A production process for titanium tetrachloride column water-cooled shower head type feeding

Abstract

This invention relates to the field of titanium tetrachloride production technology, specifically a column-cooled, spray-type feeding process for titanium tetrachloride, comprising the following steps: S1, adding liquid magnesium to the reactor to a set amount; S2, after the temperature reaches the set temperature, starting the titanium tetrachloride feeding device; S3, simultaneously starting the cooling device while starting the titanium tetrachloride feeding; S4, installing a baffle above the outlet of titanium tetrachloride; S5, starting the discharge system; S6, after reduction, transferring to the distillation section. In this column-cooled, spray-type feeding process for titanium tetrachloride, the reactor is modified by adding a water-cooling structure for titanium tetrachloride, connecting cooling water to cool the titanium tetrachloride pipeline, thereby lowering the overall reaction temperature. Furthermore, this process avoids the formation of a hard core due to central overheating in the titanium agglomerate. The baffle above the titanium tetrachloride outlet ensures that the titanium tetrachloride is sprayed into the liquid magnesium, resulting in a more uniform reaction and guaranteeing product quality.

Description

Technical Field

[0001] This invention relates to the field of titanium tetrachloride production technology, and more specifically, to a column-mounted water-cooled shower head type feeding process for titanium tetrachloride. Background Technology

[0002] Titanium sponge is a raw material for titanium processed materials. It is generally light gray granules with a clean surface and no visible inclusions. It also includes defective titanium sponge blocks, such as overheated titanium sponge blocks, oxide titanium sponge blocks with obvious dark yellow and bright yellow color, oxide and nitrogen-rich titanium sponge blocks with dark yellow and bright yellow traces, titanium sponge blocks with obvious chloride residue, and titanium sponge blocks with residues, etc. Titanium sponge is characterized by its low density, high specific hardness, and strong corrosion resistance.

[0003] Both domestic and international industrial production of sponge titanium uses the magnesium reduction of titanium tetrachloride method. This method primarily uses titanium tetrachloride as raw material, and the finished sponge titanium product is obtained through reduction, distillation, and crushing. Specifically, in the reduction and distillation process, a sieve plate is first installed at the bottom of the reaction apparatus. Magnesium is used to reduce titanium tetrachloride to obtain sponge titanium and magnesium chloride. Magnesium chloride is discharged periodically, while the sponge titanium accumulates on the sieve plate to form titanium lumps. After reduction, distillation is used to remove impurities such as magnesium chloride from the titanium lumps, thus obtaining pure sponge titanium. However, a common problem exists in the production of sponge titanium: during the reduction process, a hard core forms in the center of the sponge titanium, causing blockage and affecting its downstream applications. Summary of the Invention

[0004] The purpose of this invention is to provide a column-mounted water-cooled shower-type feeding process for titanium tetrachloride, in order to solve the problem mentioned in the background art where a hard core forms in the center of the sponge titanium during the reduction process, causing blockage and affecting the downstream application of sponge titanium.

[0005] To achieve the above objectives, the present invention provides a column-mounted water-cooled shower-type feeding process for titanium tetrachloride, comprising the following steps:

[0006] S1. Add liquid magnesium to the reactor to the set amount, and the temperature of each zone of the reduction furnace rises to the specified temperature;

[0007] S2. After the temperature reaches the set temperature, start the titanium tetrachloride feeding device and control the feeding rate and reactor pressure.

[0008] S3. Start the cooling device while starting the titanium tetrachloride feeding process, and control the inlet and outlet water flow rates.

[0009] S4. A baffle is installed above the outlet of titanium tetrachloride to ensure that titanium tetrachloride is sprayed downwards into the liquid magnesium for reaction.

[0010] S5. Two discharge ports are set at the bottom of the reactor. In order to ensure the smooth discharge, the amount of feed is calculated according to the reaction time and the feeding rate. After the amount of feed reaches the preset value, prepare the magnesium chloride lifting bag, start the discharge system, and pre-discharge 50kg. Check the discharge situation. After the discharge is normal, continue to discharge until the reaction is over.

[0011] S6. After the reduction is completed, proceed to the distillation section.

[0012] Preferably, in step S1, the amount of liquid magnesium is set to 10-18t, and the specified temperature for each zone of the reduction furnace is 800-900℃.

