CN101696031A - Method for preparing nano titanium dioxide powder by using industrial titanium liquid - Google Patents
Method for preparing nano titanium dioxide powder by using industrial titanium liquid Download PDFInfo
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- CN101696031A CN101696031A CN200910193482A CN200910193482A CN101696031A CN 101696031 A CN101696031 A CN 101696031A CN 200910193482 A CN200910193482 A CN 200910193482A CN 200910193482 A CN200910193482 A CN 200910193482A CN 101696031 A CN101696031 A CN 101696031A
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Abstract
The invention discloses a method for preparing nano titanium dioxide powder by using industrial titanium liquid, which specifically comprises the following steps: diluting the industrial titanium liquid by 1.5 to 30 times by adding water, then adding an acid scavenger accounting for 0.1 to 15 percent of the total diluted liquid in percentage by mass into the diluted liquid, and centrifugalizing the diluted liquid to obtain low-acidity titanium liquid; putting the obtained low-acidity titanium liquid into a reactor, and then adding acid accounting for 0.1 to 5 percent of the volume of low-acidity titanium liquid and 0.05 to 5 mass percent dispersant into the liquid; and mixing the mixture evenly, then reacting the mixture for 0.5 to 10 hours at a temperature of between 25 and 100 DEG C, separating and washing a product, and drying the product at the temperature of between 40 and 150 DEG C to obtain the nano titanium dioxide powder. The method has the advantages that the nano titanium dioxide powder with good crystallinity and even particle size distribution can be prepared without high temperature, the process equipment is simple, and the production cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic nano material, being specifically related to a kind of is raw material directly prepares nano titanium oxide by chemical process novel method with titanium white commercial titanium liquid directly.
Background technology
Along with the rise and the Development of Preparation Technology of nano material, nano titanium oxide (TiO
2) be different from the performance of conventional powder body material, as: as catalyzer degradable organic pollutant under ultraviolet irradiation, conversion solar can be electric energy, is used for transmitter, the enhancement additive of polymkeric substance, complex function ceramic material, and antibiotic, glass with clean etc. makes TiO
2Become the focus of research once more.TiO
2There are three kinds of crystal habits at occurring in nature: rutile-type, Detitanium-ore-type and brookite type, wherein, Detitanium-ore-type TiO
2Because of the photocatalysis performance height, and be widely used as the raw material of antibiotic paper, wastewater treatment and environmental improvement etc.
Adopt cheapness, the simple preparation method of technology to obtain high performance nano-TiO
2, be suitability for industrialized production nano-TiO now
2The major objective of being pursued.Prepare nano-TiO at present
2The most frequently used raw material is titanium alkoxide, titanium tetrachloride (TiCl
4) and titanyl sulfate (TiOSO
4), the titanium liquid raw material that produces in the titanium white industrial production is easy to get, and with its basic raw material as the preparation nano titanium oxide, has the favorable industrial application prospect.
Traditional preparation process TiO
2Can the method for nano material generally need could obtain crystal formation through pyroprocessing more than 500 ℃, has shortcomings such as preparation process temperature height, energy consumption are big, therefore prepare TiO under low temperature or normal temperature
2Nano material is the inexorable trend studied from now on and the inevitable direction of development.Synthetic crystalline state nano-TiO in the liquid phase
2Powder has that temperature of reaction is low, equipment is simple, easy to operate, low cost and other advantages, is the preparation nano-TiO of present laboratory and industrial tool application prospect
2The method of powder has become nano-TiO
2One of research focus of preparation field.At present research emphasis is how to improve the purity of product, control particle diameter uniform distribution, research crystal with controllable crystal forms synthetic rule and mechanism, development quantity-produced method and raise the efficiency etc.We believe that the method for the synthetic crystalline state nanometer Ti of liquid phase will be accepted by suitability for industrialized production, and brings huge economic benefit thus if relevant research can have breakthrough in purification of products, crystal formation control and aspect such as reduce cost.
Summary of the invention
The objective of the invention is shortcoming and defect, proposed a kind of preparation method of nano-titanium dioxide powder at above-mentioned prior art.
The present invention adopts following technical scheme to realize above-mentioned purpose:
A kind ofly prepare the method for nano-titanium dioxide powder, may further comprise the steps with commercial titanium liquid:
(1) doubly, total liquid mass per-cent was the acid scavenger of 0.1%-15% after adding accounted for and dilutes again, and back centrifugation obtains to hang down acidity titanium liquid with commercial titanium liquid thin up 1.5-30;
(2) the low acidity titanium liquid that obtains of step (1) places reactor, and adding acid and the mass percent that to account for the long-pending per-cent of low acidity titanium liquid be 0.1%-5% again is the dispersion agent of 0.05%-5%; Mix, then 25-100 ℃ of reaction, the reaction times is 0.5-10h, and resultant is after separating, washing, and drying obtains nano-titanium dioxide powder under 40-150 ℃ of condition.
