CN110040774B - Method for preparing nano titanium dioxide by using metatitanic acid - Google Patents
Method for preparing nano titanium dioxide by using metatitanic acid Download PDFInfo
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- CN110040774B CN110040774B CN201910369590.8A CN201910369590A CN110040774B CN 110040774 B CN110040774 B CN 110040774B CN 201910369590 A CN201910369590 A CN 201910369590A CN 110040774 B CN110040774 B CN 110040774B
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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
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- 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
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- 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
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Abstract
The invention discloses a method for preparing nano titanium dioxide by using metatitanic acid, which comprises the following steps: (1) dispergating: controlling the content of titanium dioxide in metatitanic acid to be 15-30 wt%, and adding barium nitrate with a molar ratio of 60% and stirring for half an hour and barium carbonate with a molar ratio of 40% and stirring for half an hour; (2) washing and purifying: washing and purifying the titanium dioxide sol, and controlling the conductivity of the filtrate to be less than or equal to 3500us/cm; (3) spray drying: removing water from the washed and purified titanium dioxide sol in a spray drying mode; (4) calcining: calcining the dried titanium dioxide, and controlling the specific surface area; (5) crushing: and crushing the calcined sample by adopting a high-pressure airflow crushing mode. The invention has the beneficial effects that the titanium dioxide prepared by the steps of dispergation, washing and purifying, spray drying, calcining, airflow crushing and the like has the advantages of uniform particle size distribution, good dispersibility and nano material characteristics.
Description
Technical Field
The invention relates to the field of a preparation method of nano titanium dioxide.
Background
Metatitanic acid is an intermediate for producing titanium dioxide by a sulfuric acid method, and is obtained by acidolysis, sedimentation, filtration, crystallization, disc filtration, concentration, hydrolysis, rinsing, bleaching and water washing processes, and the process flow is described in detail in the production of titanium dioxide by the sulfuric acid method, so that the titanium dioxide has the defects of strong inter-particle agglomeration, nonuniform particle distribution, wide particle size distribution, coarse particles, poor dispersion stability and the like, and the defects make the prepared titanium dioxide product difficult to modify and poor in effect.
Chinese patent publication No. CN109336172A discloses a method for preparing nano titanium dioxide for photocatalysis by using metatitanic acid as a raw material, wherein metatitanic acid is added into a sulfuric acid solution for acidolysis to obtain a titanyl sulfate solution; adding the titanyl sulfate solution into an inorganic alkali solution for neutralization to obtain an orthotitanic acid precipitate; preparing orthotitanic acid into a suspension, and adding hydrogen peroxide into the suspension to obtain peroxotitanic acid; and carrying out hydrothermal reaction on the peroxotitanic acid, cooling, and carrying out spray drying to obtain the nano titanium dioxide. Also, for example, chinese patent publication No. CN104667901A discloses a method for preparing a nano titanium dioxide as a denitration catalyst carrier, which comprises using metatitanic acid as a raw material, an intermediate for preparing titanium dioxide by a sulfuric acid method, adding ammonium salt, adjusting pH, washing, filtering, drying, and calcining to obtain a nano titanium dioxide product as a denitration catalyst carrier, wherein the dispersibility and uniformity of the above two nano titanium dioxide finished products have a further improved space.
Disclosure of Invention
The technical problem to be solved by the invention is that the existing nano titanium dioxide particles prepared by using metatitanic acid as a raw material have insufficient distribution uniformity and poor dispersion stability, so that the method for preparing nano titanium dioxide by using metatitanic acid has uniform particle size distribution and good dispersion stability.
The technical scheme of the invention is as follows: the method for preparing the nano titanium dioxide by using the metatitanic acid comprises the following steps: (1) dispergation: controlling the content of titanium dioxide in metatitanic acid to be 15-30 wt%, and adding barium nitrate with a molar ratio of 60% and stirring for half an hour and barium carbonate with a molar ratio of 40% and stirring for half an hour; (2) washing and purifying: washing and purifying the titanium dioxide sol by adopting an ultrafiltration membrane system, and controlling the conductivity of the filtrate to be less than or equal to 3500us/cm by continuously supplementing desalted water instead of an aqueous solution; (3) spray drying: removing water from the washed and purified titanium dioxide sol in a spray drying mode, wherein the drying temperature is 300-400 ℃; (4) calcining: calcining the dried titanium dioxide at 500-800 ℃, and controlling the specific surface area; (5) crushing: and crushing the calcined sample by adopting a high-pressure airflow crushing mode, wherein the airflow pressure is 1MPa.
