Preparation method of mesoporous catalyst and application of mesoporous catalyst in olefin epoxidation reaction

A catalyst and mesoporous technology, applied in the field of preparation of mesoporous catalysts, can solve the problems of low catalyst activity, difficulty in matching the hydrolysis rate of titanium source and silicon source, complicated preparation process, etc., achieve high specific surface area, weaken ineffective decomposition, synthesis simple effect

Pending Publication Date: 2022-04-22
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, Ti-TUD-1 is mainly prepared by hydrothermal synthesis method. The preparation process is complicated and the hydrolysis rate of titanium source and silicon source is difficult to match, which makes it difficult for titanium to enter the framework to form highly dispersed active sites, resulting in partial catalytic activity. Low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of La-Ti-TUD-1(De) Modification Catalyst

[0031] 1.46gLa(NO 3 ) 3 ·6H 2 O dissolved in 11.03g H 2 O, then mixed with 25.06gTEA evenly, the mixture was added dropwise to 35.00g TEOS, after stirring for 30min, 29.69g TEAOH solution with a mass fraction of 25% was added dropwise, and stirred for 3h to form a homogeneous transparent solution; Aging under light for 48 hours; blast drying at 100°C in a drying oven for 24 hours; grind the dried solid to a particle size below 2 mm and place it in a homogeneous reactor for dynamic heat treatment at 180°C for 8 hours; finally place the heat-treated solid In a muffle furnace, the temperature was increased from 5°C / min to 600°C for 10h to prepare the carrier La-TUD-1 doped with metal La. Take 5 g of La-TUD-1 and 150 mL of nitric acid solution with a concentration of 3 mol / L in a three-necked flask, and reflux and stir at 100 ° C for 1 h to remove La. After the removal of La was completed, the solid was filtered wh...

Embodiment 2

[0033] Preparation of Ce-Ti-TUD-1(De) Modified Catalyst for Ce Removal

[0034] Take 0.34gCeCl 3 Dissolved in 12.11g H 2 After O, mix well with 25.42gTEA, add the mixture dropwise to 36.00g TEOS, stir for 30min, then drop in 30.12g TEAOH solution with a mass fraction of 25%, and stir for 2.5h to form a homogeneous transparent solution; Aging in a dark place for 24 hours; air-drying at 100°C in a drying oven for 36 hours; after being abrasive, take a rubber block with a particle size of 900-2000 μm and dynamically heat-treat it in a homogeneous reactor at 170°C for 6 hours; Calcined at 700°C for 9h at a heating rate of 5°C / min to prepare Ce-TUD-1, a carrier doped with metal Ce. Take 5g of Ce-TUD-1, add 200mL of 5mol / L HCl solution, heat to reflux at 80°C and stir for 12h, suction filter while hot and dry at 120°C for 6h to prepare the demetallized Ce carrier Ce-TUD-1(De). Take 4g of Ce-TUD-1(De) with a particle size of 100~300μm and place it in a tube furnace at 200ml / minN ...

Embodiment 3

[0036] Preparation of Depraseodymium Modified Catalyst Pr-Ti-TUD-1(De)

[0037] According to the operation process of Example 1, the difference from Example 1 is that the doped lanthanide metal compound is PrCl 3 , The silanization process is as follows: disperse 3.0g Pr-Ti-TUD-1 into 50.0g cyclohexane, then add 1.5 times the catalyst mass of trimethylchlorosilane to the suspension, and reflux and stir at 120°C for 6 hours. The obtained powder was filtered, washed three times with 50 ml of cyclohexane, and then dried in a vacuum oven at 100° C. for 12 hours to obtain the silanized catalyst Pr-Ti-TUD-1 (De). The titanium content is 1.33%, the praseodymium content is 0.53%, and the average pore size is 18.1nm.

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Abstract

The invention discloses a preparation method of a mesoporous catalyst and application of the mesoporous catalyst in olefin epoxidation reaction. The preparation method comprises the following steps: introducing lanthanide rare earth metal into a TUD-1 carrier by adopting an in-situ synthesis method, partially removing the rare earth metal through acid treatment, carrying out chemical vapor deposition reaction with a titanium-containing compound, and carrying out silanization hydrophobic treatment to obtain the mesoporous catalyst. The lanthanide rare earth metal is controlled within a proper content range through partial removal, so that subsequent Ti vapor deposition can be benefited, the Ti content of the catalyst is increased, the structure of the catalyst can be coordinated and stabilized, the negative influence of acid sites of the catalyst on epoxidation reaction is reduced, and the epoxidation efficiency is improved. And invalid decomposition of the catalyst on alkyl hydroperoxide is weakened, so that the selectivity of the product is effectively improved, and the method has a relatively good industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of a mesoporous catalyst and its application in the epoxidation reaction of olefins and alkyl hydroperoxides. Background technique [0002] 1,2-epoxy compounds, as important intermediates in the synthesis of fine chemicals and pharmaceuticals, are widely used in medicine, surfactants, polymers and other related industries, and are a particularly important and widely used product. Usually, 1,2-epoxy compounds are prepared by epoxidation of olefins, and the preparation techniques include chlorohydrin method, hydrogen peroxide direct oxidation method, and co-oxidation method. The co-oxidation method uses alkyl hydroperoxide as the oxygen source to carry out the epoxidation reaction with olefins, which is economical and environmentally friendly, and the proportion of production capacity is gradually increasing, and the development prospect is good. [0003] Efficient catalysts, as the key to epoxidation reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C07D303/04C07D301/19
CPCB01J29/89C07D303/04C07D301/19B01J2229/183
Inventor 吴剑张亚茹张旭袁霞
Owner XIANGTAN UNIV
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