CN117509720A - Method for preparing high-purity titanium dioxide by self-generated seed crystal nucleation method - Google Patents
Method for preparing high-purity titanium dioxide by self-generated seed crystal nucleation method Download PDFInfo
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- CN117509720A CN117509720A CN202311474038.8A CN202311474038A CN117509720A CN 117509720 A CN117509720 A CN 117509720A CN 202311474038 A CN202311474038 A CN 202311474038A CN 117509720 A CN117509720 A CN 117509720A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 186
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000013078 crystal Substances 0.000 title claims abstract description 36
- 238000010899 nucleation Methods 0.000 title claims abstract description 19
- 230000006911 nucleation Effects 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000126 substance Substances 0.000 claims abstract description 19
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims description 22
- 239000002253 acid Substances 0.000 claims description 13
- 230000002378 acidificating effect Effects 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 208000028659 discharge Diseases 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000017525 heat dissipation Effects 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 30
- 239000012752 auxiliary agent Substances 0.000 abstract description 17
- 239000003513 alkali Substances 0.000 abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000002912 waste gas Substances 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 6
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002667 nucleating agent Substances 0.000 abstract description 3
- 238000010791 quenching Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000009965 odorless effect Effects 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- OTJXRUHUGBSPCL-UHFFFAOYSA-N arsanylidynechromium Chemical compound [As]#[Cr] OTJXRUHUGBSPCL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing high-purity titanium dioxide by a self-generated seed crystal nucleation method, which relates to the technical field of high-purity titanium dioxide preparation, and solves the problems that ammonia nitrogen substances are introduced and wastewater and waste gas are generated when alkali or ammonia auxiliary agents are added in the traditional high-purity titanium dioxide production process, the treatment and the discharge are required, the environmental protection cost is increased, and impurities are introduced after the alkali or ammonia auxiliary agents are added, so that the purity of a product cannot be improved. Compared with the traditional high-purity titanium dioxide production mode, the method does not add alkali or ammonia auxiliary agent as a nucleating agent, but utilizes titanium tetrachloride and pure water to excite and quench to generate autogenous crystal seeds, then nucleates, and promotes the reaction to rapidly proceed to the direction of generating hydrated titanium dioxide.
Description
Technical Field
The invention relates to the technical field of high-purity titanium dioxide preparation, in particular to a method for preparing high-purity titanium dioxide by an autogenous seed crystal nucleation method.
Background
The high-purity titanium dioxide is an important inorganic compound different from common titanium dioxide, is white powder, has excellent electrical and optical properties, is nontoxic, harmless, odorless and odorless, is an environment-friendly product for replacing lead-containing, arsenic-chromium and other materials, and is widely applied to the advanced manufacturing fields of electronic elements, optical glass, information communication, aerospace military industry, new energy automobiles and the like. Today, the environmental protection intensity of the world is bigger and bigger, and the advanced application field of the country is developed, the demand for the high-purity titanium dioxide is increasing in recent years, and the method for preparing the high-purity titanium dioxide, which is environment-friendly, energy-saving, cost-reducing and synergistic, is imperative.
In the traditional high-purity titanium dioxide production process, titanium tetrachloride is generally used as a main raw material, alkali or ammonia auxiliary agent is used as an auxiliary agent in the process to react to generate hydrated titanium dioxide, and then the hydrated titanium dioxide is subjected to the following working procedures to prepare a finished product. This method requires alkali or ammonia as an auxiliary agent to be added to the reaction process in order to achieve the purpose of allowing the reaction to proceed efficiently in the direction of formation and finally producing high purity titanium dioxide.
However, due to the use of alkali or ammonia auxiliary agents, ammonia nitrogen substances can be introduced in the production process, waste water and waste gas are generated, the waste water and waste gas are treated and discharged at great cost, the environmental protection cost is increased, and impurities can be increased or introduced after the alkali or ammonia auxiliary agents are added, so that the purity of the product cannot be improved.
Accordingly, the present invention proposes a method for preparing high purity titanium dioxide by a self-generated seed nucleation method to solve the above-mentioned problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing high-purity titanium dioxide by a self-generated seed crystal nucleation method, which solves the problems that ammonia nitrogen substances are introduced and waste water and waste gas are generated when alkali or ammonia auxiliary agent is added as an auxiliary agent in the traditional high-purity titanium dioxide production process, the treatment and the discharge are required to be carried out at great cost, the environmental protection cost is increased, impurities are introduced after the alkali or ammonia auxiliary agent is added, and the purity of the product cannot be improved.
