CN113461049A - Preparation method of ultrahigh-purity titanium dioxide - Google Patents
Preparation method of ultrahigh-purity titanium dioxide Download PDFInfo
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- CN113461049A CN113461049A CN202110917332.6A CN202110917332A CN113461049A CN 113461049 A CN113461049 A CN 113461049A CN 202110917332 A CN202110917332 A CN 202110917332A CN 113461049 A CN113461049 A CN 113461049A
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- ultrahigh
- purity
- purity titanium
- titanium dioxide
- titanium tetrachloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a preparation method of ultrahigh-purity titanium dioxide, which comprises the following steps: (1) preparing ultrahigh-purity titanium tetrachloride: rectifying and purifying titanium tetrachloride to obtain ultra-high purity titanium tetrachloride with the purity of more than or equal to 99.99999 percent; (2) hydrolyzing the ultra-high purity titanium tetrachloride: slowly dropping pure water into a hydrolysis device filled with ultrahigh-purity titanium tetrachloride, continuously and uniformly stirring to generate yellow precipitate, and then continuously dropping the pure water into the hydrolysis device until the precipitate in the hydrolysis device is completely dissolved to form yellow oily liquid; (3) vacuum distillation: distilling the yellow oily liquid for 3-5 hours under the conditions of vacuum degree of-0.08-0.1 MPa and temperature of 80-100 ℃ to obtain a solid; (4) preparing ultra-pure titanium dioxide: putting the obtained solid residues into a clean container, firing for 4-5 hours at a high temperature of 600-800 ℃, and cooling to obtain ultrahigh-purity titanium dioxide with the purity of more than or equal to 99.999%; the method realizes the preparation of the titanium dioxide with short flow, low cost and ultrahigh purity by hydrolyzing the ultrahigh-purity titanium tetrachloride with the purity of more than or equal to 99.99999 percent.
Description
Technical Field
The invention relates to the field of fine chemical products, in particular to a preparation method of ultrahigh-purity titanium dioxide.
Background
Titanium dioxide is an inorganic substance with stable physicochemical properties, and is widely applied to industries such as coatings, cosmetics, paper making and the like. The titanium dioxide has the characteristics of semiconductor performance, high dielectric constant and resistivity, and excellent mechanical and electrical properties. In recent years, titanium dioxide has been attracting attention in high-end manufacturing, electronic components, catalysts, and other related fields due to its excellent photochemical characteristics. In these fields, high purity titanium dioxide materials can be widely used in such fields as barium titanate lithium batteries, nano-scale catalyst carriers, electronic ceramics, etc., and thus the preparation method of titanium dioxide with higher purity is becoming the mainstream of research.
In recent years, a high purity titanium dioxide production method mainly includes: titanium alkoxide hydrolysis, sulfuric acid method and titanium tetrachloride hydrolysis. The titanium alkoxide hydrolysis method is mainly characterized in that titanium tetrachloride and alcohols react, metatitanic acid is formed after hydrolysis, and titanium dioxide powder is obtained after calcination of metatitanic acid. Because the process flow is long and the cost of the titanium alkoxide is too high, the preparation method cannot be put into industrial production. The sulfuric acid method is to carry out acidolysis reaction on ilmenite powder and concentrated sulfuric acid to generate titanyl sulfate, generate hydrated titanium dioxide by water, and then calcine and crush the hydrated titanium dioxide to obtain a titanium dioxide product. However, the method consumes large amount of sulfuric acid and byproducts, the waste materials generated are difficult to treat, a series of environmental problems are caused, and the purity of the obtained product is too low and is eliminated in the preparation process of high-purity titanium dioxide. The hydrolysis method of titanium tetrachloride is one of the main methods for industrially preparing high-purity titanium dioxide, and the high-purity titanium dioxide product is prepared by hydrolyzing titanium tetrachloride and then calcining, and the preparation process is short, and the material is easy to purify, and the like, so that the method is widely applied.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing titanium dioxide with ultrahigh purity, which does not introduce other substances, has a short process flow and low preparation cost, and can prepare titanium dioxide with extremely high purity.
The purpose of the invention is realized by the following technical scheme:
a preparation method of ultrahigh-purity titanium dioxide comprises the following steps:
(1) preparing ultrahigh-purity titanium tetrachloride: rectifying and purifying titanium tetrachloride to obtain ultra-high purity titanium tetrachloride with the purity of more than or equal to 99.99999 percent;
(2) hydrolyzing the ultra-high purity titanium tetrachloride: slowly dropping pure water into a hydrolysis device filled with ultrahigh-purity titanium tetrachloride, continuously and uniformly stirring to generate yellow precipitate, and then continuously dropping the pure water into the hydrolysis device until the precipitate in the hydrolysis device is completely dissolved to form yellow oily liquid;
(3) vacuum distillation: distilling the yellow oily liquid for 3-5 hours under the conditions of vacuum degree of-0.08-0.1 MPa and temperature of 80-100 ℃ to obtain a solid;
(4) preparing ultra-pure titanium dioxide: and (3) putting the obtained solid residues into a clean container, firing for 4-5 hours at a high temperature of 600-800 ℃, and cooling to obtain the ultrahigh-purity titanium dioxide with the purity of more than or equal to 99.999%.
