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Preparation method and application of MIL-125 (Ti) catalyst

A MIL-125, catalyst technology, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., to achieve the effects of simple preparation methods, improved activity, and increased specific surface area

Pending Publication Date: 2022-01-07
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, in the prior art, there are still few reports on the regulation method of the crystal size of the MIL-125(Ti) catalyst.

Method used

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  • Preparation method and application of MIL-125 (Ti) catalyst
  • Preparation method and application of MIL-125 (Ti) catalyst
  • Preparation method and application of MIL-125 (Ti) catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Measure 36mL of N,N-dimethylformamide solution and 4mL of methanol solution in a beaker and mix to obtain a mixed solvent;

[0048] (2) take 2.0g of terephthalic acid and dissolve it in the mixed solvent of step (1), stir to obtain mixed solution;

[0049] (3) Measure 1 mL of tetrabutyl titanate in the mixed solution of step (2), ultrasonicate for 15 minutes, transfer the solution to a polytetrafluoroethylene crystallization kettle, place it in a hydrothermal treatment at 150 ° C for 48 hours, and centrifuge to obtain crystals product;

[0050] (4) The crystalline product obtained in the step (3) was washed three times with N,N-dimethylformamide and methanol, respectively, and was dried under vacuum at 70° C. for 12 hours to obtain the corresponding catalyst.

Embodiment 2

[0052] (1) Measure 36mL N,N-dimethylformamide solution and 4mL methanol solution in a beaker and mix to obtain a mixed solvent;

[0053] (2) take 2.0g of terephthalic acid and dissolve it in the mixed solvent of step (1), stir to obtain mixed solution;

[0054] (3) Measure 1 mL of tetrabutyl titanate, weigh 0.1 g of glacial acetic acid in the mixed solution of step (2), ultrasonicate for 15 min, transfer the solution to a polytetrafluoroethylene crystallization kettle, and place it in water at 150° C. Heat treatment for 48h, centrifugation to obtain crystalline product;

[0055] (4) The crystalline product obtained in the step (3) was washed three times with N,N-dimethylformamide and methanol, respectively, and was dried under vacuum at 70° C. for 12 hours to obtain the corresponding catalyst.

Embodiment 3

[0057] (1) Measure 36mL N,N-dimethylformamide solution and 4mL methanol solution in a beaker and mix to obtain a mixed solvent;

[0058] (2) take 2.0g of terephthalic acid and dissolve it in the mixed solvent of step (1), stir to obtain mixed solution;

[0059] (3) Measure 1 mL of tetrabutyl titanate, weigh 0.2 g of glacial acetic acid in the mixed solution of step (2), ultrasonicate for 15 min, transfer the solution to a polytetrafluoroethylene crystallization kettle, and place it in water at 150° C. Heat treatment for 48h, centrifugation to obtain crystalline product;

[0060] (4) The crystalline product obtained in the step (3) was washed three times with N,N-dimethylformamide and methanol, respectively, and was dried under vacuum at 70° C. for 12 hours to obtain the corresponding catalyst.

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Abstract

The invention discloses a preparation method and application of an MIL-125 (Ti) catalyst, and the preparation method comprises the following steps: mixing an N, N-dimethylformamide solution and a methanol solution to obtain a mixed solvent; dissolving an organic ligand in the mixed solvent, and uniformly stirring to obtain a mixed solution; adding tetrabutyl titanate and organic acid into the mixed solution, carrying out ultrasonic treatment, transferring into a polytetrafluoroethylene crystallization kettle, carrying out hydrothermal treatment, and carrying out centrifugal separation to obtain a crystallization product; and cleaning the obtained crystallization product, and carrying out vacuum drying to obtain the MIL-125 (Ti) catalyst. The MIL-125 (Ti) catalyst disclosed by the invention can be synthesized in one step, the crystal size of the catalyst can be effectively controlled through the addition amount of organic acid, and thiophene sulfide can be catalytically oxidized at room temperature, so that more efficient desulfurization is realized; the preparation method of the catalyst is simple, and the catalyst has a good application prospect in the aspect of oil product desulfurization.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of a MIL-125 (Ti) catalyst and its application in catalytic oxidation removal of thiophene sulfides. Background technique [0002] In recent decades, with the rapid development of my country's industrialization, people's demand for fuel oil has gradually increased. However, the combustion of fuel oil will make SO in the air X concentration increased. Recent studies have shown that changes in the concentration of sulfur-containing compounds in the air can cause different hazards to the environment and also affect human health. With the gradual improvement of environmental protection laws and regulations at home and abroad, various countries have increasingly strict standards for sulfur content in fuel oil. Facing the increasingly stringent emission standards for sulfur content in fuel oil, my country's fuel oil desulfurization industry is also facing sev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/02C08G83/00C10G27/12
CPCB01J31/2239C08G83/008C10G27/12B01J2531/46C10G2300/202B01J35/40
Inventor 黄小侨李剑新吕树祥邵子奇李雨师周易谦廖小元
Owner PETROCHINA CO LTD
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