CN1076319C - Method for preparing nanometre-grade titanium dioxide - Google Patents
Method for preparing nanometre-grade titanium dioxide Download PDFInfo
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- CN1076319C CN1076319C CN97108439A CN97108439A CN1076319C CN 1076319 C CN1076319 C CN 1076319C CN 97108439 A CN97108439 A CN 97108439A CN 97108439 A CN97108439 A CN 97108439A CN 1076319 C CN1076319 C CN 1076319C
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Abstract
The present invention discloses a novel method for preparing nanometer titanium dioxide, particularly a novel method using a homogeneous precipitation method to prepare nanometer titanium dioxide. The present invention is characterized in that H2TiO3 is used as a raw material; urea is used as a uniform precipitating agent; the concentration of reactant is 1.44*10<-3>g/l; the ratio of the amount of substance of the urea to TiOSO4 is from 1: 1 to 5: 1; the temperature of the hydrolysis reaction of the urea is from 95 to 110 DEG C; the reaction time is from 2.0 to 4.0 hr; and TiO (OH) 2 as synthesized intermediate sedimentation is calcined for 2.5 to 3.5 hr under 800 to 1000 DEG C to obtain the nanometer TiO2. The method has the advantages of simple production process, convenient industrialization production and broad application prospect.
Description
The invention discloses a method for preparing nano-titanium dioxide, in particular to a method for preparing nano-titanium dioxide by using a uniform precipitation method.
Nano TiO 22Is an important inorganic functional material with the size about that of common TiO2About 1/10, the particle size is usually 1 to 100 nm. The particle size is miniaturized, so that the nano TiO2The surface effect, small-size effect, quantum effect and macroscopic quantum tunneling effect which are not possessed by the bulk material are generated, so that the material has the advantages of good weather resistance, chemical corrosion resistance, strong ultraviolet resistance, excellent transparency, uniform particle size distribution, good dispersibility and the like. Nano TiO 22Besides the basic properties of the nano material, the nano material also has the relative stability of physical properties and chemical properties, nontoxicity, non-migration, photoconductivity, photocatalysis and color effect, has transparency and ultraviolet scattering capability, and can be used for automobile finish, photosensitive materials, photocatalysts, cosmetics, food packaging materials, ceramic additives, gas sensors, temperature sensors, magnetic recording materials and the like. Domestic and overseas synthesis of nano TiO2The methods of (1) mainly include a sol-gel method (S-G method), a vapor phase method (CVD method) and a peptization method. S-G method using hydrolysis and polycondensation of metal alkoxide as an effective method for preparing nano-powder, TiO with good uniformity has been synthesized2Gel and nano TiO2Particles, but this method is costly. The CVD method has high requirements on technology and material, complex process and large investment. In comparison, the peptization method has much simpler process, but has the defect that the raw material is reagent-grade TiOSO4Or Ti (SO)4)2The source is less and the price is not very expensive.
The invention aims to provide a method which has low production cost and simple production process and is convenient for industrialized production of nano-scale so as to overcome the defects of the prior art.
The invention is realized as follows: the following details the use ofPreparation of nano-grade TiO by homogeneous precipitation method2The production process of (1).
1. The preparation principle is as follows:
the homogeneous precipitation method is a method in which a precipitant added to a solution does not react with a component to be precipitated immediately but is slowly generated in the whole solution by a chemical reaction, so that a crystal-forming ion in the solution is slowly and uniformly released from the solution by the chemical reaction. Therefore, as long as the speed of generating the precipitant is controlled, the phenomenon of uneven concentration can be avoided, and the supersaturation degree is controlled within a proper range, so that the growth speed of the particles is controlled, and the nano-scale particles with uniform and compact particle size, convenient washing and high purity are obtained.
With H2TiO3Preparing nano TiO by using urea as uniform precipitant2The reaction equation of (a) is as follows:
2. the preparation conditions are as follows:
the invention adopts urea as a precipitator, the hydrolysis speed of the urea is the key for determining the grain diameter of ultrafine grains and the product yield, the temperature is higher than 130 ℃, the urea can generate isomerization condensation, and the optimal reaction temperature is 95-110 ℃. Since the urea hydrolysis rate increases with increasing residence time, a certain reaction time, preferably 2.5-4.0hr, when TiOSO is used, must be maintained to obtain a high product yield4At a constant concentration, urea/TiOSO4The larger the ratio (amount of substance) is, the OH in the solution-The larger the concentration, the larger the supersaturation, and the more favorable the formation of a precipitate having a small particle size. At the same time, the excessive urea can ensure TiOSO in a certain time4And (4) fully reacting. Urea and TiOSO4The optimal material quantity ratio is 1: 1-51. In dilute TiOSO4At the concentration, the urea hydrolysis rate is high, but the crystallization product is easy to grow into small and large crystal grains. Therefore, the concentration of the solution should not be too low or too high. TiOSO4The optimal concentration is 1.44 × 10-3g/l. Calcining at 800-850 ℃ to obtain anatase TiO2Calcining at 850-950 ℃ to obtain mixed crystal TiO2Calcining at 950-1000 deg.C to obtain rutile-type TiO2. The calcination time is preferably 2.5 to 4.0 hr. The invention has the advantages that: nano TiO prepared by uniform precipitation method2Uniform granularity, good dispersity and greatly reduced nano TiO2The cost (about 1/3-1/4 of the cost of the S-G method and the CVD method) is reduced, and the production process is simpler and is convenient for industrial production.