Furthermore, the hydrogen chloride gas generated in the steps (1) to (4) is absorbed by the tail gas treatment device.
Still further, the hydrolysis device is a hydrolysis device with tail gas absorption.
The invention has the beneficial effects that:
according to the preparation method of the ultrahigh-purity titanium dioxide, the ultrahigh-purity titanium tetrachloride with the hydrolysis purity of more than or equal to 99.99999% is used for preparing the ultrahigh-purity titanium dioxide with short flow, low cost and high purity, no additional substance is introduced in the whole production link, the prepared titanium dioxide has low impurity content and the product has extremely high purity, and the method has simple steps and high production efficiency.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof.
Detailed Description
Hereinafter, preferred embodiments of the present invention will be described in detail. It should be understood that the preferred embodiments are illustrative of the invention only and are not limiting upon the scope of the invention.
The chemical principle of the invention is as follows: the titanium tetrachloride is rectified and purified, and reacts with water in multiple steps to generate yellow precipitate TiOCl2 firstly, and then water is added to generate yellow oily liquid, wherein the liquid component is the hydroxyl chloride of titanium.
The specific chemical reaction of the invention is as follows:
TiCl4+H2O→TiOCl2+2HCl
TiOCl2+H2O+2HCl→H2[Ti(OH)2Cl4]
example 1:
a preparation method of ultrahigh-purity titanium dioxide sequentially comprises the following steps:
(1) preparing ultrahigh-purity titanium tetrachloride: the titanium tetrachloride is rectified and purified to obtain the ultrahigh-purity titanium tetrachloride with the purity of 99.99999 percent, and the specific reference is made to a production method of the ultrahigh-purity titanium tetrachloride, the publication number of which is as follows; CN 108178185B.
(2) Slowly dropping 3kg of pure water into a hydrolysis device filled with ultrahigh-purity titanium tetrachloride and tail gas absorption, continuously and uniformly stirring to generate yellow precipitate, continuously dropping the pure water into the hydrolysis device until the precipitate in the hydrolysis device is completely dissolved to form yellow oily liquid, and stopping reaction;
(3) distilling the yellow oily liquid obtained in the last step for 4 hours under the conditions that the vacuum degree is-0.09 MPa and the temperature is 80 ℃ to obtain a solid, and absorbing hydrogen chloride gas generated in the distillation process by a tail gas treatment device;
(4) and (3) putting the obtained solid residues into a clean tray, burning for 5 hours at the constant temperature of 600 ℃, and cooling to obtain 5.5kg of finished ultrahigh-purity titanium dioxide with the purity of 99.999%.
The hydrogen chloride gas generated in the steps is absorbed by the tail gas treatment device to form a byproduct, namely hydrochloric acid, so that the environment is not polluted.
The product sampling treatment is detected by GDMS, and the impurity content results are shown in Table 1:
TABLE 1 results of analysis of the content of impurities in ultra-high purity titanium dioxide of example 1 (unit: ppb, N.D. means no detection)
Example 2:
a preparation method of ultrahigh-purity titanium dioxide sequentially comprises the following steps:
(1) preparing ultrahigh-purity titanium tetrachloride: rectifying and purifying titanium tetrachloride to obtain ultra-high purity titanium tetrachloride with the purity of 99.99999%;
(2) slowly dropping 10kg of pure water into a hydrolysis device filled with ultrahigh-purity titanium tetrachloride and tail gas absorption, continuously and uniformly stirring to generate yellow precipitate, continuously dropping the pure water into the hydrolysis device until the precipitate in the hydrolysis device is completely dissolved to form yellow oily liquid, and stopping reaction;
(3) distilling the yellow oily liquid obtained in the last step for 4 hours under the conditions that the vacuum degree is-0.08 MPa and the temperature is 98 ℃ to obtain a solid, and absorbing hydrogen chloride gas generated in the distillation process by a tail gas treatment device;
(4) and (3) putting the obtained solid residues into a clean tray, burning for 4 hours at the constant temperature of 800 ℃, and cooling to obtain 18.8kg of finished ultrahigh-purity titanium dioxide with the purity of 99.999%.
The hydrogen chloride gas generated in the steps is absorbed by the tail gas treatment device to form a byproduct, namely hydrochloric acid, so that the environment is not polluted.
