Titanium tetrachloride rectification device

Abstract

The utility model belongs to the technical field of material separation, and particularly relates to a titanium tetrachloride rectifying device which comprises a reaction kettle and a rectifying tower, the kettle top of the reaction kettle is connected with the tower bottom of the rectifying tower through a gaseous mixture discharging pipeline, copper filler is filled in the rectifying tower, the copper filler is random filler or regular filler, and the reactor top of the reaction kettle is connected with the tower bottom of the rectifying tower through a gaseous mixture discharging pipeline. The reaction kettle is connected with a heating mechanism, and the rectifying tower is connected with a condensation reflux mechanism. According to the utility model, the copper filler is used as the built-in filler of the rectifying tower, VOC (Volatile Organic Compounds) l3 can directly react with the copper filler to generate a substance which is not dissolved in Ti C l4, so that the aim of removing impurities is fulfilled; impurity separation can be achieved without increasing the number of theoretical plates of a rectifying tower and the reflux ratio, the VOC l < 3 > impurity can be removed more simply, and meanwhile the equipment investment cost and the operation energy consumption are greatly reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to a titanium tetrachloride rectification device belongs to material separation technical field. BACKGROUND

[0002] Titanium tetrachloride is an important intermediate for producing metal titanium and its compounds, and is the main raw material for producing titanium sponge and titanium dioxide. The purity of TiCl4 is required to be high in industry, and the impurity content directly affects the quality of the subsequent products titanium sponge or titanium dioxide. The purity of TiCl4 is generally required to be TiCl4>99.99%, SiCl4<0.0005%, FeCl3<0.0005%, VOCl3<0.0003%, and the appearance is colorless transparent liquid.

[0003] The impurities of titanium tetrachloride are complex, including dissolved gas impurities (O2, N2, Cl2, HCl, COCl2, CO2), dissolved liquid impurities (CCl4, VOCl3, SiCl4, SnCl2, SOCl2), dissolved solid impurities (AlCl3, FeCl3, NbCl5, TaCl5, MoCl5), and insoluble suspended solid impurities (TiO2, SiO2, MgCl2, ZrCl4, FeCl2, MnCl2, CrCl3).

[0004] The first type of gas impurities is removed with the increase of temperature in the treatment process, the fourth type of insoluble suspended impurities can be removed by solid-liquid separation, and the second type and the third type of impurities are dissolved in TiCl4 and can be removed according to their different boiling points. According to their boiling points, the second type of impurities and the third type of impurities can be divided into high-boiling-point impurities, low-boiling-point impurities and impurities with boiling points close to TiCl4, and the representative components of the three types are FeCl3, SiCl4 and VOCl3 respectively.

[0005] SiCl4 (boiling point 58℃) and FeCl3 (boiling point 318℃) in TiCl4 are low-boiling-point impurities and high-boiling-point impurities respectively, and their boiling points are quite different from that of TiCl4 (boiling point 136℃), so they can be separated by rectification and controlled to very low impurity content. The boiling point of VOCl3 is 127℃, which is close to that of TiCl4, so it is difficult to separate from TiCl4. At present, the method of increasing the theoretical plate number of the rectification tower and the operation reflux ratio is usually used to separate and purify VOCl3 from TiCl4, but this method will cause the height of the rectification tower to be too high and the operation energy consumption to be too large, resulting in high equipment investment cost and operation cost, more residual VOCl3 and poor quality of TiCl4. SUMMARY

[0006] The utility model provides a titanium tetrachloride rectification device aiming at the defects of prior art.

[0007] The technical scheme for solving the above technical problems is as follows: a titanium tetrachloride rectification device, comprising a reaction kettle and a rectification tower, a kettle top of the reaction kettle is connected with a tower bottom of the rectification tower through a gaseous mixture discharge pipeline, copper filler is filled in the rectification tower, the copper filler is loose filler or structured filler, the reaction kettle is connected with a heating mechanism, and the rectification tower is connected with a condensation reflux mechanism.

[0008] The utility model discloses the beneficial effect lies in: the utility model discloses copper filler as the built -in filler of rectification tower, in the rectification process, the VOCI3 on the surface of filler can directly react with copper filler, generates the substance that is insoluble in TiCl4, reaches the purpose of removing impurity, copper filler is structured filler or loose filler, and VOCI3 reaction generates VOCI2 and is not easy to adhere on the surface of filler, or the adhesion amount is big after easy peeling, therefore, do not need to change filler frequently, reduce the personnel operation intensity, the utility model discloses the separation of low boiling point material, high boiling point material and the component VOCI3 of the similar boiling point can be more simply removed VOCI3 impurity, and the equipment investment cost and operating energy consumption are greatly reduced.

