Device for rapidly purifying titanium tetrachloride in laboratory
Titanium tetrachloride was rapidly purified by using a reactor heating and cooling device in the laboratory, combined with packing materials such as copper mesh, nickel mesh, or activated zeolite, thus solving the purity problem and achieving the preparation of high-purity products.
Patent Information
- Application Number
- CN202520286333.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-21
- Publication Date
- 2025-12-23
- Estimated Expiration
- 2035-02-21
AI Technical Summary
The purity of titanium tetrachloride in the laboratory affects the synthesis process of catalysts and precursors. Existing technologies are difficult to purify quickly and effectively, resulting in substandard products.
A combination of reactor heating and cooling devices is used, with copper mesh, nickel mesh, activated zeolite, or activated molecular sieve as packing material. Titanium tetrachloride is purified by heating to 120°C and cooling to 30°C, achieving rapid purification.
The purity of titanium tetrachloride was increased to over 4N, and impurities such as Fe and V were reduced to below 1ppm, meeting the synthesis requirements. The product can be directly used for subsequent applications.
Smart Images
Figure CN223697724U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to the technical field of chemical purification, and particularly relates to a device for rapidly purifying titanium tetrachloride in a laboratory. BACKGROUND
[0002] TiCl4, the Chinese name titanium tetrachloride, is an important intermediate for producing metal titanium and its compounds, is the main raw material for producing sponge titanium and chlorination titanium dioxide, can be applied in the semiconductor industry, metal titanium deposition and the raw material for preparing titanium-based metal precursors, and belongs to a new market material.
[0003] Titanium tetrachloride is often produced from the chlorination reaction of titanium ore, solid suspended matter is removed by using a sedimentation filtration method, and further, silicon, aluminum, iron, vanadium and other chlorides dissolved in titanium tetrachloride are removed by using a distillation-rectification method and a chemical method. Commercially available titanium tetrachloride has a purity of about 98% to 99%, and the color is often yellow, which indicates that there is a lot of VOCl3 or VCl4 in the titanium tetrachloride, so that the titanium tetrachloride has a certain color. In the laboratory, because the titanium tetrachloride has strong corrosiveness, and reacts to generate titanium dioxide solid and hydrochloric acid droplets when encountering moisture, the purity of the titanium tetrachloride is a big problem when the titanium tetrachloride is used in the laboratory to prepare a titanium-based catalyst or synthesize a semiconductor titanium-based precursor, which affects the catalyst or the precursor synthesis process, and a quick method for treating the titanium tetrachloride raw material is urgently needed.
[0004] Therefore, in view of the above technical problems, it is necessary to provide a device for rapidly purifying titanium tetrachloride in a laboratory.
[0005] The information disclosed in this BACKGROUND section is only intended to increase an understanding of the general background of the present utility model and should not be taken as an acknowledgement or any form of suggestion that this information forms prior art that is already known to those of ordinary skill in the art. CONTENT OF THE UTILITY MODEL
[0006] The utility model aims to provide a device for rapidly purifying titanium tetrachloride in a laboratory, which can.
[0007] In order to achieve the above-mentioned purpose, the technical scheme provided by a specific embodiment of the utility model is as follows:
[0008] The device for rapidly purifying titanium tetrachloride in a laboratory comprises a reactor with a reaction cavity, a heating device and a cooling device;
[0009] One end of the reaction cavity of the reactor is provided with a titanium tetrachloride raw material inlet, and the other end is provided with a titanium tetrachloride product outlet; at least part of the area in the reaction cavity is formed into a packing filling area; the reaction cavity from the titanium tetrachloride raw material inlet to the titanium tetrachloride product outlet is filled with the packing filling area at least in the full section;
[0010] The heating device is arranged at least outside the reactor to provide a proper reaction temperature environment for the titanium tetrachloride raw material in the filler filling area in the reaction cavity;
[0011] The cooling device is arranged at least near the titanium tetrachloride product outlet to provide a temperature environment meeting the cooling of the titanium tetrachloride product.
[0012] In one or more embodiments of the present application, the filler is selected from copper mesh, nickel mesh, active zeolite and active molecular sieve.
[0013] In one or more embodiments of the present application, the copper mesh and / or nickel mesh satisfies that a porous mesh structure is obtained by piling and extruding or weaving fiber filaments of 0.01-1 mm.