The invention has the beneficial effects that the titanium dioxide prepared by the steps of dispergation, washing and purification, spray drying, calcination, jet milling and the like has the advantages of uniform particle size distribution, good dispersibility and nano material characteristics.
Drawings
FIG. 1 is a distribution diagram of the particle size of the nano titanium dioxide of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention is clearly and completely described below with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments based on the embodiments in the present invention, without any inventive work, will be apparent to those skilled in the art from the following description.
Example 1: the method for preparing the nano titanium dioxide by using the metatitanic acid comprises the following steps: (1) dispergation: controlling the titanium dioxide content in metatitanic acid to be 15wt%, and adding barium nitrate with a molar ratio of 60% in sequence and stirring for half an hour and barium carbonate with a molar ratio of 40% in sequence and stirring for half an hour; (2) washing and purifying: washing and purifying the titanium dioxide sol by adopting an ultrafiltration membrane system, and controlling the conductivity of the filtrate to be less than or equal to 3500us/cm by continuously supplementing desalted water instead of an aqueous solution; (3) spray drying: removing water from the washed and purified titanium dioxide sol in a spray drying mode, wherein the drying temperature is 300 ℃; (4) calcining: calcining the dried titanium dioxide at 500 ℃, and controlling the specific surface area; (5) crushing: and crushing the calcined sample by adopting a high-pressure airflow crushing mode, wherein the airflow pressure is 1MPa.
Example 2: the method for preparing the nano titanium dioxide by using the metatitanic acid comprises the following steps: (1) dispergation: controlling the titanium dioxide content in metatitanic acid to be 20wt%, and adding barium nitrate with a molar ratio of 60% in sequence and stirring for half an hour and barium carbonate with a molar ratio of 40% in sequence and stirring for half an hour; (2) washing and purifying: washing and purifying the titanium dioxide sol by adopting an ultrafiltration membrane system, and controlling the conductivity of the filtrate to be less than or equal to 3500us/cm by continuously supplementing desalted water instead of an aqueous solution; (3) spray drying: removing water from the washed and purified titanium dioxide sol in a spray drying mode, wherein the drying temperature is 350 ℃; (4) calcining: calcining the dried titanium dioxide at 650 ℃, and controlling the specific surface area; (5) crushing: and crushing the calcined sample by adopting a high-pressure airflow crushing mode, wherein the airflow pressure is 1MPa.
Example 3: the method for preparing the nano titanium dioxide by using the metatitanic acid comprises the following steps: (1) dispergating: controlling the titanium dioxide content in metatitanic acid to be 30wt%, and adding barium nitrate with a molar ratio of 60% in sequence and stirring for half an hour and barium carbonate with a molar ratio of 40% in sequence and stirring for half an hour; (2) washing and purifying: washing and purifying the titanium dioxide sol by adopting an ultrafiltration membrane system, and controlling the conductivity of the filtrate to be less than or equal to 3500us/cm by continuously supplementing desalted water instead of an aqueous solution; (3) spray drying: removing water from the washed and purified titanium dioxide sol in a spray drying mode, wherein the drying temperature is 400 ℃; (4) calcining: calcining the dried titanium dioxide at 800 ℃, and controlling the specific surface area; (5) crushing: and crushing the calcined sample by adopting a high-pressure airflow crushing mode, wherein the airflow pressure is 1MPa.
As shown in FIG. 1, the nano titanium dioxide particles prepared by the invention are normally distributed and have no tailing phenomenon. The particle size distribution of the nano titanium dioxide particles is uniform.
The following table shows the dispersibility comparisons for examples 1-3 and the prior art products under the same conditions:
product(s) | Dispersibility (test under equivalent conditions) |
Example 1 | 3.67mPa.s |
Example 2 | 3.62mPa.s |
Example 3 | 3.69mPa.s |
Existing products | 343mPa.s |
As can be seen from the table above, the dispersibility of the nano titanium dioxide prepared by the invention is obviously superior to that of the existing product.
