CN217555830U - System for preparing titanium tetrachloride by using titanium-containing slag as raw material - Google Patents
System for preparing titanium tetrachloride by using titanium-containing slag as raw material Download PDFInfo
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Abstract
The utility model provides a system for use and contain titanium slag as raw materials preparation titanium tetrachloride. The above-mentioned system includes: the device comprises a jet smelting unit and a separation device, wherein a jet smelting device and a negative pressure control device are arranged inside the jet smelting unit, the jet smelting device is provided with a feed inlet, a slag outlet, a dust-containing flue gas outlet and jet spray gun injection inlets, the number of the jet spray gun injection inlets is 1-50, the negative pressure control device is used for controlling the pressure inside the jet smelting device, and the negative pressure control device is a vacuum air exhaust device; the separating device is provided with a dust-containing flue gas inlet and a titanium tetrachloride outlet, and the dust-containing flue gas inlet is communicated with the dust-containing flue gas outlet through a dust-containing flue gas conveying pipeline. Use the technical scheme of the utility model, can not only improve titanium tetrachloride's productivity and the security of technology, can also carry out the heat coupling with carbonization heat absorption capacity and chlorination reaction exotherm and utilize, improve heat utilization rate, simplify process flow, shorten titanium tetrachloride production cycle and reduction in production cost.
Description
Technical Field
The utility model relates to a titanium slag smelting equipment field particularly, relates to a system for use contains titanium slag as raw materials preparation titanium tetrachloride.
Background
Titanium is an important strategic resource, and titanium products are widely applied to the fields of aerospace, energy, automobiles, medical treatment, coatings, textiles, cosmetics and the like. At present, titanium products in the world are mostly derived from high-grade titanium slag produced after iron making by titanium concentrate, and sponge titanium or titanium dioxide is obtained through further treatment; the titanium-containing slag produced by the common vanadium titano-magnetite is difficult to apply to part of common-grade titanium slag due to low titanium grade, high treatment cost and great difficulty.
At present, the application of titanium in titanium slag in China mainly comprises a carbonitriding-chlorination process, sulfuric acid leaching and the like, wherein the carbonitriding-chlorination process mainly comprises the step of firstly, tiO in the titanium slag under the high-temperature condition of an electric furnace 2 Reducing to produce products such as titanium carbide, titanium nitride and the like, quenching all slag in an electric furnace into granules, and then carrying out chlorination treatment in a fluidized bed or a fluidized bed to recover titanium chloride, wherein the technology has the problems of high energy consumption, long flow, high labor intensity and the like, and the heat released by chlorination reaction cannot be fully coupled and utilized with the heat required by the carbonization process; and part of the high titanium slag is used for producing titanium dioxide by a sulfuric acid method.
Due to the problems of large investment, high treatment cost and the like, the existing titanium slag which is applied in large scale only contains high titanium slag produced by ilmenite smelting, but the titanium slag produced by treating vanadium titano-magnetite by a blast furnace and an RKEF process is difficult to be economically utilized.
The prior document (publication number CN 111733331A) provides a method for carrying out oxidation reduction treatment on liquid high-titanium slag produced by smelting in a high-pressure coherent oxygen lance injection electric furnace, so that a black titanium ore phase is converted into an ilmenite phase. The modified titanium slag can be directly leached by hydrochloric acid to obtain qualified boiling titanium chloride. The slag produced by the process is treated by a wet method, and the problems of low recovery rate, energy waste, complex process, difficult control, poor environmental protection effect and the like exist.
The prior document (publication No. CN 108677025A) proposes a method for extracting titanium by using titanium-containing blast furnace slag, which comprises the following steps: firstly, blast furnace slag is finely ground into powder and is placed in a heating furnace, NH in the heating furnace is kept 3 The volume concentration is not less than 10 percent, and the titanium nitride slag is obtained after the reaction for 0.5 to 10 hours at the temperature of between 800 and 1200 ℃; and cooling the titanium nitride slag, adding the cooled titanium nitride slag into a fluidized bed furnace, introducing chlorine, and reacting to obtain the crude titanium tetrachloride. The process has long process flow,High ore grinding cost, high tail gas recovery cost and the like.