[0013] Preferably, in step S2, the reactor pressure is controlled at 10-30 kPa, and the feeding rate is set to 300-600 kg / h.

[0014] Preferably, in step S3, the influent and effluent flow rates are 50-100 m³ / h.

[0015] Preferably, in step S4, the height of the baffle from the reactor cover is controlled at 30-50cm.

[0016] Preferably, a pipe is provided at the center of the reactor, and a titanium tetrachloride inlet is provided at the bottom end of the pipe. The bottom end of the titanium tetrachloride inlet is connected to the feeding end of a titanium tetrachloride feeding device, which is a screw feeder.

[0017] Preferably, a hollow column is provided outside the central pipe of the reactor, and an inlet and an outlet are provided at the bottom of the hollow column. The inlet and outlet are respectively connected to the inlet and outlet of the cooling device.

[0018] Preferably, the reactor is provided with a vertical first discharge pipe and a second discharge pipe on both sides, and the bottom ends of the first discharge pipe and the second discharge pipe are connected to the bottom discharge port of the reactor.

[0019] Preferably, the upper part of the central pipe of the reactor is the discharge port, the baffle is located above the discharge port, the distance between the baffle and the discharge port is 20cm, and the outer shell of the baffle is a frustum-shaped structure with a sealed top and an open bottom.

[0020] Preferably, in step S5, the result of multiplying the reaction time by the feeding rate is the feeding amount a, and the preset value b is 4 / 5 of the reactor's maximum capacity. When the feeding amount a reaches 4 / 5 of the reactor's maximum capacity, the discharge system is started. The discharge system uses a sewage pump, and the input end of the sewage pump is connected to the outer end of the first discharge pipe and the second discharge pipe.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0022] 1. In the production process of titanium tetrachloride column water-cooled shower head feeding, the reactor is modified to add a water-cooling structure for titanium tetrachloride, and cooling water is connected to cool the titanium tetrachloride pipeline, thereby reducing the overall reaction temperature. Moreover, the titanium agglomerate produced by this process avoids the hard core caused by central overheating.

[0023] 2. In this column-cooled spray-type feeding process for titanium tetrachloride, a baffle is installed above the titanium tetrachloride outlet to ensure that the titanium tetrachloride is sprayed into the liquid magnesium, resulting in a more uniform reaction and ensuring product quality. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the overall structure of the reactor in this invention.

[0025] The meanings of the labels in the diagram are as follows:

[0026] 1. Reactor; 2. First discharge pipe; 3. Outlet; 4. Inlet; 5. Titanium tetrachloride inlet; 6. Second discharge pipe; 7. Baffle. Detailed Implementation

[0027] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example

[0028] This invention provides a column-mounted water-cooled shower-style feeding process for titanium tetrachloride, such as... Figure 1 As shown, it includes the following steps:

[0029] S1. Add liquid magnesium to reactor 1 to the set amount, and the temperature of each zone of the reduction furnace rises to the specified temperature.

[0030] S2. After the temperature reaches the set temperature, start the titanium tetrachloride feeding device and control the feeding rate and the pressure of reactor 1.

[0031] S3. Start the cooling device while starting the titanium tetrachloride feeding process, and control the inlet and outlet water flow rates.

[0032] S4. A baffle 7 is installed above the outlet of titanium tetrachloride to ensure that titanium tetrachloride is sprayed downwards into the liquid magnesium for reaction.

[0033] S5. Two discharge ports are set at the bottom of reactor 1. In order to ensure the smooth discharge, the amount of feed is calculated according to the reaction time and the feeding rate. After the amount of feed reaches the preset value, prepare the magnesium chloride lifting bag, start the discharge system, and pre-discharge 50kg. Check the discharge situation. After the discharge is normal, continue to discharge until the reaction is over.

[0034] S6. After the reduction is completed, proceed to the distillation section.

[0035] In this embodiment, in step S1, the set amount of liquid magnesium is 10t, and the specified temperature of each zone of the reduction furnace is 800℃.

[0036] Specifically, in step S2, the pressure of reactor 1 is controlled at 10 kPa, and the feeding rate is set to 300 kg / h.

[0037] Furthermore, in step S3, the influent and effluent flow rates are 50 m³ / h.

[0038] Furthermore, in step S4, the height of the baffle 7 from the cover of reactor 1 is controlled at 30cm.

