CN110040774A - The method for preparing nano-titanium dioxide using metatitanic acid - Google Patents
The method for preparing nano-titanium dioxide using metatitanic acid Download PDFInfo
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- CN110040774A CN110040774A CN201910369590.8A CN201910369590A CN110040774A CN 110040774 A CN110040774 A CN 110040774A CN 201910369590 A CN201910369590 A CN 201910369590A CN 110040774 A CN110040774 A CN 110040774A
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- titanium dioxide
- metatitanic acid
- molar ratio
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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
Abstract
The invention discloses the methods for preparing nano-titanium dioxide using metatitanic acid, it is the following steps are included: (1), dispergation: content of titanium dioxide 15wt%-30wt% in control metatitanic acid, successively adds 60% barium nitrate of molar ratio stirring half an hour and 40% barium carbonate of molar ratio stirs half an hour；(2), washing purifying: washing purifying is carried out to TiO 2 sol, controls filtrate conductivity≤3500us/cm；(3), be spray-dried: the TiO 2 sol washed after purification removes moisture removal by the way of spray drying；(4), calcine: the titanium dioxide calcination after dry controls specific surface area；(5), it crushes: post-calcination sample being crushed by the way of high pressure draught crushing.Have even particle size distribution, good dispersion the beneficial effects of the invention are as follows the titanium dioxide by the preparation of dispergation-washing purifying-spray drying-calcining-air-flow crushing and has the advantages that nano material characteristic.
Description
Technical field
The present invention relates to the preparation method fields of nano-titanium dioxide.
Background technique
Metatitanic acid is the intermediate of Production By Sulfuric Acid Process titanium dioxide, is by acidolysis, sedimentation, filtering, crystallization, disk mistake
Filter, concentration, hydrolysis, rinsing, bleaching, water-washing process and obtain, its technique is described in detail in " sulfuric acid method titanium pigment production " text
Process has the shortcomings that reunion is strong, particle distribution is uneven, size distribution is wide, particle is thick, dispersion stabilization is poor between particle, this
The modified difficulty of the titanium dioxide product that a little disadvantages prepare it, effect are poor.
Chinese invention patent publication number CN109336172A, which is disclosed, prepares photocatalysis nanometer two by raw material of metatitanic acid
Metatitanic acid is added sulfuric acid solution acidolysis, obtains titanyl sulfate solution by the method for titanium oxide；Inorganic base is added in titanyl sulfate solution
Solution neutralizes to obtain positive metatitanic acid precipitating；Positive metatitanic acid is configured to suspension, hydrogen peroxide is added into suspension and obtains pertitanic acid；It will
Pertitanic acid carries out hydro-thermal reaction and carries out being spray-dried to obtain nano-titanium dioxide after cooling.For another example Chinese invention patent publication number
CN104667901A discloses a kind of preparation method of denitration catalyst carrier nano-titanium dioxide, with method for producing gtitanium dioxide with sulphuric acid
Intermediate metatitanic acid be raw material, addition ammonium salt simultaneously adjusts pH value, washed, filtering, it is dry, roast and denitrating catalyst is made carries
Body nanometer titanium dioxide titanium products, the dispersibility and uniformity of both the above nano-titanium dioxide finished product have the sky further promoted
Between.
Summary of the invention
The technical problem to be solved by the present invention is to the existing nano-titania particles point prepared using metatitanic acid as raw material
Cloth lack of uniformity, dispersion stabilization is poor, provide thus a kind of even particle size distribution, dispersion stabilization it is good utilize metatitanic acid system
The method of standby nano-titanium dioxide.
The technical scheme is that the method for preparing nano-titanium dioxide using metatitanic acid, it the following steps are included:
(1), dispergation: it is small successively to add the stirring half of 60% barium nitrate of molar ratio by content of titanium dioxide 15wt%-30wt% in control metatitanic acid
When and 40% barium carbonate of molar ratio stir half an hour；(2), washing purifying: TiO 2 sol is washed using ultrafiltration membrane system
Purifying is washed, by way of desalted water is continuously replenished and substitutes aqueous solution, controls filtrate conductivity≤3500us/cm；(3), spraying
It is dry: wash TiO 2 sol after purification using removing moisture removal by the way of being spray-dried, 300 DEG C -400 DEG C of drying temperature；
(4), calcine: the titanium dioxide after dry controls specific surface area in 500 DEG C of -800 DEG C of calcinings；(5), it crushes: using high pressure draught
The mode of crushing crushes post-calcination sample, stream pressure 1MPa.
The beneficial effects of the invention are as follows by dispergation-washing purifying-spray drying-calcining-air-flow crushing
The titanium dioxide of preparation has even particle size distribution, good dispersion and has the advantages that nano material characteristic.
Detailed description of the invention
Fig. 1 is nano-titanium dioxide grain size distribution of the invention.
Specific embodiment
With reference to the accompanying drawing, technical scheme in the embodiment of the invention is clearly and completely described.Obviously, it is retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, originally
Field those of ordinary skill every other embodiment without making creative work, belongs to protection model of the invention
It encloses.