The patent (publication No. 103011267B) provides a low-temperature boiling chlorination process for carbonized blast furnace slag, which chlorinates the carbonized blast furnace titanium slag at 520-580 ℃. The technology for treating the blast furnace slag firstly carbonizes the blast furnace titanium slag, and chloridizes the blast furnace titanium slag after cooling, and the temperature of nitrogen under different conditions needs to be controlled in the chlorination stage, so that the technology has the problems of long process flow, complex operation, high treatment cost, incapability of realizing large-scale production and the like.
The existing pyrogenic process for treating titanium-containing blast furnace slag or titanium slag mainly comprises the steps of carbonizing the titanium slag at high temperature in a carbonization furnace, but the carbonization process is an endothermic reaction, so that heat is supplemented by adopting an electrode heat supply mode, the energy consumption of the whole process is extremely high, and the treatment cost is high; meanwhile, the carbonized slag needs to be cooled and then subjected to low-temperature chlorination in a boiling chlorination furnace or a fluidized bed to obtain a titanium chloride crude product, and then the titanium chloride crude product is subjected to subsequent application. Therefore, the process has the problems of long process flow, high energy consumption, high treatment cost and the like caused by the fact that heat between chlorination heat release and carbonization heat absorption cannot be coupled and utilized.
Therefore, a device for producing titanium tetrachloride with short process flow, low energy consumption, low cost, high efficiency and high titanium extraction rate is needed.
SUMMERY OF THE UTILITY MODEL
The main object of the utility model is to provide a system for preparing titanium tetrachloride by using titanium-containing slag as raw material to solve the problems of long process flow, high energy consumption, high cost and low production efficiency of carbon tetrachloride in the prior art.
In order to achieve the above object, the utility model provides a system for use contains titanium sediment as raw materials preparation titanium tetrachloride to contain titanium sediment and include as the system of raw materials preparation titanium tetrachloride: a jet smelting unit and a separation device. The jet smelting unit is internally provided with a jet smelting device and a negative pressure control device, the jet smelting device is provided with a feed inlet, a slag outlet, a dust-containing flue gas outlet and jet spray gun injection ports, the number of the jet spray gun injection ports is 1-50, the negative pressure control device is used for controlling the pressure in the jet smelting device, and the negative pressure control device is a vacuum air extraction device; the separating device is provided with a dust-containing flue gas inlet and a titanium tetrachloride outlet, and the dust-containing flue gas inlet is communicated with the dust-containing flue gas outlet through a dust-containing flue gas conveying pipeline.
Further, the separation device comprises: dust arrester installation and temperature regulating device. The dust collecting device is provided with a dust-containing flue gas inlet and a titanium tetrachloride outlet; the temperature control device is used for controlling the temperature of the dust-containing smoke in the dust collection device.
Furthermore, the height from the jet orifice of the jet spray gun to the surface of the molten pool in the jet smelting device is 1/2-9/10 of the depth of the molten pool, and the depth of the molten pool is 0.5-2.0 m; preferably, the height of the jet orifice of the jet lance from the surface of the molten bath inside the jet smelting device is 8/10 to 9/10 of the depth of the molten bath.
Furthermore, the height of the injection ports of the jet flow spray guns is below the liquid level of the titanium-containing slag in the jet flow smelting device, and the number of the injection ports of the jet flow spray guns is 2-50.
Furthermore, the system for preparing titanium tetrachloride by using titanium-containing slag as a raw material also comprises a waste heat recovery device, and the waste heat recovery device is arranged on the dust-containing flue gas conveying pipeline.
Furthermore, the system for preparing titanium tetrachloride by using the titanium-containing slag as the raw material also comprises a molten titanium-containing slag supply device, wherein the molten titanium-containing slag supply device is provided with a molten titanium-containing slag supply port, and the molten titanium-containing slag supply port is communicated with the feed inlet.
Furthermore, the system for preparing titanium tetrachloride by using titanium-containing slag as a raw material also comprises a titanium tetrachloride refining device, wherein the titanium tetrachloride refining device is provided with a refining inlet and a pure titanium tetrachloride outlet, and the refining inlet is communicated with the titanium tetrachloride outlet.
Further, the titanium tetrachloride refining apparatus is selected from a rectifying apparatus or a fractionating apparatus.