In order to achieve the above purpose, the invention is realized by the following technical scheme: the method for preparing the high-purity titanium dioxide by using the self-generated seed crystal nucleation method specifically comprises the following steps:
firstly, weighing a certain amount of pure water according to a proportion, and placing the pure water in a crystallization kettle for standby;
adding titanium tetrachloride into the crystallization kettle filled with quantitative pure water in the first step at a certain rate, stirring by using a planetary stirrer, and controlling the rotating speed of the planetary stirrer to enable the titanium tetrachloride to react with the pure water to form autogenous seed crystals;
step three, adding the autogenous seed crystal in the step two into the step one, so as to promote the reaction to accelerate to generate more crystals and enable the crystals to be all solid particles;
step four, performing precipitation and acid removal treatment on the crystallized titanium dioxide to remove impurities and acidic substances in the titanium dioxide to form a pure titanium dioxide product;
step five, washing the titanium dioxide product obtained in the step three to remove residual acidic substances and impurities in the titanium dioxide product to obtain a purer titanium dioxide product;
step six, acid discharge treatment is carried out again after the treatment in the step four so as to remove residual acidic substances in the titanium dioxide to obtain purer titanium dioxide products;
step seven, carrying out plate-frame filter pressing treatment after the treatment in the step five so as to separate solid matters from water and obtain titanium dioxide solids containing certain water;
step eight, calcining the pressure-filtered titanium dioxide product in a calciner to form a dry titanium dioxide product;
and step nine, putting the dried titanium dioxide product into a grinder for grinding, and packaging the ground product.
In the first step, titanium tetrachloride and pure water react exothermically at room temperature, and a heat dissipation device is arranged in the reaction kettle.
Further, in the second and third steps, the stirring speed is 30r/min.
Further, in the fifth step, the water washing time is 10-15 minutes.
In the sixth step, the PH test paper or other PH measuring tool is used to measure the PH of the solution after acid discharge, and the PH is kept neutral.
Further, in the seventh step, the press filtration time is 40-60 minutes.
Further, in the step eight, the temperature of the calciner is 800-900 ℃ and the calcination time is 1-3 hours.
Further, in the step nine, the grinding machine is forbidden to be mixed with other products, and the grinding granularity of the titanium dioxide is controlled to be 0.1-10 microns.
Advantageous effects
The invention provides a method for preparing high-purity titanium dioxide by a self-generated seed crystal nucleation method. Compared with the prior art, the method has the following beneficial effects:
1. a method for preparing high-purity titanium dioxide by a self-generated seed crystal nucleation method comprises the following steps of firstly, weighing a certain amount of pure water in proportion, and placing the pure water in a crystallization kettle for standby; adding titanium tetrachloride into the crystallization kettle filled with quantitative pure water in the first step at a certain rate, stirring by using a planetary stirrer, and controlling the rotating speed of the planetary stirrer to enable the titanium tetrachloride to react with the pure water to form autogenous seed crystals; step three, adding the autogenous seed crystal in the step two into the step one, so as to promote the reaction to accelerate to generate more crystals and enable the crystals to be all solid particles; step four, performing precipitation and acid removal treatment on the crystallized titanium dioxide to remove impurities and acidic substances in the titanium dioxide to form a pure titanium dioxide product; step five, washing the titanium dioxide product obtained in the step three to remove residual acidic substances and impurities in the titanium dioxide product to obtain a purer titanium dioxide product; step six, acid discharge treatment is carried out again after the treatment in the step four so as to remove residual acidic substances in the titanium dioxide to obtain purer titanium dioxide products; step seven, carrying out plate-frame filter pressing treatment after the treatment in the step five so as to separate solid matters from water and obtain titanium dioxide solids; step eight, calcining the pressure-filtered titanium dioxide product in a calciner to form a dry titanium dioxide product; and step nine, grinding the dried titanium dioxide product in a grinder, and packaging the ground product, wherein in the step one, titanium tetrachloride and pure water react exothermically at room temperature, and a heat dissipation device is arranged in a reaction kettle. In the second and third steps, the stirring speed is 30r/min. In the fifth step, the water washing time is 10-15 minutes. And step six, measuring the pH value of the solution after acid discharge by using pH test paper or other pH value measuring tools, and keeping the pH value neutral. In the seventh step, the filter pressing time is 40-60 minutes. In the eighth step, the temperature of the calciner is 800-1000 ℃ and the calcination time is 1-3 hours. In the step nine, the grinding machine is forbidden to be mixed with other products, the grinding granularity of the titanium dioxide is controlled to be 0.1-10 microns, and the problems that ammonia nitrogen substances are introduced and waste water and waste gas are generated when alkali or ammonia auxiliary agents are added in the traditional titanium dioxide production process, the waste water and the waste gas are required to be treated and discharged at great cost, the environmental protection cost is increased, impurities are also introduced after the alkali or ammonia auxiliary agents are added, and the purity of the products cannot be improved are solved.