Two embodiments of the invention:
1. according to the ratio of urea to H2TiO3The two raw materials are respectively weighed according to the mass ratio of 5: 1, and are added into the mixture H2TiO3Adding H2SO4Heating the solution to complete the reaction, adding urea to the solutionAdding distilled water to make TiOSO4The concentration is 1.44X 10-3g/l, reaction at 95 ℃ for 3hr to obtain TiO (OH)2Precipitating, filtering, washing, drying, calcining at 800 deg.C for 2.5hr to obtain nanometer TiO2The yield was 80.36%, and the average particle diameter was 30 nm.
2. According to the ratio of urea to H2TiO3The two raw materials are respectively weighed according to the mass ratio of 5: 1, and are added into the mixture H2TiO3Adding H2SO4Heating the solution to complete the reaction, adding urea into the solution, and adding distilled water to make TiOSO4The concentration is 1.44X 10-3g/1, reaction at 95 ℃ for 3hr to obtain TiO (OH)2Precipitating, filtering, washing, drying, calcining at 950 deg.C for 3hr to obtain nanometer TiO2The yield was 91.40%, and the average particle diameter was 45 nm.
Claims (2)
1. A kind ofThe method for preparing the nano titanium dioxide by using the uniform precipitation method is characterized by comprising thefollowing steps: with H2TiO3And H2SO4TiOSO produced by the reaction4As raw material, urea as homogeneous precipitant, wherein TiOSO is controlled4The concentration is 1.44X 10-3g/l, amount of urea and TiOSO4The mass ratio of the components is 1: 1-5: 1, the reaction temperature is 95-110 ℃, the reaction time is 2.5-4.0hr, and TiO (OH) is generated2(ii) a And the intermediate precipitate TiO (OH) synthesized2Calcining at 800-1000 deg.C for 2.5-3.5hr to obtain nanometer TiO2。
2. The method for producing nano-sized titanium dioxide according to claim 1, wherein: calcining at 800-850 ℃ to obtain anatase TiO2Calcining at 850-950 ℃ to obtain mixed crystal TiO2Calcining at 950-1000 deg.C to obtain rutile-type TiO2。
Priority Applications (1)
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CN97108439A CN1076319C (en) | 1997-03-06 | 1997-03-06 | Method for preparing nanometre-grade titanium dioxide |
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CN97108439A CN1076319C (en) | 1997-03-06 | 1997-03-06 | Method for preparing nanometre-grade titanium dioxide |
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CN1192992A CN1192992A (en) | 1998-09-16 |
CN1076319C true CN1076319C (en) | 2001-12-19 |
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Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1086364C (en) * | 1999-05-12 | 2002-06-19 | 中国科学院上海硅酸盐研究所 | Process for preparing titanic schorl phase titanium dioxide nanometer crystal under room temp. |
FR2803223B1 (en) * | 1999-12-30 | 2002-06-21 | Rhodia Chimie Sa | PROCESS FOR THE PREPARATION OF A MESOSTRUCTURE MATERIAL FROM PARTICLES OF NANOMETRIC DIMENSIONS |
CN100368301C (en) * | 2005-09-13 | 2008-02-13 | 山东轻工业学院 | Mesoporous nanopowder titanium dioxide bionic synthesis method |
CN100391852C (en) * | 2006-03-03 | 2008-06-04 | 河北大学 | Method for preparing hano-level titanium dioxide by controlling crystal form |
CN101654280B (en) * | 2009-08-25 | 2011-04-13 | 苏州大学 | Preparation method of titanium dioxide nano powder |
CN104649317A (en) * | 2015-01-13 | 2015-05-27 | 漯河兴茂钛业股份有限公司 | Special nano titanium dioxide for flue gas denitration catalysts and preparation method thereof |
CN111233033B (en) * | 2020-03-26 | 2021-01-01 | 华东理工大学 | Process method for regulating particle size of titanium dioxide |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS6065725A (en) * | 1983-09-20 | 1985-04-15 | Fuji Titan Kogyo Kk | Preparation of spherical particles of titania |
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JPS6065725A (en) * | 1983-09-20 | 1985-04-15 | Fuji Titan Kogyo Kk | Preparation of spherical particles of titania |
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