Use the technical scheme of the utility model, make and contain titanium sediment, chlorine and carbon back reductant and carry out the side-blown efflux smelting reaction, above-mentioned smelting process goes on in same system, has simplified the system architecture, can emit the heat with carbonization heat absorption volume and chlorination and carry out the heat coupling and utilize, can realize not having outside heat supply to handle titanium sediment output titanium tetrachloride and other chloride products, and then realize simplifying process flow, shorten production cycle and reduce cost's purpose. In addition, a negative pressure environment is kept in the side-blown jet flow smelting reaction process, so that the leakage of chlorine can be inhibited, and the safety of reaction proceeding is ensured. On the basis, the system can improve the yield of the titanium tetrachloride and the safety of the process, improve the utilization rate of heat in the whole process, simplify the process flow, shorten the production period of the titanium tetrachloride and reduce the production cost of the titanium tetrachloride.
Drawings
The accompanying drawings, which form a part of the present application, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a process flow for producing titanium tetrachloride by smelting titanium-containing slag according to an embodiment of the present invention; and
FIG. 2 is a schematic structural diagram of a system for preparing titanium tetrachloride from titanium-containing slag according to an embodiment of the present invention.
Wherein the figures include the following reference numerals:
100. a jet smelting unit; 110. a jet smelting device; 111. a feed inlet; 112. a slag outlet; 113. a dust-containing flue gas outlet; 120. a negative pressure control device;
200. a separation device; 210. a dust collecting device; 211. a dusty flue gas inlet; 212. a titanium tetrachloride outlet; 220. a temperature control device;
300. a waste heat recovery device;
400. a titanium tetrachloride refining device;
500. a molten titanium-containing slag supply device; 511. a molten titanium-containing slag supply port.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background art, the existing blast furnace titanium-containing slag and the low-grade titanium slag produced by processing vanadium titano-magnetite by the RKEF process are difficult to be economically utilized, and the existing titanium tetrachloride production process has the problems of long process flow, high energy consumption, high cost and low production efficiency of carbon tetrachloride. In order to solve the technical problem, the present application provides a system for preparing titanium tetrachloride by using titanium-containing slag as a raw material, wherein the system for preparing titanium tetrachloride by using titanium-containing slag as a raw material comprises: a jet smelting unit 100 and a separation device 200. The jet smelting unit 100 is internally provided with a jet smelting device 110 and a negative pressure control device 120, the jet smelting device 110 is provided with a feed inlet 111, a slag outlet 112, a dust-containing flue gas outlet 113 and jet spray gun injection ports, the number of the jet spray gun injection ports is 1-50, the negative pressure control device 120 is used for controlling the pressure in the jet smelting device 110, and the negative pressure control device 120 is a vacuum air extraction device; the separating device 200 is provided with a dust-containing flue gas inlet 211 and a titanium tetrachloride outlet 212, and the dust-containing flue gas inlet 211 is communicated with the dust-containing flue gas outlet 113 through a dust-containing flue gas conveying pipeline.
By adopting the system, the side-blown jet smelting reaction of the titanium-containing slag, the chlorine and the carbon-based reducing agent can be carried out. Wherein, the feed inlet 111 can be used for adding solid reaction raw materials (such as titanium-containing slag and reducing agent), and the spray inlet of the jet spray gun can be used for adding chlorine and/or reducing agent. As the reaction proceeds, the generated dust-containing flue gas is discharged from the dust-containing flue gas outlet 113, and the slag obtained by the reaction settles at the bottom of the jet smelting device 110 due to the high density and is discharged from the slag outlet 112 at the bottom of the jet smelting device 110. The dust-containing flue gas enters the separation device 200 through the dust-containing flue gas inlet 211, and titanium tetrachloride obtained after separation treatment is discharged from the titanium tetrachloride outlet 212. Therefore, the titanium tetrachloride can be prepared by using the titanium-containing slag as a raw material through the system. In addition, a negative pressure environment is kept in the side-blown jet flow smelting reaction process, so that the leakage of chlorine can be inhibited, and the safety of reaction proceeding is ensured.