[0014] In one or more embodiments of the present application, the particle size of the active zeolite and / or active molecular sieve in the filler satisfies 0.1-2 mm.
[0015] In one or more embodiments of the present application, when the filler is active zeolite or active molecular sieve, a mesh grid limiting the filler is further arranged at both ends of the filler filling area adjacent to the titanium tetrachloride raw material inlet and the titanium tetrachloride product outlet.
[0016] In one or more embodiments of the present application, the heating device is a jacket device formed outside the reaction cavity of the reactor, and the jacket device includes a sleeve body sleeved outside the reactor and a heat medium source connected to a heat medium inlet.
[0017] In one or more embodiments of the present application, the heat medium inlet is arranged on the sleeve body at one side adjacent to the titanium tetrachloride product outlet.
[0018] In one or more embodiments of the present application, the titanium tetrachloride raw material inlet is connected to a raw material supply device, and the raw material supply device includes a gas source device and a conveying pipe driven by the gas supplied by the gas source device, and the conveying pipe is connected to a titanium tetrachloride raw material storage device.
[0019] In one or more embodiments of the present application, a stirring device is further arranged in the reaction cavity of the reactor adjacent to the titanium tetrachloride product outlet.
[0020] In one or more embodiments of the present application, the reaction cavity of the reactor adjacent to the titanium tetrachloride raw material inlet is further connected with a discharge port.
[0021] In one or more embodiments of the present application, the reaction cavity of the reactor is further connected with a liquid level meter.
[0022] Compared with existing technologies, the device for rapid purification of titanium tetrachloride in the laboratory of this invention can purify commercially available titanium tetrachloride raw materials into products with 4N or higher that meet the synthesis indicators through a simple method. Impurities such as Fe and V can be reduced to below 1 ppm. At the same time, the product can be directly filled into precursor cylinders for subsequent use. Attached Figure Description
[0023] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0024] Figure 1 This is a schematic diagram of the apparatus for rapid laboratory purification of titanium tetrachloride in one embodiment of the present invention. Detailed Implementation
[0025] To enable those skilled in the art to better understand the technical solutions of this utility model, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort should fall within the protection scope of this utility model.
[0026] like Figure 1 As shown in the figure, the apparatus for rapid laboratory purification of titanium tetrachloride in one embodiment of this utility model employs a reactor with an integrated design for heating, reaction, and collection. Liquid titanium tetrachloride is fed into the reactor via a nitrogen gas supply through a delivery pipe. After adsorption reaction, the product is condensed by a condenser in a cooling device. The reactor's reaction chamber is appropriately filled with copper or nickel wire mesh, activated zeolite, or activated molecular sieve packing materials to react with highly oxidizing ions such as vanadium. To meet reaction requirements, the reactor has a heating function in at least the packing area, ensuring the reaction temperature can reach above 120°C. The purified product from the reactor is cooled to 30°C and collected by an external cooling water system.
[0027] like Figure 1As shown, in particular, the device for rapid purification of titanium tetrachloride in the laboratory in an embodiment of the utility model, including the reactor 1 with the reaction cavity, heating device 2 and cooling device 3, the reaction cavity one end of reactor 1 is provided with titanium tetrachloride raw material import 12, the conveying pipe connected to it is under the power of nitrogen pressure and sends titanium tetrachloride raw material to the reaction cavity, and the other end is provided with titanium tetrachloride product export, and the reaction cavity is formed with the packing filling area 11 in at least partial area, wherein the 0.2mm copper fiber silk is filled in the 1mm aperture porous mesh structure obtained by warp knitting, and the thickness of the staggered stack that is tightly contacted to the inner wall is 5cm, the jacket device 2 that is connected to the heat medium import 21 with the heat oil supply pump as the heat source is set to the outside of reactor, to heat the titanium tetrachloride raw material of the packing filling area in the reaction cavity to 120 DEG C, and the heat oil after heat exchange is excluded jacket device 2 from the heat medium export 22, and the liquid is continuously stirred in the reaction process with stirring paddle, and the center tube of water cooling coil cooler connected to cooling water is connected to titanium tetrachloride product export and provides 30 DEG C cooling environment, and the product after purification is condensed to form.
[0028] In addition, the reaction cavity of reactor 1 adjacent to titanium tetrachloride raw material import is also connected with discharge port 13, and nitrogen and the like are timely excluded.