2. Compared with the traditional titanium dioxide production mode, the novel core technology does not add alkali or ammonia auxiliary agent as a nucleating agent, but utilizes titanium tetrachloride and pure water to excite and quench to generate self-generated crystal seeds, then nucleate, and promote the reaction to rapidly proceed towards the direction of generating hydrated titanium dioxide.
Drawings
FIG. 1 is a flow chart of a method for preparing high purity titanium dioxide by the self-generated seed nucleation method of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1, the present invention proposes a technical solution: the method for preparing the high-purity titanium dioxide by using the self-generated seed crystal nucleation method specifically comprises the following steps:
firstly, weighing a certain amount of pure water according to a proportion, and placing the pure water in a crystallization kettle for standby;
adding titanium tetrachloride into the crystallization kettle filled with quantitative pure water in the first step at a certain rate, stirring by using a planetary stirrer, and controlling the rotating speed of the planetary stirrer to enable the titanium tetrachloride to react with the pure water to form autogenous seed crystals;
step three, adding the autogenous seed crystal in the step two into the step one, so as to promote the reaction to accelerate to generate more crystals and enable the crystals to be all solid particles;
step four, performing precipitation and acid removal treatment on the crystallized titanium dioxide to remove impurities and acidic substances in the titanium dioxide to form a pure titanium dioxide product;
and fifthly, washing the titanium dioxide product obtained in the step three to remove residual acidic substances and impurities in the titanium dioxide product to obtain a purer titanium dioxide product, and washing the solid substance obtained by precipitation for multiple times to remove the residual acidic substances and impurities in the titanium dioxide product. Washing is usually performed with high purity water such as deionized water or distilled water.
Step six, acid discharge treatment is carried out again after the treatment in the step four so as to remove residual acidic substances in the titanium dioxide to obtain purer titanium dioxide products;
step seven, carrying out plate-frame filter pressing treatment after the treatment in the step five so as to separate solid matters from water and obtain titanium dioxide solids, wherein the specific treatment process is as follows: preparing plate-frame filter pressing equipment: cleaning and sterilizing the plate-and-frame filter press machine, so as to ensure that the equipment is clean and sanitary and has no impurities and pollutants; filling solid substances: filling the solid matters subjected to water washing and acid discharge treatment into a plate-and-frame filter pressing machine, and paying attention to uniform distribution so as to avoid accumulation and gaps; and (3) performing filter pressing: carrying out filter pressing treatment on the filled plate-and-frame filter pressing machine, and generally adopting a pressure filtering mode to separate solid matters from water; separating solid and liquid: separating solid and liquid obtained after filter pressing, and separating by adopting methods such as centrifugal separation or filtration; drying the solid: and drying the separated solid matters to remove water and solvent in the solid matters to obtain titanium dioxide solids.
Step eight, calcining the pressure-filtered titanium dioxide product in a calciner to form a dry titanium dioxide product;
and step nine, putting the dried titanium dioxide product into a grinder for grinding, and packaging the ground product.
Solves the problems that the method for adding alkali or ammonia auxiliary agent in the traditional titanium dioxide production process can produce waste water and waste gas and introduce ammonia nitrogen compound, needs to be treated and discharged, increases the environmental protection cost, increases the possibility of introducing impurities by adding alkali or ammonia auxiliary agent, reduces the purity of the product and is unfavorable for the sales and subsequent use of the product.