In the side-blown jet smelting reaction process, the chemical reactions mainly comprise: tiO 2 2 +C+Cl 2 →TiCl 4 +CO。
In a preferred embodiment, the separation device 200 comprises: a dust collecting device 210 and a temperature control device 220. The dust collecting device 210 is provided with a dust-containing flue gas inlet 211 and a titanium tetrachloride outlet 212; the temperature control device 220 is used for controlling the temperature of the dust-containing flue gas in the dust collecting device 210. The dust collection device 210 has a good dust collection effect on dust-containing smoke gas brought out from the interior of the jet smelting device 110, and can reduce the impurity content in the titanium tetrachloride crude product; meanwhile, the temperature of the dust-containing flue gas is adjusted by the temperature control device 220, so that chlorides with different melting points (such as silicon tetrachloride, aluminum chloride, ferric chloride and a small amount of calcium chloride and magnesium chloride) can be separated out along with the reduction of the temperature, and then the separation of titanium tetrachloride is realized, and a crude product of titanium tetrachloride is obtained.
In a preferred embodiment, the height of the jet lance outlet from the surface of the molten bath inside the jet smelting device (110) is 1/2 to 9/10 of the depth of the molten bath, and the depth of the molten bath is 0.5 to 2.0m. The position of the injection port of the jet spray gun is arranged in the area, and the injected reaction raw materials can be directly introduced into the titanium-containing slag raw materials in the molten pool, so that the direct contact and reaction among the reaction raw materials are facilitated, and the reaction rate and the generation rate of titanium tetrachloride are improved. In order to further increase the reaction rate and the production rate of titanium tetrachloride, it is preferable that the height of the injection port of the jet lance from the surface of the molten bath inside the jet melting apparatus 110 is 8/10 to 9/10 of the depth of the molten bath.
In a preferred embodiment, the height of the injection ports of the jet lances is below the surface of the titanium-containing slag in the interior of the jet smelting unit 110, and the number of injection ports of the jet lances is 2 to 50. The position of the injection port of the jet flow spray gun is arranged at the position, so that the raw materials injected by the jet flow spray gun can be ensured to be directly contacted with the titanium-containing slag, the reaction raw materials are directly contacted, and the reaction speed and the reaction degree of the jet flow smelting reaction can be further improved; meanwhile, the spraying ports of the jet flow spray guns are arranged, so that reasonable distribution of raw materials in the whole reaction system can be ensured, and the rapid melting, rapid carbonization and chlorination of titanium-containing slag materials on the upper part of the molten slag can be realized. The above-described jet smelting device 110 includes, but is not limited to, a rectangular shape, an oval shape, or a racetrack shape, and the injection port of the jet lance is oriented toward the inside of the molten bath and is oriented in the same direction as the length of the jet smelting device 110.
In a preferred embodiment, the system for preparing titanium tetrachloride by using titanium-containing slag as a raw material further comprises a waste heat recovery device 300, and the waste heat recovery device 300 is arranged on a dust-containing flue gas conveying pipeline. Because the dust-containing flue gas obtained after the smelting treatment has a large amount of heat, the heat in the dust-containing flue gas can be collected through the waste heat recovery device 300, so that the heat energy utilization rate is improved, and the economic utilization value of the titanium-containing slag is improved.
In a preferred embodiment, the system for producing titanium tetrachloride using titanium-containing slag as a raw material further comprises a molten titanium-containing slag supply device 500, wherein the molten titanium-containing slag supply device 500 is provided with a molten titanium-containing slag supply port 511, and the molten titanium-containing slag supply port 511 is provided so as to communicate with the feed port 111. The molten titanium-containing slag supply device 500 is communicated with the feed inlet 111 of the jet flow smelting device 110, so that the molten titanium-containing slag can be directly transferred into the jet flow smelting device 110, the heat contained in the molten titanium-containing slag is brought into a subsequent treatment process, the efficient utilization of heat energy is realized, the heat required to be supplemented in the jet flow smelting reaction is reduced, and the energy consumption is reduced.