[0029] In addition, further, in order to monitor the liquid inventory in the reaction cavity in real time, the reaction cavity of reactor is also connected with liquid level gauge, and maintenance alarm is triggered and operation is stopped when liquid level is too low or too high.
[0030] As above, the packing can also be replaced with any of the following situations equally: the packing is selected from: copper mesh, nickel mesh, active zeolite, active molecular sieve. Copper mesh and / or nickel mesh satisfy: the porous mesh structure obtained by stacking extrusion or weaving of 0.01-1mm fiber silk. The particle size of active zeolite and / or active molecular sieve in the packing satisfies: 0.1-2mm. When the packing is active zeolite or active molecular sieve, the packing filling area is also provided with a mesh grid limiting the packing at both ends adjacent to titanium tetrachloride raw material import and titanium tetrachloride product export.
[0031] It is obvious for those skilled in the art that the utility model is not limited to the details of the above-mentioned exemplary embodiments, and the utility model can be realized in other specific forms without departing from the spirit or basic characteristics of the utility model. Therefore, no matter from which point, the embodiments should be regarded as exemplary and non-limiting, the scope of the utility model is defined by the appended claims instead of the above description, and therefore all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the utility model. Any figure mark in the claims should not be regarded as limiting the involved claims.
[0032] Furthermore, it should be understood that although the specification is described in terms of embodiments, not every embodiment includes every feature described. The specification can include implicit combinations of explicitly mentioned features and / or explicit combinations of implicitely mentioned features. Each embodiment depends on the explicit combinations of features and / or the implicit combinations of features made specifically within that embodiment, and each such embodiment can be combined with every other such embodiment to create further embodiments.
Claims
1. A device for rapid purification of titanium tetrachloride in a laboratory, characterized in that, The reactor comprises a reaction chamber, a heating device and a cooling device; The reaction chamber of the reactor is provided with a titanium tetrachloride raw material inlet at one end and a titanium tetrachloride product outlet at the other end, and at least part of the reaction chamber is filled with a packing filling area; the packing filling area at least fills part of the cross section from the titanium tetrachloride raw material inlet to the titanium tetrachloride product outlet; The heating device is arranged at least outside the reactor to provide a proper reaction temperature environment for the titanium tetrachloride raw material in the packing filling area of the reaction chamber; The cooling device is arranged at least near the titanium tetrachloride product outlet to provide a temperature environment suitable for cooling the titanium tetrachloride product.
2. The device for rapid purification of titanium tetrachloride in the laboratory according to claim 1, characterized by the fact that, The packing is selected from copper mesh, nickel mesh, active zeolite and active molecular sieve.
3. The device for rapid purification of titanium tetrachloride in the laboratory according to claim 2, characterized by the fact that, The copper mesh and / or nickel mesh is a porous mesh structure obtained by stacking and extruding or weaving fiber filaments of 0.01-1mm.
4. The device for rapid purification of titanium tetrachloride in the laboratory according to claim 2, characterized by the fact that, The particle size of the active zeolite and / or active molecular sieve in the packing satisfies 0.1-2mm.
5. The device for rapid laboratory purification of titanium tetrachloride according to claim 4, characterized by the fact that, When the packing is active zeolite or active molecular sieve, the packing filling area is further provided with a mesh grid for limiting the packing at both ends adjacent to the titanium tetrachloride raw material inlet and the titanium tetrachloride product outlet.
6. The device for rapid purification of titanium tetrachloride in the laboratory according to claim 1, characterized by the fact that, The heating device is a jacket device formed outside the reaction chamber of the reactor, which comprises a jacket body arranged outside the reactor and a heat medium source connected to a heat medium inlet.
7. The device for rapid laboratory purification of titanium tetrachloride according to claim 6, characterized by the fact that, The heat medium inlet is arranged on the jacket body adjacent to one side of the titanium tetrachloride product outlet.
8. The device for rapid purification of titanium tetrachloride in the laboratory according to claim 1, characterized by the fact that, The titanium tetrachloride raw material inlet is connected to a raw material supply device, which comprises a gas source device and a conveying pipe driven by the gas supplied by the gas source device, and the conveying pipe is connected to a titanium tetrachloride raw material storage device.
9. The device for rapid purification of titanium tetrachloride in the laboratory according to claim 1, characterized by the fact that, The reaction chamber of the reactor is further connected with a liquid level meter.