In the above-mentioned method, the main component that the described commercial titanium liquid of step (1) contains is titanyl sulfate, chlorination oxygen titanium, titanium sulfate, titanium tetrachloride and titanium alkoxide.
In the above-mentioned method, the acid scavenger of step (1) comprises more than one in sodium bicarbonate, lime carbonate, barium carbonate, the yellow soda ash.
In the above-mentioned method, the described acid of step (2) is more than one in concentrated nitric acid, concentrated hydrochloric acid, phosphoric acid, sulfuric acid, acetate, the diacetyl oxide.
In the above-mentioned method, the described dispersion agent of step (2) comprises more than one in ethanol, ethylene glycol, glycerol, Polyethylene Glycol-600, polyoxyethylene glycol-2000, polyethylene glycol 6000, the cetomacrogol 1000 0.
The present invention compared with prior art has following advantage and useful effect:
(1) nano titanium oxide of the present invention's preparation is to finish under the low temperature liquid phase condition, this method reaction conditions gentleness, and not high to equipment requirements, the product of preparing is good, has good industrial prospect.
(2) product that obtains of the present invention need not the nano titanium oxide calcining back particulate that calcination avoids preparing and reunites, and can prepare the nano titanium oxide of good dispersity.
(3) the commercial titanium liquid that the present invention utilized is the titanium liquid that titanium powder plant is produced titanium dioxide, and the source is enriched and along with the mass-producing of producing becomes cheap day by day, helped large-scale industrial production of the present invention.
Description of drawings
The high resolving power transmission electron microscope picture of the nano titanium oxide that Fig. 1 prepares for embodiment.
The scanning electron microscope Electronic Speculum figure of the nano titanium oxide that Fig. 2 prepares for embodiment.
Embodiment
Below in conjunction with specific examples concrete enforcement of the present invention is described in further detail, but enforcement of the present invention is not limited thereto.
Embodiment 1:
(1) get commercial titanium liquid 50ml, 5 times of thin ups, the mass percent that adds sodium bicarbonate is 0.2%, back centrifugation obtains to hang down the titanium liquid of acidity;
(2) mixture powder that obtains of step (1) is in reactor, adds volume percent again and be 2.0% nitric acid and mass percent and be 2.0% ethylene glycol; Mix, be added in 60 ℃ of reactions then, the reaction times is 1h, resultant through separate, drying obtains nano-titanium dioxide powder under the washing, 60 ℃ of conditions;
Embodiment 2:
(1) get commercial titanium liquid 10ml, 10 times of thin ups, the mass percent that adds lime carbonate is 1.0%, back centrifugation obtains to hang down the titanium liquid of acidity
(2) mixture powder that obtains of step (1) is in reactor, adds volume percent again and be 4.0% acetic acid and mass percent and be 2.6% ethanol; Mix, be added in 50 ℃ of reactions then, the reaction times is 1.2h, resultant through separate, drying obtains nano-titanium dioxide powder under the washing, 30 ℃ of conditions;
Embodiment 3:
(1) get commercial titanium liquid 70ml, 20 times of thin ups, the mass percent that adds barium carbonate is 0.5%, back centrifugation obtains to hang down the titanium liquid of acidity
(2) mixture powder that obtains of step (1) is in reactor, adds volume percent again and be 2.0% hydrochloric acid and mass percent and be 2.0% glycerol; Mix, be added in 60 ℃ of reactions then, the reaction times is 1h, resultant through separate, drying obtains nano-titanium dioxide powder under the washing, 60 ℃ of conditions;
Embodiment 4:
(1) get commercial titanium liquid 30ml, 12 times of thin ups, the mass percent that adds yellow soda ash is 0.5%, back centrifugation obtains to hang down the titanium liquid of acidity
(2) mixture powder that obtains of step (1) is in reactor, adds volume percent again and be 2.5% diacetyl oxide and mass percent and be 3.2% polyoxyethylene glycol-10000; Mix, be added in 40 ℃ of reactions then, the reaction times is 0.5h, resultant through separate, drying obtains nano-titanium dioxide powder under the washing, 45 ℃ of conditions;
Prepared the byproduct that titanium liquid that nano titanium oxide obtains produced and can be used for other chemical industries, the device of the low temperature of employed nano titanium oxide preparation is bought outside can be on market in the technology.
Fig. 1 and Fig. 2 are respectively the high resolving power transmission electron microscope picture and the sem photographs of embodiment 2 resulting nano titanium oxides, spheric titanium dioxide nanoparticle as can be seen from Figure 1, the lattice of nano titanium oxide is high-visible, spacing of lattice is 0.351nm, is 101 lattice width of anatase-type nanometer titanium dioxide.The distribution of the spheroidal particle of nano titanium oxide is high-visible as can be seen from Figure 2, the about 60nm of aggregate particle size, and visible low temperature method of the present invention can be prepared advantages of good crystallization, the nano titanium oxide that is evenly distributed.