[0009] Further, the heating mechanism includes at least one reboiler, the kettle side liquid outlet pipeline is arranged on the side surface of the tower bottom of the reaction kettle, the kettle side liquid outlet pipeline is connected to the bottom of the reboiler, and the top of the reboiler is connected to the top of the reaction kettle through a gas-liquid mixture input pipeline.

[0010] The beneficial effect of the above further technical scheme is that the material is stirred and mixed by the reaction kettle. When the distillation is in the later stage, the material is relatively viscous, the reaction kettle bottom is used for depositing viscous material, the kettle side opening is arranged on the side surface of the reaction kettle, the less viscous material enters the reboiler through the kettle side liquid outlet pipeline for forced circulation heating, the gas-liquid mixture after heating reenters the reaction kettle, the temperature in the reaction kettle is increased, and finally can be increased to 150 DEG C.

[0011] Further, the kettle bottom circulating pump is arranged on the kettle side liquid outlet pipeline.

[0012] Further, the condensation reflux mechanism includes a condenser and a reflux tank, the top of the rectification tower is connected to the gaseous inlet of the condenser through a tower top gaseous output pipeline, and the condensate outlet of the condenser is connected to the reflux tank through a condensate pipeline.

[0013] Further, the reflux tank is provided with a reflux liquid output pipeline at the bottom, and the reflux liquid output pipeline is connected to the top of the rectification tower through a tower top reflux pipeline.

[0014] The beneficial effect of adopting the further technical scheme is that the gaseous substance becomes liquid after being condensed by the condenser and then flows back to the rectifying tower, and the reflux liquid performs heat and mass transfer and reaction with the ascending gas on the surface of the copper filler.

[0015] Further, a reflux pump is arranged on the reflux liquid output pipeline, and the reflux liquid output pipeline is connected with the production pipeline.

[0016] Further, the bottom of the rectifying tower is connected with the top of the reaction kettle through a kettle side liquid outlet pipeline.

[0017] The beneficial effect of adopting the further technical scheme is that the high-boiling residual liquid at the bottom of the rectifying tower is refluxed to the reaction kettle through the kettle bottom liquid outlet pipeline and discharged from the kettle bottom of the reaction kettle.

[0018] Further, the kettle bottom of the reaction kettle is connected with a kettle bottom liquid outlet pipeline, and a kettle bottom production pump is arranged on the kettle bottom liquid outlet pipeline.

[0019] Further, the kettle top of the reaction kettle is connected with a mother liquid feeding pipeline.

[0020] Further, two reboilers are arranged, and the kettle side liquid outlet pipeline is connected with the two reboilers through two kettle bottom circulating pumps.

[0021] The beneficial effect of adopting the further technical scheme is that when the reboiler is easily blocked after multiple distillations, the two groups of reboilers can be switched to use the other one when one of the reboilers is faulty or blocked, so that the system operation is not affected. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 The utility model discloses a structure schematic view.

[0023] The reference signs are recorded as follows: 1, mother liquid feeding pipeline; 2, gaseous mixture discharge pipeline; 3, tower top gaseous output pipeline; 4, condensed liquid pipeline; 5, reflux liquid output pipeline; 6, tower top reflux pipeline; 7, production pipeline; 8, kettle side liquid outlet pipeline; 9, reaction kettle; 10, reboiler; 11, rectifying tower; 12, condenser; 13, gas-liquid mixture input pipeline; 14, reflux tank; 15, kettle bottom liquid outlet pipeline; 16, kettle bottom liquid outlet pipeline; 17, kettle bottom circulating pump; 18, reflux pump; 19, kettle bottom production pump. DETAILED DESCRIPTION

[0024] The principles and characteristics of the utility model are described below in combination with the drawings, and the examples are only used for explaining the utility model and are not used for limiting the range of the utility model.

[0025] Reference is made to Figure 1The titanium tetrachloride rectification device comprises a reaction kettle 9 and a rectification tower 11, the kettle top of the reaction kettle 9 is connected with the bottom of the rectification tower 11 through a gaseous mixture discharge pipeline 2, the rectification tower 11 is filled with copper packing, the copper packing is loose packing or regular packing, the reaction kettle 9 is connected with a heating mechanism, and the rectification tower 11 is connected with a condensation reflux mechanism.