[0039] Furthermore, a pipe is installed at the center of reactor 1, and a titanium tetrachloride inlet 5 is installed at the bottom end of the pipe. The bottom end of the titanium tetrachloride inlet 5 is connected to the feeding end of the titanium tetrachloride feeding device, which is a screw feeder, to facilitate stable feeding operations.

[0040] Furthermore, a hollow column is installed outside the central pipe of reactor 1. The bottom of the hollow column is provided with an inlet 4 and an outlet 3. The inlet 4 and the outlet 3 are respectively connected to the inlet and outlet of the cooling device. The cooling device is a water cooling system that is already available in the art. Through the external water cooling system, cold water enters the hollow column from the inlet 4 to quickly cool down the central pipe of reactor 1. Then, hot water is discharged from the outlet 3 to achieve circulating cooling of reactor 1.

[0041] Furthermore, vertical first discharge pipe 2 and second discharge pipe 6 are provided on both sides of reactor 1. The bottom ends of the first discharge pipe 2 and the second discharge pipe 6 are connected to the bottom discharge port of reactor 1 to facilitate discharge operation.

[0042] Furthermore, the upper part of the central pipe of reactor 1 is the discharge port, and the baffle 7 is located above the discharge port, 20cm away from the discharge port. The outer shell of the baffle 7 is a frustum-shaped structure with a sealed top and an open bottom. The baffle 7 blocks the material after it is discharged, and it is evenly distributed inside the reactor 1 in a sprinkled manner, which facilitates the full and uniform reaction.

[0043] Furthermore, in step S5, the result of multiplying the reaction time by the feeding rate is the feeding amount a, and the preset value b is 4 / 5 of the maximum capacity of reactor 1. When the feeding amount a reaches 4 / 5 of the maximum capacity of reactor 1, the discharge system is started. The discharge system uses a sewage pump, and the input end of the sewage pump is connected to the outer end of the first discharge pipe 2 and the second discharge pipe 6, so as to facilitate timely discharge operation. Example

[0044] This invention also provides a production process for titanium tetrachloride column water-cooled shower head type feeding, such as... Figure 1 As shown, it includes the following steps:

[0045] S1. Add liquid magnesium to reactor 1 to the set amount, and the temperature of each zone of the reduction furnace rises to the specified temperature.

[0046] S2. After the temperature reaches the set temperature, start the titanium tetrachloride feeding device and control the feeding rate and the pressure of reactor 1.

[0047] S3. Start the cooling device while starting the titanium tetrachloride feeding process, and control the inlet and outlet water flow rates.

[0048] S4. A baffle 7 is installed above the outlet of titanium tetrachloride to ensure that titanium tetrachloride is sprayed downwards into the liquid magnesium for reaction.

[0049] S5. Two discharge ports are set at the bottom of reactor 1. In order to ensure the smooth discharge, the amount of feed is calculated according to the reaction time and the feeding rate. After the amount of feed reaches the preset value, prepare the magnesium chloride lifting bag, start the discharge system, and pre-discharge 50kg. Check the discharge situation. After the discharge is normal, continue to discharge until the reaction is over.

[0050] S6. After the reduction is completed, proceed to the distillation section.

[0051] In this embodiment, in step S1, the set amount of liquid magnesium is 15t, and the specified temperature of each zone of the reduction furnace is 850℃.

[0052] Specifically, in step S2, the pressure of reactor 1 is controlled at 20 kPa, and the feeding rate is set to 450 kg / h.

[0053] Furthermore, in step S3, the influent and effluent flow rates are 80 m³ / h.

[0054] Furthermore, in step S4, the height of the baffle 7 from the cover of the reactor 1 is controlled at 40cm.

[0055] Furthermore, a pipe is installed at the center of reactor 1, and a titanium tetrachloride inlet 5 is installed at the bottom end of the pipe. The bottom end of the titanium tetrachloride inlet 5 is connected to the feeding end of the titanium tetrachloride feeding device, which is a screw feeder, to facilitate stable feeding operations.

[0056] Furthermore, a hollow column is installed outside the central pipe of reactor 1. The bottom of the hollow column is provided with an inlet 4 and an outlet 3. The inlet 4 and the outlet 3 are respectively connected to the inlet and outlet of the cooling device. The cooling device is a water cooling system that is already available in the art. Through the external water cooling system, cold water enters the hollow column from the inlet 4 to quickly cool down the central pipe of reactor 1. Then, hot water is discharged from the outlet 3 to achieve circulating cooling of reactor 1.

