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Preparation method of anatase phase mesohole nano-titanium dioxide powder

A technology of nano-titanium dioxide and anatase phase, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of reducing the specific surface area of ​​nano-materials, having no catalytic activity, and the collapse of porous structures, so as to achieve broad application prospects and low energy consumption. And the effect of low cost and favorable low temperature formation

Active Publication Date: 2007-02-07
湖北铁神新材料有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

However, the porous TiO prepared by the surfactant template method 2 It is usually an amorphous structure without catalytic activity, which will lead to the collapse of the porous structure during its crystallization into anatase, which greatly reduces the specific surface area of ​​nanomaterials
Therefore, currently domestic and foreign research on nano-TiO with crystallized anatase mesoporous structure 2 not published or used

Method used

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preparation example Construction

[0025] The preparation process of the present invention is as follows:

[0026]

[0027] The basic steps are: weigh titanium sulfate and alkyl primary amine hydrochloride, add ethanol under magnetic stirring, and then add water; secondly, adjust the pH of the solution, and age at room temperature; thirdly, seal the reaction vessel with adhesive tape, 100-110 Continue to age at ℃; the fourth is to remove the template agent with saturated ethanol solution of sodium chloride after centrifugation and washing; the fifth is to heat treat at different temperatures after washing and drying.

[0028] The specific implementation method of preparing a kind of anatase phase mesoporous nano titanium dioxide powder is as follows:

[0029] (1) Weigh 1.6-1.8g of titanium sulfate [Ti(SO 4 ) 2 ] and 1.1-1.3g alkylamine hydrochloride (or by Ti: primary amine molar ratio is 2: 1 or 1: 1, take dodecylamine hydrochloride or stearylamine hydrochloride respectively);

[0030] (2) Place the abov...

Embodiment 1

[0038] Embodiment 1: take by weighing 1.7600g Ti(SO 4 ) 2 and 1.2172g of dodecylamine hydrochloride, add 20ml of ethanol under magnetic stirring, after stirring for 10min, then slowly add 20ml of secondary water, and stir for 30min. Aging at room temperature for 48 hours. Then it was sealed with adhesive tape and aged at 100°C for 48 hours. After cooling, centrifuge and wash twice with water until 2% barium nitrate [Ba(NO 3 ) 2 ] detected to no SO 4 2- , washed with ethanol and dried. Remove the template agent with saturated ethanol solution of sodium chloride, wash with secondary water and ethanol again, and dry.

[0039] Calcined at 300°C for 2 hours, the morphology of the obtained product is shown in figure 1 with figure 2 , the particle distribution is relatively uniform, the average particle size is 25nm, the average pore size is 3.3nm, the average grain size is 3.9nm, and the specific surface area is 212m 2 / g, the degree of crystallization of the pore wall is...

Embodiment 2

[0040] Embodiment 2: take by weighing 1.7600g Ti(SO 4 ) 2 and 3.3605g of octadecylamine hydrochloride, add 20ml of ethanol under magnetic stirring, after stirring for 10min, slowly add 20ml of secondary water, and stir for 30min. Aging at room temperature for 48 hours. Then it was sealed with adhesive tape and aged at 100°C for 48 hours. After cooling, centrifuge and wash twice with water until 2% barium nitrate [Ba(NO 3 ) 2 ] detected to no SO 4 2- , washed with ethanol and dried. Remove the template agent with saturated ethanol solution of sodium chloride, wash with water and ethanol twice, and dry.

[0041] Calcined at 300°C for 2 hours, the particle distribution of the product obtained is relatively uniform, the average particle size is 38.3nm, the average pore size is 5.0nm, the average grain size is 3.4nm, and the specific surface area is 296.6m 2 / g, the degree of crystallization of the pore wall is higher. Calcined at 400°C for 2 hours, the particle distributi...

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Abstract

A process for preparing anatase-type mesoporous TiO2 nanoparticles includes such steps as proportionally adding titanium sulfate and alkyltriamine hydrochloride to alcohol while magnetic stirring, adding water, regulating pH value, ageing, sealing, ageing at 100 deg.C, centrifugal separation, washing, removing template agent by saturated alcohol solution of sodium chloride, washing, drying and heat treating at different temps.

Description

technical field [0001] The invention relates to the field of fine chemical industry, and more specifically relates to a preparation method of anatase-phase mesoporous nano-titanium dioxide powder, which has broad application prospects in the fields of photocatalytic degradation of pollutants, photoelectrochemical cells, and hydrogen production by photolysis of water. This method can be used to prepare nano-titanium dioxide powder with high thermal stability, high specific surface area and highly crystallized anatase pore wall. Background technique [0002] Nano titanium dioxide (TiO 2 ) refers to titanium dioxide products with a particle size of less than 100 nanometers. Due to its small particle size and large specific surface area, it has high chemical activity and is widely used in chemical production, photoelectrochemical conversion, photocatalysis and other fields. Currently preparing TiO 2 The method generally uses TiCl 4 Hydrolysis or high temperature annealing met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047C01G23/053
Inventor 彭天右戴珂
Owner 湖北铁神新材料有限公司
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