Because the purity requirement of titanium tetrachloride is high in the application process, the titanium tetrachloride crude product needs to be refined before application, the impurity content in the titanium tetrachloride crude product is reduced, and then pure titanium tetrachloride is obtained, so that the titanium tetrachloride crude product can be used as a raw material to produce titanium dioxide or titanium sponge in the subsequent process. In a preferred embodiment, the system for producing titanium tetrachloride from a titanium-containing slag as a raw material further comprises a titanium tetrachloride refining apparatus 400, wherein the titanium tetrachloride refining apparatus 400 is provided with a refining inlet and a pure titanium tetrachloride outlet 212, and the refining inlet is provided so as to communicate with the titanium tetrachloride outlet 212. By adopting the titanium tetrachloride refining device 400, the crude product of titanium tetrachloride can be purified, the purity of the crude product of titanium tetrachloride can be improved, and pure titanium tetrachloride can be obtained, so that the pure titanium tetrachloride can be conveniently used as a raw material for preparing titanium dioxide or titanium sponge.
The rectifying device can utilize the properties that each component in the mixture has different volatility and the vapor pressure of each component is different at the same temperature to realize the separation. Fractional distillation is a method of separating a mixture of several volatile components of different boiling points. In a preferred embodiment, the titanium tetrachloride refining apparatus 400 includes, but is not limited to, a rectification apparatus or a fractionation apparatus. The different titanium tetrachloride refining devices 400 are selected to obtain pure titanium tetrachloride with higher purity, so that the pure titanium tetrachloride can be conveniently used as a raw material for preparing titanium dioxide or titanium sponge.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
Using titanium-containing blast furnace slag as raw material, wherein TiO is 2 The content is 25wt%, and the components contained in the raw materials are shown in Table 1. As shown in figure 1, side-blown jet smelting is carried out by using a side-blown smelting furnace, and the negative pressure is-20 Pa. The side-blown jet smelting is carried out by adopting the system structure which takes the titanium-containing slag as the raw material to prepare the titanium tetrachloride and is shown in figure 2.
TABLE 1 content of each component in the titanium-containing blast furnace slag
Molten titanium-containing blast furnace slag (with the temperature of 1350 ℃) directly flows into a molten pool through a feeding hole 111, the depth of the molten pool is 1.5m, and the temperature of a side-blown smelting furnace is set to be 1350 ℃. Spraying anthracite coal powder and nitrogen by using a double-channel spray gun (the number of the spray guns is 20), wherein the average particle size of the coal powder is 1 +/-0.5 mm (the nitrogen is used as carrier gas, and the gas-solid ratio is 20 kg/m) 3 ) Chlorine and nitrogen are mixed by the double-channel spray gun and then sprayed into the molten pool (wherein, chlorine accounts for 85% of the mixed gas of chlorine and nitrogen, and nitrogen is used as cooling gas to protect the spray gun). The height of the jet nozzle of the jet spray gun from the surface of the titanium-containing slag is 1.1m. The conveying concentration of the pulverized coal is 25kg/m 3 。
As shown in figure 1, the titaniferous blast furnace slag reacts with chlorine and coal powder to meltSmelting reaction to generate slag and dust-containing flue gas. Ca and Mg elements in the slag respectively flow out of the slag outlet 112 in the form of molten chloride molten salt. And Ti, al, si and Fe as chlorides TiCl 4 、AlCl 3 、SiCl 4 And FeCl 3 The gas phase to form high temperature dust-containing flue gas. The high-temperature dust-containing flue gas is discharged from the dust-containing flue gas outlet 113, enters the waste heat boiler through the dust-containing flue gas inlet 211, recovers waste heat and is cooled to 350 ℃. Then the dust-containing flue gas is further cooled and separated by a dust collecting device 210, and TiCl can be respectively collected 4 、AlCl 3 、SiCl 4 、FeCl 3 And (5) obtaining a crude product. Coarse TiCl 4 The titanium white powder or the sponge titanium can be used as raw materials for preparing the titanium white powder or the sponge titanium after purification.
In the side-blown jet smelting reaction, 187.43kg anthracite is consumed by each ton of titanium-containing blast furnace slag, and 560.22Nm chlorine is injected 3 Blowing nitrogen 788.43Nm 3 The weight ratio of the titanium-containing slag to the chlorine to the anthracite is 1000; the output slag 681.20kg (64.59wt% CaCl therein) 2 And 26.62wt% MgCl 2 ) The temperature of the dust-containing flue gas is reduced to 350 ℃ after the waste heat of the dust-containing flue gas is recovered by a waste heat boiler, and the dust-containing flue gas is further separated by a separation device 200 to respectively obtain TiCl with the weights of 553.44kg, 418.68kg, 538.21kg and 68.56kg 4 、AlCl 3 、SiCl 4 And FeCl 3 . Rectifying the crude titanium tetrachloride to obtain pure titanium tetrachloride with the purity of 99.89 percent. The yield of the crude titanium tetrachloride product was found to be 93.33%.
