CN109264776B - Method for removing impurity tin in crude titanium tetrachloride - Google Patents
Method for removing impurity tin in crude titanium tetrachloride Download PDFInfo
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- CN109264776B CN109264776B CN201811325189.6A CN201811325189A CN109264776B CN 109264776 B CN109264776 B CN 109264776B CN 201811325189 A CN201811325189 A CN 201811325189A CN 109264776 B CN109264776 B CN 109264776B
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
Abstract
The invention relates to a method for removing impurity tin in crude titanium tetrachloride, which comprises four steps of component detection, preparation of trivalent titanium slurry, vanadium removal, tin removal and the like. On one hand, the method has the advantages of standard process flow, simple and convenient operation, low implementation cost, relatively low material loss, energy consumption and pollution to the surrounding environment, and on the other hand, the method effectively overcomes the defects of narrowing the use range of raw materials, increasing the difficulty in selecting the raw materials and increasing the production cost of the titanium tetrachloride in the prior art.
Description
Technical Field
The invention relates to a method for removing impurity tin in crude titanium tetrachloride, belonging to the field of chemical metallurgy.
Background
The refined titanium tetrachloride is an important raw material for producing titanium dioxide and titanium sponge, and is prepared by chloridizing rutile, high titanium slag and other titanium-rich materials as raw materials into crude titanium tetrachloride, and condensing, refining and purifying the crude titanium tetrachloride into the refined titanium tetrachloride. The current national standards for refined titanium tetrachloride have strict requirements for impurity elements such as Fe, V, Si, Al and Sn, which exist in the form of chlorides in titanium tetrachloride. The purification of the crude titanium tetrachloride, which is the removal of the impurity element in the crude titanium tetrachloride, is mainly realized by rectification. The boiling point of titanium tetrachloride is 136 ℃, the boiling point of ferric chloride is 315 ℃, the boiling point of vanadium oxychloride is 127.2 ℃, the boiling point of silicon tetrachloride is 57 ℃, the boiling point of anhydrous aluminum chloride is 180.5 ℃ and the boiling point of tin tetrachloride is 114.1 ℃. Wherein, the boiling points of the vanadium oxychloride and the tin tetrachloride are close to that of the titanium tetrachloride.
The literature, "influence of shallow precipitation raw materials on metallurgical quality of titanium alloy" reports that the mass fraction of Sn detected by a certain batch of titanium plates with the thickness of 3mm in a certain factory during finished product inspection is 0.23%, and the mass fraction obviously higher than the standard requirement is less than or equal to 0.1%. The investigation shows that the lead is the reason of the unqualified tin content in the used raw material titanium tetrachloride. However, there are few reports on the patent documents on how to remove the tin content in titanium tetrachloride, and there is a document "shallow analysis of source of tin impurity in titanium sponge" which proposes that the tin content in titanium tetrachloride can be reduced by using a titanium-rich material product with a low tin content because no suitable refining technology is available, but this is undoubtedly to narrow the application range of the titanium-rich material, and increase the difficulty of selecting the titanium-rich material and the production cost of titanium tetrachloride. In another patent CN 104326505 a "a deep separation method for reducing tin content in titanium tetrachloride" mentioned that the boiling points of titanium tetrachloride and tin tetrachloride are different, and it is presumed that the volatility of tin tetrachloride is higher than that of titanium tetrachloride under the same pressure, so a rectifying tower is additionally added to separate the two substances. In actual production, the crude titanium tetrachloride produced by part of manufacturers has very low tin content which is higher than the national standard requirement but lower than 100ppm or even lower, and in this case, if a rectification method is used for separating two substances, a large amount of steam and electricity are consumed, and the production cost is increased.