[0057] Furthermore, vertical first discharge pipe 2 and second discharge pipe 6 are provided on both sides of reactor 1. The bottom ends of the first discharge pipe 2 and the second discharge pipe 6 are connected to the bottom discharge port of reactor 1 to facilitate discharge operation.

[0058] Furthermore, the upper part of the central pipe of reactor 1 is the discharge port, and the baffle 7 is located above the discharge port, 20cm away from the discharge port. The outer shell of the baffle 7 is a frustum-shaped structure with a sealed top and an open bottom. The baffle 7 blocks the material after it is discharged, and it is evenly distributed inside the reactor 1 in a sprinkled manner, which facilitates the full and uniform reaction.

[0059] Furthermore, in step S5, the result of multiplying the reaction time by the feeding rate is the feeding amount a, and the preset value b is 4 / 5 of the maximum capacity of reactor 1. When the feeding amount a reaches 4 / 5 of the maximum capacity of reactor 1, the discharge system is started. The discharge system uses a sewage pump, and the input end of the sewage pump is connected to the outer end of the first discharge pipe 2 and the second discharge pipe 6, so as to facilitate timely discharge operation. Example

[0060] This invention also provides a production process for titanium tetrachloride column water-cooled shower head type feeding, such as... Figure 1 As shown, it includes the following steps:

[0061] S1. Add liquid magnesium to reactor 1 to the set amount, and the temperature of each zone of the reduction furnace rises to the specified temperature.

[0062] S2. After the temperature reaches the set temperature, start the titanium tetrachloride feeding device and control the feeding rate and the pressure of reactor 1.

[0063] S3. Start the cooling device while starting the titanium tetrachloride feeding process, and control the inlet and outlet water flow rates.

[0064] S4. A baffle 7 is installed above the outlet of titanium tetrachloride to ensure that titanium tetrachloride is sprayed downwards into the liquid magnesium for reaction.

[0065] S5. Two discharge ports are set at the bottom of reactor 1. In order to ensure the smooth discharge, the amount of feed is calculated according to the reaction time and the feeding rate. After the amount of feed reaches the preset value, prepare the magnesium chloride lifting bag, start the discharge system, and pre-discharge 50kg. Check the discharge situation. After the discharge is normal, continue to discharge until the reaction is over.

[0066] S6. After the reduction is completed, proceed to the distillation section.

[0067] In this embodiment, in step S1, the set amount of liquid magnesium is 18t, and the specified temperature of each zone of the reduction furnace is 900℃.

[0068] Specifically, in step S2, the pressure of reactor 1 is controlled at 30 kPa, and the feeding rate is set to 600 kg / h.

[0069] Furthermore, in step S3, the influent and effluent flow rates are 100 m³ / h.

[0070] Furthermore, in step S4, the height of the baffle 7 from the cover of reactor 1 is controlled at 50cm.

[0071] Furthermore, a pipe is installed at the center of reactor 1, and a titanium tetrachloride inlet 5 is installed at the bottom end of the pipe. The bottom end of the titanium tetrachloride inlet 5 is connected to the feeding end of the titanium tetrachloride feeding device, which is a screw feeder, to facilitate stable feeding operations.

[0072] Furthermore, a hollow column is installed outside the central pipe of reactor 1. The bottom of the hollow column is provided with an inlet 4 and an outlet 3. The inlet 4 and the outlet 3 are respectively connected to the inlet and outlet of the cooling device. The cooling device is a water cooling system that is already available in the art. Through the external water cooling system, cold water enters the hollow column from the inlet 4 to quickly cool down the central pipe of reactor 1. Then, hot water is discharged from the outlet 3 to achieve circulating cooling of reactor 1.

[0073] Furthermore, vertical first discharge pipe 2 and second discharge pipe 6 are provided on both sides of reactor 1. The bottom ends of the first discharge pipe 2 and the second discharge pipe 6 are connected to the bottom discharge port of reactor 1 to facilitate discharge operation.