Compared with the traditional titanium dioxide production mode, the invention uses a brand new core technology, does not add alkali or ammonia auxiliary agent as a nucleating agent, but utilizes titanium tetrachloride and pure water to excite, quench and generate autogenous crystal seeds, then nucleates, and promotes the reaction to rapidly proceed to the direction of generating hydrated titanium dioxide.
In the embodiment of the invention, in the first step, titanium tetrachloride and pure water react exothermically at room temperature, and a heat dissipation device is arranged in a reaction kettle. The heat dissipation device is the prior art and is not described here in detail.
In the embodiment of the invention, in the second step and the third step, the stirring speed is 30r/min.
In the embodiment of the invention, in the fifth step, the water washing time is 10-15 minutes.
In the embodiment of the invention, in the step six, the PH test paper or other PH measuring tools are used for measuring the PH value of the solution after acid discharge, and the PH value is kept to be neutral.
In the embodiment of the invention, in the step seven, the filter pressing time is 40-60 minutes.
In the embodiment of the invention, the temperature of the calciner in the step eight is 800-900 ℃ and the calcination time is 1-3 hours.
In the embodiment of the invention, in the step nine, the grinding machine is forbidden to be mixed with other products, and the grinding granularity of the titanium dioxide is controlled to be 0.1-10 microns.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for preparing high-purity titanium dioxide by a self-generated seed crystal nucleation method is characterized in that: the method specifically comprises the following steps:
firstly, weighing a certain amount of pure water according to a proportion, and placing the pure water in a crystallization kettle for standby;
adding titanium tetrachloride into the crystallization kettle filled with quantitative pure water in the first step at a certain rate, stirring by using a planetary stirrer, and controlling the rotating speed of the planetary stirrer to enable the titanium tetrachloride to react with the pure water to form autogenous seed crystals;
step three, adding the autogenous seed crystal in the step two into the step one, so as to promote the reaction to accelerate to generate more crystals and enable the crystals to be all solid particles;
step four, performing precipitation and acid removal treatment on the crystallized titanium dioxide to remove impurities and acidic substances in the titanium dioxide to form a pure titanium dioxide product;
step five, washing the titanium dioxide product obtained in the step three to remove residual acidic substances and impurities in the titanium dioxide product to obtain a purer titanium dioxide product;
step six, acid discharge treatment is carried out again after the treatment in the step four so as to remove residual acidic substances in the titanium dioxide to obtain purer titanium dioxide products;
step seven, carrying out plate-frame filter pressing treatment after the treatment in the step five so as to separate solid matters from water and obtain titanium dioxide solids;
step eight, calcining the pressure-filtered titanium dioxide product in a calciner to form a dry titanium dioxide product;
and step nine, placing the dried high-purity titanium dioxide product into a grinder for grinding, and packaging the ground product.
2. The method for preparing high-purity titanium dioxide by using the self-generated seed crystal nucleation method according to claim 1, wherein the method comprises the following steps: in the first step, titanium tetrachloride and pure water react exothermically at room temperature, and a heat dissipation device is arranged in the reaction kettle.
3. The method for preparing high-purity titanium dioxide by using the self-generated seed crystal nucleation method according to claim 1, wherein the method comprises the following steps: in the second step and the third step, the stirring speed is 30r/min.
4. The method for preparing high-purity titanium dioxide by using the self-generated seed crystal nucleation method according to claim 1, wherein the method comprises the following steps: in the fifth step, the water washing time is 10-15 minutes.
5. The method for preparing high-purity titanium dioxide by using the self-generated seed crystal nucleation method according to claim 1, wherein the method comprises the following steps: in the step six, PH test paper or other PH measuring tools are used for measuring the PH value of the solution after acid discharge, and the PH value is kept neutral.
6. The method for preparing high-purity titanium dioxide by using the self-generated seed crystal nucleation method according to claim 1, wherein the method comprises the following steps: in the seventh step, the filter pressing time is 40-60 minutes.
7. The method for preparing high-purity titanium dioxide by using the self-generated seed crystal nucleation method according to claim 1, wherein the method comprises the following steps: in the step eight, the temperature of the calciner is 800-900 ℃ and the calcination time is 1-3 hours.
8. The method for preparing high-purity titanium dioxide by using the self-generated seed crystal nucleation method according to claim 1, wherein the method comprises the following steps: in the step nine, the grinding machine is forbidden to be mixed with other products, and the grinding granularity of the titanium dioxide is controlled to be in the range of 0.1-10 microns according to requirements.
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