Embodiment 1: the method for preparing nano-titanium dioxide using metatitanic acid, it is the following steps are included: (1), dispergation: control
Content of titanium dioxide 15wt% in metatitanic acid successively adds 60% barium nitrate of molar ratio stirring half an hour and 40% barium carbonate of molar ratio
Stir half an hour；(2), washing purifying: washing purifying is carried out to TiO 2 sol using ultrafiltration membrane system, by being continuously replenished
Desalted water substitutes the mode of aqueous solution, controls filtrate conductivity≤3500us/cm；(3), it is spray-dried: washing two after purification
Titanium oxide sol removes moisture removal by the way of spray drying, and 300 DEG C of drying temperature；(4), it calcines: the titanium dioxide after dry
It is calcined at 500 DEG C, controls specific surface area；(5), it crushes: post-calcination sample being crushed by the way of high pressure draught crushing, air-flow
Pressure is 1MPa.
Embodiment 2: the method for preparing nano-titanium dioxide using metatitanic acid, it is the following steps are included: (1), dispergation: control
Content of titanium dioxide 20wt% in metatitanic acid successively adds 60% barium nitrate of molar ratio stirring half an hour and 40% barium carbonate of molar ratio
Stir half an hour；(2), washing purifying: washing purifying is carried out to TiO 2 sol using ultrafiltration membrane system, by being continuously replenished
Desalted water substitutes the mode of aqueous solution, controls filtrate conductivity≤3500us/cm；(3), it is spray-dried: washing two after purification
Titanium oxide sol removes moisture removal by the way of spray drying, and 350 DEG C of drying temperature；(4), it calcines: the titanium dioxide after dry
It is calcined at 650 DEG C, controls specific surface area；(5), it crushes: post-calcination sample being crushed by the way of high pressure draught crushing, air-flow
Pressure is 1MPa.
Embodiment 3: the method for preparing nano-titanium dioxide using metatitanic acid, it is the following steps are included: (1), dispergation: control
Content of titanium dioxide 30wt% in metatitanic acid successively adds 60% barium nitrate of molar ratio stirring half an hour and 40% barium carbonate of molar ratio
Stir half an hour；(2), washing purifying: washing purifying is carried out to TiO 2 sol using ultrafiltration membrane system, by being continuously replenished
Desalted water substitutes the mode of aqueous solution, controls filtrate conductivity≤3500us/cm；(3), it is spray-dried: washing two after purification
Titanium oxide sol removes moisture removal by the way of spray drying, and 400 DEG C of drying temperature；(4), it calcines: the titanium dioxide after dry
It is calcined at 800 DEG C, controls specific surface area；(5), it crushes: post-calcination sample being crushed by the way of high pressure draught crushing, air-flow
Pressure is 1MPa.
As shown in Figure 1, nano-titania particle prepared by the present invention is at normal distribution, without trailing phenomenon.Explanation is received
Rice TiO 2 particles even particle size distribution.
Following table is under equal conditions to compare to the dispersibility of embodiment 1-3 and existing product:
| Product | Dispersed (being tested under equal conditions) |
| Embodiment 1 | 3.67mPa.s |
| Embodiment 2 | 3.62mPa.s |
| Embodiment 3 | 3.69mPa.s |
| Existing product | 343mPa.s |
From upper table as it can be seen that nano-titanium dioxide dispersibility prepared by the present invention is substantially better than existing product.
Sulfuric acid reaction of the barium nitrate with free sulfuric acid and in conjunction with titanium generates barium sulfate precipitate in the present invention, reduces titanium dioxide
Active force between titanium molecule is completely dispersed the titania molecule reunited, and dissolves part insoluble matter in the presence of nitric acid
Reduce impurity；Barium carbonate itself directly and effect of sulfuric acid, and cannot generate barium nitrate and titanium dioxide with nitric acid reaction as precipitating
Titanium gas, the reaction was continued for barium nitrate.Why the molar ratio of barium nitrate and barium carbonate is set as 0.6:0.4, is because if nitre
Sour barium content is low, and reaction is not thorough, and content height is then acid low, and the acid low easy gel of sample.Filtrate conductivity in step (2)
≤ 3500us/cm is that then impurity content is high because of conductivity height, and impurity content height continues to wash energy consumption height.
Claims (1)
1. the method for preparing nano-titanium dioxide using metatitanic acid, it is characterized in that it is the following steps are included: (1), dispergation: control is inclined
Content of titanium dioxide 15wt%-30wt% in metatitanic acid successively adds 60% barium nitrate of molar ratio stirring half an hour and 40% carbon of molar ratio
Sour barium stirs half an hour；(2), washing purifying: washing purifying is carried out to TiO 2 sol using ultrafiltration membrane system, by continuous
The mode for supplementing desalted water substitution aqueous solution, controls filtrate conductivity≤3500us/cm；(3), be spray-dried: washing is after purification
TiO 2 sol remove moisture removal by the way of spray drying, 300 DEG C -400 DEG C of drying temperature；(4), it calcines: after dry
Titanium dioxide 500 DEG C -800 DEG C calcining, control specific surface area；(5), it crushes: to forging by the way of high pressure draught crushing
Sample comminution after burning, stream pressure 1MPa.
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| CN201910369590.8A CN110040774B (en) | 2019-05-06 | 2019-05-06 | Method for preparing nano titanium dioxide by using metatitanic acid |
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| CN201910369590.8A CN110040774B (en) | 2019-05-06 | 2019-05-06 | Method for preparing nano titanium dioxide by using metatitanic acid |
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| CN110040774B CN110040774B (en) | 2022-10-21 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112707556A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Titanium-containing waste liquid treatment method and titanium-containing dry powder |
| 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 |
-
2019
- 2019-05-06 CN CN201910369590.8A patent/CN110040774B/en active Active
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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112707556A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Titanium-containing waste liquid treatment method and titanium-containing dry powder |
| 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 |
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| CN110040774B (en) | 2022-10-21 |
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