[0026] The heating mechanism comprises a reboiler 10, the side of the kettle bottom of the reaction kettle 9 is provided with a kettle side liquid outlet pipeline 8, the kettle side liquid outlet pipeline 8 is connected to the bottom of the reboiler 10, the kettle side liquid outlet pipeline 8 is provided with a kettle bottom circulating pump 17, the top of the reboiler 10 is connected to the top of the reaction kettle 9 through a gas-liquid mixture input pipeline 13, the reboiler 10 is connected to a steam supply device through a low-pressure steam input pipeline and a low-pressure steam output pipeline, low-pressure steam is used to provide heat for the reboiler 10, the pressure of the low-pressure steam is ≤0.6 MPaG, and the temperature is ≥165 DEG C.

[0027] The condensation reflux mechanism comprises a condenser 12 and a reflux tank 14, the top of the rectification tower 11 is connected to the gaseous inlet of the condenser 12 through a tower top gaseous output pipeline 3, and the condensate outlet of the condenser 12 is connected to the reflux tank 14 through a condensate pipeline 4.

[0028] The bottom of the reflux tank 14 is provided with a reflux liquid output pipeline 5, the reflux liquid output pipeline 5 is connected to the top of the rectification tower 11 through a tower top reflux pipeline 6. The reflux liquid output pipeline 5 is provided with a reflux pump 18, and the reflux liquid output pipeline 5 is connected to a production pipeline 7.

[0029] The bottom of the rectification tower 11 is connected to the kettle top of the reaction kettle 9 through a tower bottom liquid outlet pipeline 15.

[0030] The bottom of the reaction kettle 9 is connected to a kettle bottom liquid outlet pipeline 16, and the kettle bottom liquid outlet pipeline 16 is provided with a kettle bottom production pump 19.

[0031] The kettle top of the reaction kettle 9 is connected with a mother liquor feeding pipeline 1, and the reaction kettle 9 is provided with a stirring mechanism.

[0032] The reboiler 10 is provided with two, the kettle side liquid outlet pipeline 8 is connected to the two reboilers 10 through two kettle bottom circulating pumps 17, one of the two reboilers 10 is a standby, and when the reboiler 10 is easily blocked after multiple rectifications, the other reboiler 10 can be switched to use.

[0033] The working process of the titanium tetrachloride rectification device is as follows:

[0034] I. The TiCl4 mother liquor (containing SiCl4, FeCl3, VOCl3 and other impurities) to be treated is conveyed into the reaction kettle 9 through the mother liquor feeding pipeline 1, the reaction kettle 9 is continuously stirred, and the materials are mixed;

[0035] II. In the reactor 9, the material enters the bottom circulating pump 17 through the side outlet pipeline 8, and then enters the reboiler 10. The low-pressure steam indirectly heats the material through the reboiler 10, and the material is partially vaporized and enters the top of the reactor 9 in the form of a gas-liquid mixture through the gas-liquid mixture input pipeline 13;

[0036] III. In the reactor 9, the gaseous mixture enters the rectifying column 11 through the gaseous mixture outlet pipeline 2. In the copper filler surface of the rectifying column 11, VOCI3 in the gaseous mixture reacts with copper to generate VOCl2 and adhere to the filler surface;

[0037] IV. The gaseous components at the top of the rectifying column 11 enter the condenser 12 through the top gaseous output pipeline 3. The condenser 12 is cooled by circulating water, and the gaseous components are condensed into liquid;

[0038] V. The condensed liquid enters the reflux tank 14 through the condensed liquid pipeline 4, and is refluxed and extracted through the reflux liquid output pipeline 5 and the reflux pump 18. Part of the reflux liquid enters the top of the rectifying column 11 through the top reflux pipeline 6 and continues to participate in separation and reaction in the filler. Another part of the reflux liquid is extracted through the extraction pipeline 7;

[0039] VI. After the rectification is completed, the residue at the bottom of the reactor 9 enters the bottom extraction pump 19 through the bottom liquid outlet pipeline 16 and is discharged to the outside of the system.

[0040] The rectifying column of the utility model is filled with copper loose filler or structured filler. The specific surface area of the filler is large, and the porosity is large. The utility model uses copper filler as a reducing agent to selectively reduce VOCI3 into VOCl2 and Cu2Cl2. Cu2Cl2 is a high-boiling component that is enriched at the bottom of the reactor. The generated VOCl2 is a solid material with a relatively high boiling point and insoluble in TiCl4. It can adhere to the surface of the copper filler, thereby separating from TiCl4. The reaction process equation is as follows:

[0041] VOCl3+Cu→VOCl2↓+0.5Cu2Cl2.