Disclosure of Invention
The invention aims to overcome the defects and provide a method for removing tin impurity in crude titanium tetrachloride. The technical scheme adopted by the invention for solving the technical problems is as follows:
in order to realize the purpose, the invention is realized by the following technical scheme:
a method for removing impurity tin from crude titanium tetrachloride, comprising the steps of:
s1, component detection, namely selecting 3-10 groups of detection samples from the crude titanium tetrachloride products produced in the same batch, then respectively detecting the content of vanadium and tin in each detection sample, then respectively calculating the average value of the content of vanadium and tin in each detection sample, and taking the average value as the content value of vanadium and tin in the crude titanium tetrachloride products in the batch;
s2, preparing trivalent titanium slurry, mixing aluminum powder and refined titanium tetrachloride, enabling the mass of the aluminum powder to be 0.8% -1% of that of the refined titanium tetrachloride, then adding anhydrous aluminum chloride with the same mass as the aluminum powder, stirring at a constant speed, heating the mixture to 120-150 ℃ within 10-20 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, and preserving heat and carrying out condensation reflux operation for 10-20 minutes to obtain the trivalent titanium slurry; wherein the grain diameter of the aluminum powder is less than 0.08mm, and the Al content is more than or equal to 99 percent.
S3, removing vanadium, mixing the trivalent titanium slurry prepared in the step S2 and the crude titanium tetrachloride product in the step S1 in a ratio of 1: 1-2, uniformly stirring, heating the mixture to 120-150 ℃ within 10-20 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 5-15min, and obtaining the rectified titanium tetrachloride;
s4, removing tin, namely, mixing the trivalent titanium slurry prepared in the step S2 with the rectified titanium tetrachloride in the step S3 to obtain a mixture of 1: 1-4, stirring at constant speed, heating the mixture to 80-100 ℃ within 10-20 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, wherein the time of the heat preservation and the condensation reflux operation is 15-20min, and obtaining the finished product of the impurity-removed titanium tetrachloride.
Further, in the step S3, the mass ratio of the trivalent titanium slurry to the crude titanium tetrachloride is adjusted according to the vanadium content, and when the vanadium content is not less than 400ppm, the mass ratio is 1: 1; when the vanadium content is less than 400ppm, the mass ratio of 1:2 to less than or equal to 1: 1.
Further, in the step S4, the mass ratio of the trivalent titanium slurry to the refined titanium tetrachloride is adjusted according to the tin content, and when the tin content is not less than 400ppm, the mass ratio is 1: 1; when the tin content is less than or equal to 50ppm and less than 400ppm, the mass ratio of 1:4 is less than 1: 1; when the tin content is less than 50ppm, the mass ratio is 1: 4.
Further, the stirring speed in S2, S3 and S4 is 70-150 r/min.
On one hand, the method has the advantages of standard process flow, simple and convenient operation, low implementation cost, relatively low material loss, energy consumption and pollution to the surrounding environment, and on the other hand, the method effectively overcomes the defects of narrowing the use range of raw materials, increasing the difficulty in selecting the raw materials and increasing the production cost of the titanium tetrachloride in the prior art.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
Example 1
As shown in fig. 1, a method for removing tin impurity from crude titanium tetrachloride comprises the following steps:
s1, component detection, namely selecting 3 detection samples from the crude titanium tetrachloride products produced in the same batch, then respectively detecting the vanadium and tin contents in each detection sample, then respectively calculating the average value of the vanadium and tin contents of each detection sample, and taking the average value as the vanadium and tin content value of the crude titanium tetrachloride product in the batch;
s2, preparing trivalent titanium slurry, mixing aluminum powder and refined titanium tetrachloride, enabling the mass of the aluminum powder to be 0.8% of that of the refined titanium tetrachloride, then adding anhydrous aluminum chloride with the same mass as the aluminum powder, stirring at a constant speed, heating the mixture to 120 ℃ within 10 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, and preserving heat and carrying out condensation reflux operation for 10 minutes to obtain the trivalent titanium slurry;
s3, removing vanadium, mixing the trivalent titanium slurry prepared in the step S2 and the crude titanium tetrachloride product in the step S1 in a ratio of 1:1, mixing in proportion, stirring at constant speed, heating the mixture to 120 ℃ within 10 minutes, preserving heat, and simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 5min, so as to obtain the rectified titanium tetrachloride;
s4, removing tin, namely, mixing the trivalent titanium slurry prepared in the step S2 with the rectified titanium tetrachloride in the step S3 to obtain a mixture of 1:1, stirring at a constant speed, heating the mixture to 80 ℃ within 10 minutes, preserving heat, and simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 15min, thus obtaining the finished product of the impurity-removed titanium tetrachloride.