Claims (5)
1. one kind prepares the method for nano-titanium dioxide powder with commercial titanium liquid, it is characterized in that may further comprise the steps:
(1) doubly, total liquid mass per-cent was the acid scavenger of 0.1%-15% after adding accounted for and dilutes again, and back centrifugation obtains to hang down acidity titanium liquid with commercial titanium liquid thin up 1.5-30;
(2) the low acidity titanium liquid that obtains of step (1) places reactor, and adding acid and the mass percent that to account for the long-pending per-cent of low acidity titanium liquid be 0.1%-5% again is the dispersion agent of 0.05%-5%; Mix, then 25-100 ℃ of reaction, the reaction times is 0.5-10h, and resultant is after separating, washing, and drying obtains nano-titanium dioxide powder under 40-150 ℃ of condition.
2. method according to claim 1 is characterized in that, the main component that the described commercial titanium liquid of step (1) contains is titanyl sulfate, chlorination oxygen titanium, titanium sulfate, titanium tetrachloride and titanium alkoxide.
3. method according to claim 1 is characterized in that, the acid scavenger of step (1) comprises more than one in sodium bicarbonate, lime carbonate, barium carbonate, the yellow soda ash.
4. method according to claim 1 is characterized in that, the described acid of step (2) is more than one in concentrated nitric acid, concentrated hydrochloric acid, phosphoric acid, sulfuric acid, acetate, the diacetyl oxide.
5. according to each described method of claim 1～4, it is characterized in that the described dispersion agent of step (2) comprises more than one in ethanol, ethylene glycol, glycerol, Polyethylene Glycol-600, polyoxyethylene glycol-2000, polyethylene glycol 6000, the cetomacrogol 1000 0.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844805A (en) * | 2010-06-08 | 2010-09-29 | 上海工程技术大学 | Method for preparing aqueous high-dispersion nano titanium dioxide |
| CN101973580A (en) * | 2010-09-10 | 2011-02-16 | 西昌新钒钛有限公司 | Method for preparing high-purity titanium pigment by using high-purity water |
| CN102515763A (en) * | 2011-11-10 | 2012-06-27 | 哈尔滨工业大学 | Preparation method for perovskite structural ceramic sol |
| CN104479208A (en) * | 2014-12-24 | 2015-04-01 | 东莞市迪彩塑胶五金有限公司 | Ti-PO4-PEG flame retardant, flame retardant composite thereof and preparation methods |
| RU2576054C1 (en) * | 2014-09-19 | 2016-02-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный университет тонких химических технологий имени М.В. Ломоносова" (МИТХТ им. М.В. Ломоносова) | METHOD OF OBTAINING η-TiO2 NANOSIZED MODIFICATION |
| CN107697948A (en) * | 2017-11-21 | 2018-02-16 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of titanium sulfate liquid high-efficient purification |
| WO2022007763A1 (en) * | 2020-07-06 | 2022-01-13 | 宁波极微纳新材料科技有限公司 | Preparation method for titanium dioxide material |
-
2009
- 2009-10-30 CN CN200910193482A patent/CN101696031A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844805A (en) * | 2010-06-08 | 2010-09-29 | 上海工程技术大学 | Method for preparing aqueous high-dispersion nano titanium dioxide |
| CN101973580A (en) * | 2010-09-10 | 2011-02-16 | 西昌新钒钛有限公司 | Method for preparing high-purity titanium pigment by using high-purity water |
| CN102515763A (en) * | 2011-11-10 | 2012-06-27 | 哈尔滨工业大学 | Preparation method for perovskite structural ceramic sol |
| CN102515763B (en) * | 2011-11-10 | 2013-05-22 | 哈尔滨工业大学 | Preparation method for perovskite structural ceramic sol |
| RU2576054C1 (en) * | 2014-09-19 | 2016-02-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный университет тонких химических технологий имени М.В. Ломоносова" (МИТХТ им. М.В. Ломоносова) | METHOD OF OBTAINING η-TiO2 NANOSIZED MODIFICATION |
| CN104479208A (en) * | 2014-12-24 | 2015-04-01 | 东莞市迪彩塑胶五金有限公司 | Ti-PO4-PEG flame retardant, flame retardant composite thereof and preparation methods |
| CN107697948A (en) * | 2017-11-21 | 2018-02-16 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of titanium sulfate liquid high-efficient purification |
| WO2022007763A1 (en) * | 2020-07-06 | 2022-01-13 | 宁波极微纳新材料科技有限公司 | Preparation method for titanium dioxide material |
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Open date: 20100421 |