In the invention, barium nitrate reacts with free sulfuric acid and sulfuric acid combined with titanium to generate barium sulfate precipitate, reduces intermolecular force of titanium dioxide, completely disperses agglomerated titanium dioxide molecules, and dissolves partial insoluble substances in the presence of nitric acid to reduce impurities; barium carbonate itself cannot directly react with sulfuric acid as a precipitate, but reacts with nitric acid to generate barium nitrate and titanium dioxide gas, and the barium nitrate continues to react. The molar ratio of barium nitrate to barium carbonate was set to 0.6:0.4, because the reaction is not complete if the barium nitrate content is low, the acidity is low if the content is high, and the sample with low acidity is easy to gel. The conductivity of the filtrate in the step (2) is less than or equal to 3500us/cm, because the conductivity is high, the impurity content is high, and the energy consumption for continuous washing is high.
Claims (1)
1. The method for preparing the nano titanium dioxide by using the metatitanic acid is characterized by comprising the following steps of: (1) dispergating: controlling the content of titanium dioxide in metatitanic acid to be 15-30 wt%, sequentially adding barium nitrate with a molar ratio of 60% and stirring for half an hour and barium carbonate with a molar ratio of 40% and stirring for half an hour, reacting the barium nitrate with free sulfuric acid and sulfuric acid combined with titanium to generate barium sulfate precipitate, dissolving part of insoluble substances in the presence of nitric acid to reduce impurities, reacting the barium carbonate with the nitric acid to generate barium nitrate and carbon dioxide gas, and continuously reacting the barium nitrate; (2) washing and purifying: washing and purifying the titanium dioxide sol by adopting an ultrafiltration membrane system, and controlling the conductivity of the filtrate to be less than or equal to 3500us/cm by continuously supplementing desalted water instead of an aqueous solution; (3) spray drying: removing water from the washed and purified titanium dioxide sol in a spray drying mode, wherein the drying temperature is 300-400 ℃; (4) calcining: calcining the dried titanium dioxide at 500-800 ℃, and controlling the specific surface area; (5) crushing: and crushing the calcined sample by adopting a high-pressure airflow crushing mode, wherein the airflow pressure is 1MPa.
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CN113620333A (en) * | 2021-09-01 | 2021-11-09 | 佛山集美精化科技有限公司 | Method for synthesizing composite barium sulfate from metatitanic acid |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS54146286A (en) * | 1978-05-09 | 1979-11-15 | Kobe Steel Ltd | Denitration catalyst carrier |
DE3628661A1 (en) * | 1986-08-23 | 1988-03-03 | Metallgesellschaft Ag | METHOD FOR PRODUCING TIO (DOWN ARROW) 2 (DOWN ARROW) COMPOSITION PIGMENTS |
CN101318698A (en) * | 2008-07-11 | 2008-12-10 | 四川华铁钒钛科技股份有限公司 | Method for preparing anatase type nano-titanium dioxide |
CN103721726A (en) * | 2013-12-18 | 2014-04-16 | 攀枝花市钛都化工有限公司 | Preparation method of high-intensity titanium dioxide for denitration catalyst |
CN106140144A (en) * | 2016-06-28 | 2016-11-23 | 攀枝花学院 | SCR denitration and preparation method thereof |
CN108299863A (en) * | 2018-01-31 | 2018-07-20 | 攀枝花学院 | A kind of clean preparation method of titanium white |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS54146286A (en) * | 1978-05-09 | 1979-11-15 | Kobe Steel Ltd | Denitration catalyst carrier |
DE3628661A1 (en) * | 1986-08-23 | 1988-03-03 | Metallgesellschaft Ag | METHOD FOR PRODUCING TIO (DOWN ARROW) 2 (DOWN ARROW) COMPOSITION PIGMENTS |
CN101318698A (en) * | 2008-07-11 | 2008-12-10 | 四川华铁钒钛科技股份有限公司 | Method for preparing anatase type nano-titanium dioxide |
CN103721726A (en) * | 2013-12-18 | 2014-04-16 | 攀枝花市钛都化工有限公司 | Preparation method of high-intensity titanium dioxide for denitration catalyst |
CN106140144A (en) * | 2016-06-28 | 2016-11-23 | 攀枝花学院 | SCR denitration and preparation method thereof |
CN108299863A (en) * | 2018-01-31 | 2018-07-20 | 攀枝花学院 | A kind of clean preparation method of titanium white |
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