In this embodiment, in the step S3, the mass ratio of the trivalent titanium slurry to the crude titanium tetrachloride is adjusted according to the content of vanadium, and when the content of vanadium is not less than 400ppm, the mass ratio is 1: 1; when the vanadium content is less than 400ppm, the mass ratio of 1:2 to less than or equal to 1: 1.
In this embodiment, in the step S4, the mass ratio of the trivalent titanium slurry to the refined titanium tetrachloride is adjusted according to the tin content, and when the tin content is ≧ 400ppm, the mass ratio is 1: 1; when the tin content is less than or equal to 50ppm and less than 400ppm, the mass ratio of 1:4 is less than 1: 1; when the tin content is less than 50ppm, the mass ratio is 1: 4.
In this example, the stirring speeds in S2, S3 and S4 were all 70 rpm.
Example 2
As shown in fig. 1, a method for removing tin impurity from crude titanium tetrachloride comprises the following steps:
s1, component detection, namely selecting 10 groups of detection samples from the crude titanium tetrachloride products produced in the same batch, then respectively detecting the vanadium and tin contents in each detection sample, then respectively calculating the average value of the vanadium and tin contents of each detection sample, and taking the average value as the vanadium and tin content value of the crude titanium tetrachloride product in the batch;
s2, preparing trivalent titanium slurry, mixing aluminum powder and refined titanium tetrachloride, enabling the mass of the aluminum powder to be 1% of that of the refined titanium tetrachloride, then adding anhydrous aluminum chloride with the same mass as the aluminum powder, stirring at a constant speed, heating the mixture to 150 ℃ within 20 minutes, preserving heat, and simultaneously carrying out condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 20min, so as to obtain the trivalent titanium slurry;
s3, removing vanadium, mixing the trivalent titanium slurry prepared in the step S2 and the crude titanium tetrachloride product in the step S1 in a ratio of 1:2, mixing in proportion, stirring at a constant speed, heating the mixture to 150 ℃ within 20 minutes, preserving heat, and simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 15min, so as to obtain the rectified titanium tetrachloride;
s4, removing tin, namely, mixing the trivalent titanium slurry prepared in the step S2 with the rectified titanium tetrachloride in the step S3 to obtain a mixture of 1:4, mixing at a constant speed, heating the mixture to 100 ℃ within 20 minutes, preserving heat, and simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 20min, thus obtaining the finished product of the impurity-removed titanium tetrachloride.
In this embodiment, in the step S3, the mass ratio of the trivalent titanium slurry to the crude titanium tetrachloride is adjusted according to the content of vanadium, and when the content of vanadium is not less than 400ppm, the mass ratio is 1: 1; when the vanadium content is less than 400ppm, the mass ratio of 1:2 to less than or equal to 1: 1.
In this embodiment, in the step S4, the mass ratio of the trivalent titanium slurry to the refined titanium tetrachloride is adjusted according to the tin content, and when the tin content is ≧ 400ppm, the mass ratio is 1: 1; when the tin content is less than or equal to 50ppm and less than 400ppm, the mass ratio of 1:4 is less than 1: 1; when the tin content is less than 50ppm, the mass ratio is 1: 4.
In this example, the stirring speeds in S2, S3 and S4 were all 150 rpm.
Example 3
As shown in fig. 1, a method for removing tin impurity from crude titanium tetrachloride comprises the following steps:
s1, component detection, namely selecting 5 groups of detection samples from the crude titanium tetrachloride products produced in the same batch, then respectively detecting the vanadium and tin contents in each detection sample, then respectively calculating the average value of the vanadium and tin contents of each detection sample, and taking the average value as the vanadium and tin content value of the crude titanium tetrachloride product in the batch;
s2, preparing trivalent titanium slurry, mixing aluminum powder and refined titanium tetrachloride, enabling the mass of the aluminum powder to be 0.9% of that of the refined titanium tetrachloride, then adding anhydrous aluminum chloride with the same mass as the aluminum powder, stirring at a constant speed, heating the mixture to 130 ℃ within 15 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, and preserving heat and carrying out condensation reflux operation for 15 minutes to obtain the trivalent titanium slurry;
s3, removing vanadium, mixing the trivalent titanium slurry prepared in the step S2 and the crude titanium tetrachloride product in the step S1 in a ratio of 1: mixing the raw materials according to the proportion of 1.5, stirring at a constant speed, heating the mixture to 140 ℃ within 15 minutes, preserving heat, and simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 10min, so as to obtain the rectified titanium tetrachloride;
s4, removing tin, namely, mixing the trivalent titanium slurry prepared in the step S2 with the rectified titanium tetrachloride in the step S3 to obtain a mixture of 1: 2.5, stirring at a constant speed, heating the mixture to 70 ℃ within 15 minutes, preserving heat, simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 17min, and thus obtaining the finished product of the impurity-removed titanium tetrachloride.
