Method for preparing medium pore molecular sieve of titanium dioxide

Abstract

The method for preparing nano titanium dioxide metaporous material includes the following steps: mixing titanium source and triethanolamine at room temp., uniformly stirring them, drop-adding one of water, propanetriol, glycol and ethyl alcohol as solvent, regulating pH value and making it be 7-9; drying for 2-48 hr, at 25 deg.C-180 deg.C to form homogeneous gel, making crystallization for 12-96 hr, at 25-180 deg.C in a closed reactor, heating to 300-800 deg.C, heat-insulating for 10-20 hr, or using alcohol solution to extract for 24-72 hr, and grinding so as to obtain the titanium dioxide metaporous molecular sieve.

Description

technical field

[0001] The invention relates to a preparation method of titanium dioxide material, in particular to a preparation method of nanometer titanium dioxide mesoporous material. Background technique

[0002] Porous materials have a wide range of applications in catalytic separation and other fields. Compared with classical microporous molecular sieves, mesoporous molecular sieves have larger pore size and specific surface area. As catalysts or catalyst supports, mesoporous molecular sieve materials provide favorable spatial configuration and type-selective active centers for organic macromolecules to participate in reactions, and have potential application advantages in petroleum processing or fine chemical industry.

[0003] Transition metal oxides have special properties, and transition metal oxides with various mesoporous structures have received unprecedented attention in recent years. Titanium dioxide is a non-toxic and harmless semiconductor. It can generat...

Examples

Embodiment 1

[0031] Mix 12ml tetrabutyl titanate and 4.7ml triethanolamine at room temperature, stir evenly, add 16ml water dropwise and measure the pH value to 8, continue stirring to obtain a homogeneous mixture, dry the above homogeneous mixture at 100°C for 12 hours and then solidify A homogeneous gel is formed, and then the gel is moved into a reaction kettle and crystallized at 150°C for 12 hours to obtain a block gel, and then the above product is calcined at a rate of 1°C / min to 600°C, Insulated for 10 hours, ground to obtain a white powder, its XRD diffraction pattern is as follows figure 1 As shown, the pore size distribution is as figure 2 as shown in a.

Embodiment 2

[0033] Mix 12ml tetrabutyl titanate and 4.7ml triethanolamine at room temperature, stir evenly, add 16ml water dropwise and measure the pH value to 8, continue stirring to obtain a homogeneous mixture, dry the above homogeneous mixture at 100°C for 12 hours and then solidify A homogeneous gel was formed, and then the gel was transferred into a reaction kettle for crystallization at a temperature of 150° C. for 48 hours to obtain a block gel that was equally divided into three parts. Extracted with a Soxhlet extractor for 24 hours, 48 ​​hours, and 72 hours, the extract was ethanol solution, and the obtained massive gel was ground into powder, and the product pore size distribution obtained by extraction for 24 hours was as follows: figure 2 as shown in b.

Embodiment 3

[0035] Mix 3.4ml tetrabutyl titanate and 6.7ml triethanolamine at room temperature, stir evenly, add 18ml water dropwise and measure the pH value to be 8, continue stirring to obtain a homogeneous mixture, dry the above homogeneous mixture at 180°C for 2 hours Solidify to form a homogeneous gel, then move the gel into the reaction kettle and crystallize at 180°C for 48 hours to obtain a block gel; then heat the above product at a rate of 5°C / min to 400°C after calcination , kept warm for 10 hours, and ground to obtain a white powder. Its XRD diffraction pattern is as image 3 as shown in a.

technical field

[0001] The invention relates to a preparation method of titanium dioxide material, in particular to a preparation method of nanometer titanium dioxide mesoporous material. Background technique

[0002] Porous materials have a wide range of applications in catalytic separation and other fields. Compared with classical microporous molecular sieves, mesoporous molecular sieves have larger pore size and specific surface area. As catalysts or catalyst supports, mesoporous molecular sieve materials provide favorable spatial configuration and type-selective active centers for organic macromolecules to participate in reactions, and have potential application advantages in petroleum processing or fine chemical industry.

[0003] Transition metal oxides have special properties, and transition metal oxides with various mesoporous structures have received unprecedented attention in recent years. Titanium dioxide is a non-toxic and harmless semiconductor. It can generat...

Examples

Embodiment 1

[0031] Mix 12ml tetrabutyl titanate and 4.7ml triethanolamine at room temperature, stir evenly, add 16ml water dropwise and measure the pH value to 8, continue stirring to obtain a homogeneous mixture, dry the above homogeneous mixture at 100°C for 12 hours and then solidify A homogeneous gel is formed, and then the gel is moved into a reaction kettle and crystallized at 150°C for 12 hours to obtain a block gel, and then the above product is calcined at a rate of 1°C / min to 600°C, Insulated for 10 hours, ground to obtain a white powder, its XRD diffraction pattern is as follows figure 1 As shown, the pore size distribution is as figure 2 as shown in a.

Embodiment 2

[0033] Mix 12ml tetrabutyl titanate and 4.7ml triethanolamine at room temperature, stir evenly, add 16ml water dropwise and measure the pH value to 8, continue stirring to obtain a homogeneous mixture, dry the above homogeneous mixture at 100°C for 12 hours and then solidify A homogeneous gel was formed, and then the gel was transferred into a reaction kettle for crystallization at a temperature of 150° C. for 48 hours to obtain a block gel that was equally divided into three parts. Extracted with a Soxhlet extractor for 24 hours, 48 ​​hours, and 72 hours, the extract was ethanol solution, and the obtained massive gel was ground into powder, and the product pore size distribution obtained by extraction for 24 hours was as follows: figure 2 as shown in b.

Embodiment 3

[0035] Mix 3.4ml tetrabutyl titanate and 6.7ml triethanolamine at room temperature, stir evenly, add 18ml water dropwise and measure the pH value to be 8, continue stirring to obtain a homogeneous mixture, dry the above homogeneous mixture at 180°C for 2 hours Solidify to form a homogeneous gel, then move the gel into the reaction kettle and crystallize at 180°C for 48 hours to obtain a block gel; then heat the above product at a rate of 5°C / min to 400°C after calcination , kept warm for 10 hours, and ground to obtain a white powder. Its XRD diffraction pattern is as image 3 as shown in a.

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