Example 2
Using electric furnace smelting titanium slag as raw material, wherein TiO 2 The content was 51.44% and the components contained in the feed are shown in table 2. As shown in figure 1, side-blown jet smelting is carried out by using a side-blown smelting furnace, and the negative pressure is-30 Pa. The side-blown jet smelting is carried out by adopting the system structure which takes the titanium-containing slag as the raw material to prepare the titanium tetrachloride and is shown in figure 2.
TABLE 2 contents of the respective components in the titanium slag smelted in the electric furnace
| TiO 2 | CaO | MgO | SiO 2 | Al 2 O 3 | MnO | V 2 O 5 | FeO |
| 51.44 | 9.69 | 5.06 | 9.69 | 14.43 | 7.21 | 0.50 | 1.29 |
The titanium slag (the temperature is 1600 ℃) smelted by the electric furnace in a molten state directly flows into a molten pool through a feed inlet 111, the depth of the molten pool is 2.0m, and the temperature of a side-blown smelting furnace is 1250 ℃. Pulverized coal and nitrogen are injected by a double-channel spray gun (the number of the spray guns is 20), and the granularity of the pulverized coal is less than 0.5mm (wherein, nitrogen is carrier gas, and the gas-solid ratio is 40kg/m 3 ) Chlorine gas is sprayed into a molten pool, and nitrogen is sprayed through a channel outside a spray gun, wherein the chlorine gas accounts for 70% of the mixed gas of the chlorine gas and the nitrogen gas, and the nitrogen gas is used as cooling gas. The above-mentioned rayThe height of the jet orifice of the flow spray gun from the surface of the titanium-containing slag is 1.6m.
As shown in figure 1, the circuit smelting titanium slag reacts with chlorine and coal powder to carry out smelting reaction, and slag and dust-containing flue gas are generated. Ca and Mg elements in the slag respectively flow out from the slag outlet 112 in the form of molten chloride molten salt. And Ti, al, si and Fe as chlorides TiCl 4 、AlCl 3 、SiCl 4 And FeCl 3 The gas phase to form high temperature dust-containing flue gas. The high-temperature dust-containing flue gas is discharged from the dust-containing flue gas outlet 113, enters the waste heat boiler through the dust-containing flue gas inlet 211, recovers waste heat and is cooled to 350 ℃. Then the dust-containing flue gas is further cooled and separated by a dust collecting device 210, and TiCl can be respectively collected 4 、AlCl 3 、 SiCl 4 、FeCl 3 And (5) obtaining a crude product. Coarse TiCl 4 Purified to be used as a raw material for preparing titanium dioxide or sponge titanium.
In the jet smelting reaction, anthracite 189.04kg is consumed for smelting titanium slag per ton of circuit, and chlorine 562.81Nm is injected 3 Blowing nitrogen 644.96Nm 3 The weight ratio of the titanium-containing slag to the chlorine to the anthracite is 1000.78; producing 292.34kg of molten slag (containing 56.65wt% of CaCl) 2 And 35.01wt% MgCl 2 ) The dust-containing flue gas is cooled to 350 ℃ by a waste heat boiler and is further separated by a separation device 200 to obtain TiCl with the weight of 1197.57kg, 379.41kg, 285.57kg and 22.60kg respectively 4 、AlCl 3 、SiCl 4 And FeCl 3 . Rectifying the crude titanium tetrachloride to obtain pure titanium tetrachloride with the purity of 99.95 percent. The yield of the crude titanium tetrachloride product was found to be 98.07%.
Example 3
The high titanium slag smelted by the submerged arc furnace is used as a raw material, wherein TiO 2 The content was 75wt%, and the components contained in the raw materials are shown in Table 3. As shown in figure 1, side-blown jet smelting is carried out by using a side-blown smelting furnace, and the negative pressure is-40 Pa. The side-blown jet smelting is carried out by adopting the system structure which takes the titanium-containing slag as the raw material to prepare the titanium tetrachloride and is shown in figure 2.