In this embodiment, in the step S3, the mass ratio of the trivalent titanium slurry to the crude titanium tetrachloride is adjusted according to the content of vanadium, and when the content of vanadium is ≧ 400ppm, the mass ratio is 1: 1.
In this example, in the step S4, the mass ratio of the trivalent titanium slurry to the refined titanium tetrachloride was adjusted according to the tin content, and when the tin content was ≧ 400ppm, the mass ratio was 1:.
In this example, the stirring speeds in S2, S3 and S4 were all 80 rpm.
Example 4
A method for removing impurity tin from crude titanium tetrachloride, comprising the steps of:
s1, component detection, namely selecting 6 groups of detection samples from the crude titanium tetrachloride products produced in the same batch, then respectively detecting the vanadium and tin contents in each detection sample, then respectively calculating the average value of the vanadium and tin contents of each detection sample, and taking the average value as the vanadium and tin content value of the crude titanium tetrachloride product in the batch;
s2, preparing trivalent titanium slurry, mixing aluminum powder and refined titanium tetrachloride, enabling the mass of the aluminum powder to be 0.95% of that of the refined titanium tetrachloride, then adding anhydrous aluminum chloride with the same mass as the aluminum powder, stirring at a constant speed, heating the mixture to 136 ℃ within 13 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, and preserving heat and carrying out condensation reflux operation for 10-20min to obtain the trivalent titanium slurry;
s3, removing vanadium, mixing the trivalent titanium slurry prepared in the step S2 and the crude titanium tetrachloride product in the step S1 in a ratio of 1: 1.2, uniformly stirring, heating the mixture to 136 ℃ within 17 minutes, preserving heat, and simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 8min, so as to obtain the rectified titanium tetrachloride;
s4, removing tin, namely, mixing the trivalent titanium slurry prepared in the step S2 with the rectified titanium tetrachloride in the step S3 to obtain a mixture of 1: mixing at a ratio of 1.5, stirring at a constant speed, heating the mixture to 95 ℃ within 11 minutes, preserving heat, simultaneously performing condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 17min, and thus obtaining the finished product of the impurity-removed titanium tetrachloride.
In this example, in the step S3, the mass ratio of the trivalent titanium slurry to the crude titanium tetrachloride is adjusted according to the vanadium content, and when the vanadium content is less than 400ppm, the mass ratio of 1:2 ≦ 1: 1.
In this example, in the step S4, the mass ratio of the trivalent titanium slurry to the refined titanium tetrachloride is adjusted according to the tin content, when the tin content is less than or equal to 50ppm and less than 400ppm, and the mass ratio of 1:4 and less than 1: 1.
In this example, the stirring speeds in S2, S3 and S4 are all 140 rpm.
Example 5:
a method for removing impurity tin from crude titanium tetrachloride, comprising the steps of:
s1, component detection, wherein the content of vanadium in the crude titanium tetrachloride is 112.37ppm and the content of tin is 48.07ppm detected by an ICP spectrometer.
S2, preparing trivalent titanium slurry: 523.12g of refined titanium tetrachloride is placed in a three-neck flask, 4.18g of aluminum powder (mass ratio is 0.8%) is added and mixed, 4.18g of anhydrous aluminum chloride is added and stirred, the temperature is controlled at 136 ℃, and the mixture is condensed and refluxed for 20 min.
