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Mesopore titanium dioxide and its SO42-/TiO2 solid super strong acid preparation method and SO42-/TiO2 solid super strong acid

A technology of mesoporous titanium dioxide and metatitanic acid, which is applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of expensive polymer polyether surfactants, poor thermal stability of mesoporous materials, and lack of economical competitive advantages. , to achieve excellent thermal stability, low cost and good catalytic activity

Inactive Publication Date: 2010-02-24
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, no matter whether a polymer polyether surfactant or a cationic surfactant is used as the template formed by the mesoporous precursor, the mesoporous structure of titanium dioxide is easy to collapse during the process of removing the template agent in the precursor to form pores; The titanium dioxide-based mesoporous materials obtained by this method have poor thermal stability, and in order to avoid structural collapse, the removal of the template agent is not complete, which limits the practical application of such materials.
[0005] In addition, there are few reports on the synthesis of mesoporous titania-based superacids. For example, the patent application with publication number CN1395995A uses polymer polyether surfactants, including P123, P84, and P65, as template preparation methods to synthesize a series of mesoporous Super acid material, the specific surface area can reach 200m 2 / g, but the polymer polyether surfactant used in this method is expensive and has limited sources, so it does not have a competitive advantage economically

Method used

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  • Mesopore titanium dioxide and its SO42-/TiO2 solid super strong acid preparation method and SO42-/TiO2 solid super strong acid
  • Mesopore titanium dioxide and its SO42-/TiO2 solid super strong acid preparation method and SO42-/TiO2 solid super strong acid
  • Mesopore titanium dioxide and its SO42-/TiO2 solid super strong acid preparation method and SO42-/TiO2 solid super strong acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] In the first step of hydrolysis, 200ml of industrial titanium sulfate solution and 20ml of water are mixed into a homogeneous solution, and then hydrolyzed in a reactor at 90°C for 30 minutes; then the second step is carried out to hydrolyze 1 / 10 (volume) is quickly added to another reactor filled with 100ml boiling water and stirred quickly, and the gray point appears in about 30s. At this time, the remaining industrial titanium sulfate solution that has been hydrolyzed in the first step is 9 / 10 volume and preheated 120ml of water was added in parallel, and the feeding time was about 15 minutes. The reaction is carried out in a boiling state for 2h, aging for 6h, and liquid-solid separation is carried out after cooling, and the hydrolysate is obtained by adsorbing a large amount of Fe 2+ And SO 4 2- Mesoporous structure of metatitanic acid, washed with deionized water at 80℃ ultrasonically, to remove Fe contained in metatitanic acid 2+ And SO 4 2 , Until the color of th...

Embodiment 2～6

[0049] Change the water / titanium liquid ratio and the hydrolysis temperature in the hydrolysis process, and the other operation steps are the same as in Example 1. Among them, Example 6 was subjected to ultrasonic action for 30 minutes during the first hydrolysis. The specific surface area and pore diameter parameters of the mesoporous titanium dioxide prepared in Examples 1 to 6 are shown in Table 1.

[0050] Table 1 Specific surface area and average pore diameter of mesoporous titanium dioxide

[0051]

Embodiment 7～9

[0053] The calcination temperature was changed, and the other operation steps were the same as in Example 1. The specific surface area and average pore diameter of the prepared mesoporous titanium dioxide are shown in Table 2.

[0054] Table 2 The specific surface area and average pore diameter of mesoporous titanium dioxide

[0055] Example

[0056] 2. Mesoporous SO 4 2- / TiO 2 Example of preparation of solid super acid

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Abstract

The invention relates to a preparation method for meso-pore TiO2 and SO42- / TiO2 solid super strong acid. Wherein, with industrial TiSO4 liquor as material, hydrolyzing step by step to obtain meso-poremetatitanic acid; clearing, separating, drying, and calcinating to obtain the final product. The low angle X-ray diffraction diagram of the obtained meso-pore TiO2 shows as in figure 2 with 150-200m2 / g specific surface area and well thermal stability. The obtained solid super strong acid has 1-8% sulfur content, 0. 02-3% iron content, 2-8nm pore size, and about 200m2 / g specific surface area, andpresents well catalytic activity for esterification reaction.

Description

1. Technical Field [0001] The invention relates to the technical field of preparation of inorganic mesoporous materials and their catalytic materials, and more specifically, to a mesoporous titanium dioxide and its mesoporous SO 4 2- / TiO 2 Preparation method of solid super acid and mesoporous SO 4 2- / TiO 2 Type solid super acid. 2. Background technology [0002] Titanium dioxide with a certain pore structure and high specific surface area is widely used as a catalyst and catalyst carrier, and has shown its extremely superior catalytic desulfurization performance in the desulfurization of natural gas, petroleum gas and coal gas (CN1712500, CN1508221); as a catalyst carrier, vanadium oxide The vanadium-titanium catalyst formed on titanium dioxide can be widely used in selective oxidation and reduction reactions. The vanadium-titanium catalyst has an irreplaceable role in the selective reduction of flue gas deNOx process. It has been burned in developed countries such as Europe, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053B01J27/053
Inventor 张昭沈俊张明俊游贤贵黄学超
Owner SICHUAN UNIV
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