TABLE 3 contents of the components in the high titanium slag smelted by the submerged arc furnace
| TiO 2 | CaO | MgO | SiO 2 | Al 2 O 3 | MnO | V 2 O 5 | FeO |
| 75 | 2 | 8 | 5 | 2 | 1 | 0.2 | 6 |
The high titanium slag (the temperature is 1600 ℃) smelted by the molten state submerged arc furnace directly flows into a molten pool through a feed inlet 111, the depth of the molten pool is 1m, and the temperature of a side-blown smelting furnace is 1450 ℃. Spraying pulverized coal and nitrogen gas (the number of the spray guns is 30) by using a double-channel spray gun, wherein the granularity of the pulverized coal is less than 5mm (the nitrogen gas is carrier gas, and the gas-solid ratio is 10 kg/m) 3 ) Chlorine gas is sprayed by jetsAnd the inner channel of the spray gun is sprayed into the molten pool, wherein chlorine gas accounts for 90% of the mixed gas of chlorine gas and nitrogen gas, and the outer channel of the spray gun is sprayed with nitrogen gas as cooling gas. The height of the jet nozzle of the jet spray gun from the surface of the titanium-containing slag is 0.8m.
As shown in figure 1, the high titanium slag smelted by the submerged arc furnace reacts with chlorine and coal powder to carry out smelting reaction, and slag and dust-containing smoke are generated. Ca and Mg elements in the slag respectively flow out of the slag outlet 112 in the form of molten chloride molten salt. And Ti, al, si and Fe as chlorides TiCl 4 、AlCl 3 、SiCl 4 And FeCl 3 The gas phase to form high temperature dust-containing flue gas. The high-temperature dust-containing flue gas is discharged from the dust-containing flue gas outlet 113, enters the waste heat boiler through the dust-containing flue gas inlet 211, recovers waste heat and is cooled to 350 ℃. Then the dust-containing flue gas is further cooled and separated by a dust collecting device 210, and TiCl can be respectively collected 4 、AlCl 3 、 SiCl 4 、FeCl 3 And (5) obtaining a crude product. Coarse TiCl 4 Purified to be used as a raw material for preparing titanium dioxide or sponge titanium.
In the jet smelting reaction, each ton of the submerged arc furnace smelts high titanium slag and consumes 186.00kg of anthracite, and injects 558.24Nm of chlorine 3 Blowing nitrogen 448.73Nm 3 The weight ratio of the titanium-containing slag to the chlorine to the anthracite is 1000.77; the output slag 215.01kg (containing 16.84wt% CaCl) 2 And 75.01wt% MgCl 2 ) The dust-containing flue gas is cooled to 350 ℃ by a waste heat boiler, the temperature of the dust-containing flue gas is cooled to 350 ℃ after waste heat of the dust-containing flue gas is recovered by the waste heat boiler, and the dust-containing flue gas is further separated by a separating device 200 to respectively obtain TiCl with the weight of 1745.93kg, 66.91kg, 157.89kg and 102.44kg 4 、AlCl 3 、SiCl 4 And FeCl 3 . And rectifying the crude titanium tetrachloride to obtain pure titanium tetrachloride with the purity of 99.4 percent. The yield of the crude titanium tetrachloride product was found to be 98.06%.
Comparative example 1
The difference from example 1 is that: firstly, carrying out carbonization reaction on carbon-based reducing agent coal dust and titanium-containing blast furnace slag in a carbonization furnace, and providing heat for carbonization endothermic reaction through electric heating in the reaction process to obtain molten titanium carbide; and transferring the titanium carbide to a chlorination furnace for chlorination reaction, and separating to obtain titanium tetrachloride. Meanwhile, the carbonization reaction and the chlorination reaction are not controlled to be in a negative pressure environment.