[0074] Furthermore, the upper part of the central pipe of reactor 1 is the discharge port, and the baffle 7 is located above the discharge port, 20cm away from the discharge port. The outer shell of the baffle 7 is a frustum-shaped structure with a sealed top and an open bottom. The baffle 7 blocks the material after it is discharged, and it is evenly distributed inside the reactor 1 in a sprinkled manner, which facilitates the full and uniform reaction.

[0075] Furthermore, in step S5, the result of multiplying the reaction time by the feeding rate is the feeding amount a, and the preset value b is 4 / 5 of the maximum capacity of reactor 1. When the feeding amount a reaches 4 / 5 of the maximum capacity of reactor 1, the discharge system is started. The discharge system uses a sewage pump, and the input end of the sewage pump is connected to the outer end of the first discharge pipe 2 and the second discharge pipe 6, so as to facilitate timely discharge operation.

[0076] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A column-mounted water-cooled shower-type feeding process for titanium tetrachloride, characterized in that: Includes the following steps: S1. Add liquid magnesium to reactor (1) to the set amount, and raise the temperature of each zone of the reduction furnace to the specified temperature; S2. After the temperature reaches the set temperature, turn on the titanium tetrachloride feeding device and control the feeding speed and reactor (1) pressure. S3. Start the cooling device while starting the titanium tetrachloride feeding process, and control the inlet and outlet water flow rates. S4. A baffle (7) is installed above the outlet of titanium tetrachloride to ensure that titanium tetrachloride is sprayed downwards into the liquid magnesium for reaction; S5. Two discharge ports are set at the bottom of the reactor (1). In order to ensure the smooth discharge, the amount of feed is calculated according to the reaction time and the feeding rate. After the amount of feed reaches the preset value, prepare the magnesium chloride lifting bag, start the discharge system, and pre-discharge 50kg. Check the discharge situation. After the discharge is normal, continue to discharge until the reaction is over. S6. After reduction is complete, proceed to the distillation section; A pipe is provided at the center of the reactor (1), and a titanium tetrachloride inlet (5) is provided at the bottom end of the pipe. The bottom end of the titanium tetrachloride inlet (5) is connected to the feeding end of the titanium tetrachloride feeding device, which is a screw feeder. A hollow column is provided outside the central pipe of the reactor (1). The bottom end of the hollow column is provided with an inlet (4) and an outlet (3). The inlet (4) and the outlet (3) are respectively connected to the inlet and outlet ends of the cooling device. The upper part of the central pipe of the reactor (1) is the discharge port, the baffle (7) is located above the discharge port, and the distance between the baffle (7) and the discharge port is 20cm. The outer shell of the baffle (7) is a frustum-shaped structure with a sealed top and an open bottom.

2. The titanium tetrachloride column water-cooled shower-type feeding production process according to claim 1, characterized in that: In step S1, the set amount of liquid magnesium is 10-18t, and the specified temperature for each zone of the reduction furnace is 800-900℃.

3. The titanium tetrachloride column water-cooled shower-type feeding production process according to claim 1, characterized in that: In step S2, the pressure of reactor (1) is controlled at 10-30 kPa, and the feeding rate is set to 300-600 kg / h.

4. The titanium tetrachloride column water-cooled shower-type feeding production process according to claim 1, characterized in that: In step S3, the influent and effluent flow rates are 50-100 m³ / h. 3 / h.

5. The titanium tetrachloride column water-cooled shower-type feeding production process according to claim 1, characterized in that: In step S4, the height of the baffle (7) from the cover of the reactor (1) is controlled at 30-50cm.

6. The titanium tetrachloride column water-cooled shower-type feeding production process according to claim 1, characterized in that: The reactor (1) is provided with a vertical first discharge pipe (2) and a second discharge pipe (6) on both sides. The bottom ends of the first discharge pipe (2) and the second discharge pipe (6) are connected to the bottom discharge port of the reactor (1).

7. The titanium tetrachloride column water-cooled shower-type feeding production process according to claim 6, characterized in that: In step S5, the reaction time multiplied by the feeding rate is the feeding amount a. The preset value b is 4 / 5 of the maximum capacity of reactor (1). When the feeding amount a reaches 4 / 5 of the maximum capacity of reactor (1), the discharge system is turned on. The discharge system uses a sewage pump. The input end of the sewage pump is connected to the outer end of the first discharge pipe (2) and the second discharge pipe (6).

Images