S3, removing vanadium: 387.67g of crude titanium tetrachloride is taken and placed in a three-neck flask, 193.84g of trivalent titanium slurry (the mass ratio of the trivalent titanium slurry to the crude titanium tetrachloride is 1: 2) is added and mixed, the mixture is stirred, the temperature is controlled to be 136 ℃ at the boiling point of the titanium tetrachloride, the mixture is condensed and refluxed, and the reaction time is 5 min. After the reaction is finished, the titanium tetrachloride is rectified.
S4, removing tin: 407.36g of rectified titanium tetrachloride is taken and placed in a three-neck flask, 101.84g of trivalent titanium slurry (the mass ratio of the trivalent titanium slurry to the rectified titanium tetrachloride is 1: 4) is added and mixed, the mixture is stirred, the temperature is controlled at 80 ℃, and the reaction time is 15 min. After the reaction is finished, the titanium tetrachloride is rectified.
In this example, the stirring speeds in S2, S3 and S4 are all 140 rpm.
The ICP spectrometer is used for detecting, and the tin content of the refined titanium tetrachloride prepared by the method meets the national standard requirement, namely SnCl4 is less than 0.005%.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A method for removing impurity tin in crude titanium tetrachloride is characterized in that: the method for removing the impurity tin in the crude titanium tetrachloride comprises the following steps:
s1, component detection, namely selecting 3-10 groups of detection samples from the crude titanium tetrachloride products produced in the same batch, then respectively detecting the content of vanadium and tin in each detection sample, then respectively calculating the average value of the content of vanadium and tin in each detection sample, and taking the average value as the content value of vanadium and tin in the crude titanium tetrachloride products in the batch;
s2, preparing trivalent titanium slurry, mixing aluminum powder and refined titanium tetrachloride, enabling the mass of the aluminum powder to be 0.8% -1% of that of the refined titanium tetrachloride, then adding anhydrous aluminum chloride with the same mass as the aluminum powder, stirring at a constant speed, heating the mixture to 120-150 ℃ within 10-20 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, and preserving heat and carrying out condensation reflux operation for 10-20 minutes to obtain the trivalent titanium slurry;
s3, removing vanadium, mixing the trivalent titanium slurry prepared in the step S2 and the crude titanium tetrachloride product in the step S1 in a ratio of 1: 1-2, uniformly stirring, heating the mixture to 120-150 ℃ within 10-20 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, wherein the heat preservation and condensation reflux operation time is 5-15min, and obtaining the rectified titanium tetrachloride;
s4, removing tin, namely, mixing the trivalent titanium slurry prepared in the step S2 with the rectified titanium tetrachloride in the step S3 to obtain a mixture of 1: 1-4, stirring at constant speed, heating the mixture to 80-100 ℃ within 10-20 minutes, preserving heat, simultaneously carrying out condensation reflux operation during heating, wherein the time of the heat preservation and the condensation reflux operation is 15-20min, and obtaining the finished product of the impurity-removed titanium tetrachloride.
2. The method according to claim 1, wherein in the step S3, the mass ratio of the trivalent titanium slurry to the crude titanium tetrachloride is adjusted according to the content of vanadium, and when the content of vanadium is equal to or greater than 400ppm, the mass ratio is 1: 1; when the vanadium content is less than 400ppm, the mass ratio of 1:2 to less than or equal to 1: 1.
3. The method according to claim 1, wherein in the step S4, the mass ratio of the trivalent titanium slurry to the refined titanium tetrachloride is adjusted according to the tin content, and when the tin content is not less than 400ppm, the mass ratio is 1: 1; when the tin content is less than or equal to 50ppm and less than 400ppm, the mass ratio of 1:4 is less than 1: 1; when the tin content is less than 50ppm, the mass ratio is 1: 4.
4. The method of claim 1, wherein the stirring speed in each of S2, S3 and S4 is 70-150 rpm.
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| US8906340B2 (en) * | 2011-02-23 | 2014-12-09 | E I Du Pont De Nemours And Company | Purification of TiCl4 through the production of new co-products |
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| CN104326505A (en) * | 2014-10-20 | 2015-02-04 | 洛阳双瑞万基钛业有限公司 | Deep separation method for reducing tin content in titanium tetrachloride |
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