (14); the molten salt discharge port (10) is positioned at the bottom of the molten salt section.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021442159.6U CN212504027U (en) | 2020-07-21 | 2020-07-21 | Device for preparing titanium tetrachloride |
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| CN202021442159.6U CN212504027U (en) | 2020-07-21 | 2020-07-21 | Device for preparing titanium tetrachloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113753945A (en) * | 2021-10-23 | 2021-12-07 | 河北吉诚新材料有限公司 | Composite chlorination preparation method of titanium tetrachloride |
| CN113955797A (en) * | 2020-07-21 | 2022-01-21 | 青海北辰科技有限公司 | Novel process and device for preparing titanium tetrachloride suitable for characteristics of titanium resources in China |
-
2020
- 2020-07-21 CN CN202021442159.6U patent/CN212504027U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113955797A (en) * | 2020-07-21 | 2022-01-21 | 青海北辰科技有限公司 | Novel process and device for preparing titanium tetrachloride suitable for characteristics of titanium resources in China |
| CN113753945A (en) * | 2021-10-23 | 2021-12-07 | 河北吉诚新材料有限公司 | Composite chlorination preparation method of titanium tetrachloride |
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