The yield of the titanium tetrachloride crude product was measured to be 78.00%; the purity of the purified titanium tetrachloride obtained after the refining treatment was 80.00%.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
comparing example 1 with comparative example 1, it can be seen that the side-blown jet smelting reaction is performed on the titanium-containing slag, the chlorine and the carbon-based reducing agent, the smelting process is performed in the same system, the system structure is simplified, the heat absorbed by the carbonization reaction and the heat released by the chlorination reaction can be coupled and utilized, the titanium tetrachloride and other chloride products can be produced by treating the titanium slag without external heat supply, and the purposes of simplifying the process flow, shortening the production period and reducing the cost are achieved. In addition, a negative pressure environment is kept in the side-blown jet flow smelting reaction process, so that the leakage of chlorine can be inhibited, and the safety of reaction proceeding is ensured. On the basis, the system can improve the yield of the titanium tetrachloride and the safety of the process, improve the utilization rate of heat in the whole process, simplify the process flow, shorten the production period of the titanium tetrachloride and reduce the production cost of the titanium tetrachloride.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described or illustrated herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A system for preparing titanium tetrachloride by taking titanium-containing slag as a raw material is characterized by comprising the following steps:
the device comprises a jet flow smelting unit (100), wherein a jet flow smelting device (110) and a negative pressure control device (120) are arranged inside the jet flow smelting unit (100), the jet flow smelting device (110) is provided with a feeding hole (111), a slag outlet (112), a dust-containing flue gas outlet (113) and jet flow spray gun injection ports, the number of the jet flow spray gun injection ports is 1-50, the negative pressure control device (120) is used for controlling the pressure inside the jet flow smelting device (110), and the negative pressure control device (120) is a vacuum air extraction device;
the separation device (200) is provided with a dust-containing flue gas inlet (211) and a titanium tetrachloride outlet (212), and the dust-containing flue gas inlet (211) is communicated with the dust-containing flue gas outlet (113) through a dust-containing flue gas conveying pipeline.
2. The system for producing titanium tetrachloride using slag containing titanium as a raw material according to claim 1, wherein said separation device (200) comprises:
the dust collecting device (210), the dust collecting device (210) is provided with the dust-containing flue gas inlet (211) and the titanium tetrachloride outlet (212);
and the temperature control device (220), the temperature control device (220) is used for controlling the temperature of the dust-containing flue gas in the dust collection device (210).
3. The system for producing titanium tetrachloride from titanium-containing slag as a raw material according to claim 1 or 2, wherein the height of the jet lance outlet from the surface of the molten bath inside the jet melting apparatus (110) is 1/2 to 9/10 of the depth of the molten bath, and the depth of the molten bath is 0.5 to 2.0m.
4. The system for producing titanium tetrachloride using titanium-containing slag as a raw material according to claim 3, wherein the height of the injection port of said jet lance from the surface of the molten pool inside said jet melting apparatus (110) is 8/10 to 9/10 of the depth of said molten pool.
5. The system for producing titanium tetrachloride using titanium-containing slag as a raw material according to claim 4, wherein the height of the injection ports of the jet lances is below the liquid level of the titanium-containing slag in the interior of the jet smelting apparatus (110), and the number of the injection ports of the jet lances is 2 to 50.
6. The system for preparing titanium tetrachloride by using titanium-containing slag as a raw material according to claim 4, wherein the system for preparing titanium tetrachloride by using titanium-containing slag as a raw material further comprises a waste heat recovery device (300), and the waste heat recovery device (300) is arranged on the dust-containing flue gas conveying pipeline.
7. The system for producing titanium tetrachloride using titanium-containing slag as a raw material according to claim 6, wherein the system for producing titanium tetrachloride using titanium-containing slag as a raw material further comprises a molten titanium-containing slag supply apparatus (500), the molten titanium-containing slag supply apparatus (500) is provided with a molten titanium-containing slag supply port (511), and the molten titanium-containing slag supply port (511) is provided so as to communicate with the feed port (111).
8. The system for producing titanium tetrachloride using slag containing titanium as a raw material according to claim 7, wherein the system for producing titanium tetrachloride using slag containing titanium as a raw material further comprises a titanium tetrachloride refining apparatus (400), wherein the titanium tetrachloride refining apparatus (400) is provided with a refining inlet and a pure titanium tetrachloride outlet (212), and the refining inlet is provided so as to communicate with the titanium tetrachloride outlet (212).
9. The system for producing titanium tetrachloride using titanium-containing slag as a raw material according to claim 8, wherein said titanium tetrachloride refining apparatus (400) is selected from a rectifying apparatus and a fractionating apparatus.
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