[0042] VOCl2 adheres to the surface of the filler and appears green. When there is too much material adhering to the surface of the filler, it will be disturbed by the rising gas phase or the descending liquid phase, and then it will fall off to the reactor, thereby avoiding clogging the filler.

[0043] In the embodiment, the theoretical plate number of the rectifying column is 10-50, the rectifying column is filled with a gas-liquid distributor, the rectifying column body, the reboiler, the condenser, and the reflux storage are made of 316L stainless steel, or other stainless steel metal materials.

[0044] The above rectification operation process is operated at normal pressure or slightly positive pressure to avoid water vapor in the air from entering the system and corroding the equipment by reacting with TiCl4.

[0045] The above rectification operation process is operated in a batch mode, and a component with a high light component content is first taken out in the early stage of rectification, the column bottom temperature is continuously increased, the light component content is continuously reduced, qualified products are taken out, and the heavy component content in the column bottom is continuously increased. Different content products are continuously taken out as the operation time changes, that is, low-boiling-point components are first removed in the early stage of rectification, qualified TiCl4 products are distilled out in the middle stage, and high-boiling still residues are obtained in the later stage. After the rectification operation is completed, the products are discharged from the bottom of the reaction kettle.

[0046] The above only describes preferred embodiments of the present application and is not intended to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A titanium tetrachloride rectification apparatus characterized by comprising: The application relates to a distillation device, which comprises a reaction kettle (9) and a rectifying tower (11), the kettle top of the reaction kettle (9) is connected with the tower bottom of the rectifying tower (11) through a gaseous mixture discharge pipeline (2), the rectifying tower (11) is filled with copper packing, the copper packing is loose packing or regular packing, the reaction kettle (9) is connected with a heating mechanism, and the rectifying tower (11) is connected with a condensation reflux mechanism.

2. The titanium tetrachloride rectification apparatus according to claim 1, characterized by The heating mechanism comprises at least one reboiler (10), the tower bottom side of the reaction kettle (9) is provided with a kettle side liquid discharge pipeline (8), the kettle side liquid discharge pipeline (8) is connected to the bottom of the reboiler (10), and the top of the reboiler (10) is connected to the top of the reaction kettle (9) through a gas-liquid mixture input pipeline (13).

3. The titanium tetrachloride rectification apparatus according to claim 2, wherein A kettle bottom circulating pump (17) is arranged on the kettle side liquid discharge pipeline (8).

4. The titanium tetrachloride rectification apparatus according to claim 3, characterized by The condensation reflux mechanism comprises a condenser (12) and a reflux tank (14), the tower top of the rectifying tower (11) is connected with the gaseous inlet of the condenser (12) through a tower top gaseous output pipeline (3), and the condensate outlet of the condenser (12) is connected with the reflux tank (14) through a condensate pipeline (4).

5. The titanium tetrachloride rectification apparatus according to claim 4, wherein The bottom of the reflux tank (14) is provided with a reflux liquid output pipeline (5), the reflux liquid output pipeline (5) is provided with a reflux pump (18), and the reflux liquid output pipeline (5) is connected with the tower top of the rectifying tower (11) through a tower top reflux pipeline (6).

6. The titanium tetrachloride rectification apparatus according to claim 5, wherein The reflux liquid output pipeline (5) is connected with a production pipeline (7).

7. The titanium tetrachloride rectification apparatus according to claim 6, wherein The tower bottom of the rectifying tower (11) is connected with the kettle top of the reaction kettle (9) through a tower bottom liquid discharge pipeline (15).

8. The titanium tetrachloride rectification apparatus according to claim 7, wherein The kettle bottom of the reaction kettle (9) is connected with a kettle bottom liquid discharge pipeline (16), and the kettle bottom liquid discharge pipeline (16) is provided with a kettle bottom production pump (19).

9. The titanium tetrachloride rectification apparatus according to claim 8, wherein The kettle top of the reaction kettle (9) is connected with a mother liquor feeding pipeline (1).

10. The titanium tetrachloride rectification apparatus according to claim 9, wherein The reboiler (10) is provided with two, and the kettle side liquid discharge pipeline (8) is connected with the two reboilers (10) through two kettle bottom circulating pumps (17) respectively.

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