The product sampling treatment is detected by GDMS, and the impurity content results are shown in Table 2:
TABLE 2 results of analysis of the content of impurities in ultra-high purity titanium dioxide of example 2 (unit: ppb, N.D. means no detection)
Example 3:
a preparation method of ultrahigh-purity titanium dioxide sequentially comprises the following steps:
(1) preparing ultrahigh-purity titanium tetrachloride: rectifying and purifying titanium tetrachloride to obtain ultra-high purity titanium tetrachloride with the purity of 99.99999%;
(2) slowly dropping 20kg of pure water into a hydrolysis device filled with ultrahigh-purity titanium tetrachloride and tail gas absorption, continuously and uniformly stirring to generate yellow precipitate, continuously dropping the pure water into the hydrolysis device until the precipitate in the hydrolysis device is completely dissolved to form yellow oily liquid, and stopping reaction;
(3) distilling the yellow oily liquid obtained in the last step for 5 hours under the conditions that the vacuum degree is-0.1 MPa and the temperature is 100 ℃ to obtain a solid, and absorbing hydrogen chloride gas generated in the distillation process by a tail gas treatment device;
(4) and (3) putting the obtained solid residues into a clean tray, burning for 4 hours at the constant temperature of 700 ℃, and cooling to obtain 37.5kg of finished ultrahigh-purity titanium dioxide with the purity of 99.999%.
The hydrogen chloride gas generated in the steps is absorbed by the tail gas treatment device to form a byproduct, namely hydrochloric acid, so that the environment is not polluted.
The product sampling treatment is detected by GDMS, and the impurity content results are shown in Table 3:
TABLE 3 results of analysis of the content of impurities in ultra-high purity titanium dioxide of example 3 (unit: ppb, N.D. means no detection)
Compared with the prior art, the method does not add any other substances such as oxalic acid and the like in the process of preparing the ultrahigh-purity titanium dioxide.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (3)
1. A preparation method of ultrahigh-purity titanium dioxide is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing ultrahigh-purity titanium tetrachloride: rectifying and purifying titanium tetrachloride to obtain ultra-high purity titanium tetrachloride with the purity of more than or equal to 99.99999 percent;
(2) hydrolyzing the ultra-high purity titanium tetrachloride: slowly dropping pure water into a hydrolysis device filled with ultrahigh-purity titanium tetrachloride, continuously and uniformly stirring to generate yellow precipitate, and then continuously dropping the pure water into the hydrolysis device until the precipitate in the hydrolysis device is completely dissolved to form yellow oily liquid;
(3) vacuum distillation: distilling the yellow oily liquid for 3-5 hours under the conditions of vacuum degree of-0.08-0.1 MPa and temperature of 80-100 ℃ to obtain a solid;
(4) preparing the ultrahigh-purity titanium dioxide: and (3) putting the obtained solid residues into a clean container, firing for 4-5 hours at a high temperature of 600-800 ℃, and cooling to obtain the ultrahigh-purity titanium dioxide with the purity of more than or equal to 99.999%.
2. The process for producing ultra-high purity titanium dioxide according to claim 1, wherein: and (4) absorbing the hydrogen chloride gas generated in the steps (1) to (4) by a tail gas treatment device.
3. The process for producing ultra-high purity titanium dioxide according to claim 1 or 2, wherein: the hydrolysis device is a hydrolysis device with tail gas absorption.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621479A (en) * | 2016-03-18 | 2016-06-01 | 常州大学 | Green preparation technology for TiO2 |
| CN107393622A (en) * | 2017-06-27 | 2017-11-24 | 宁波墨西科技有限公司 | A kind of graphene Asia titanium oxide combined conductive agent and preparation method thereof |
| CN108178185A (en) * | 2018-02-07 | 2018-06-19 | 贵阳精科技有限公司 | A kind of production method of ultra-high purity titanium tetrachloride |
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- 2021-08-11 CN CN202110917332.6A patent/CN113461049A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621479A (en) * | 2016-03-18 | 2016-06-01 | 常州大学 | Green preparation technology for TiO2 |
| CN107393622A (en) * | 2017-06-27 | 2017-11-24 | 宁波墨西科技有限公司 | A kind of graphene Asia titanium oxide combined conductive agent and preparation method thereof |
| CN108178185A (en) * | 2018-02-07 | 2018-06-19 | 贵阳精科技有限公司 | A kind of production method of ultra-high purity titanium tetrachloride |
Non-Patent Citations (2)
| Title |
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| 张鹏等: "四氯化钛热水解制备钛白粉的研究", 《钢铁钒钛》 * |
| 陈瑞澄: "四氯化钛水解过程的研究", 《湿法冶金》 * |
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Application publication date: 20211001 |