Method for preparing porous manganese oxide catalyst

A manganese oxide and catalyst technology, which is applied in the field of preparing porous manganese oxide catalysts, can solve the problems of low specific surface and difficulty in meeting requirements, and achieve the effect of excellent performance.

Active Publication Date: 2018-07-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the low specific surface area of ​​existing manganese oxide ca

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Mix 10.0g 50% manganese nitrate solution (mass concentration, 10g includes the quality of water in the manganese salt solution, the same below), 30.0g water, 30g ethanol, 10g oxalic acid, 10g 1,2-propylene glycol in a beaker, stir well , placed in a 50°C oil bath, heated and stirred until expanded and foamed, dried in an oven at 80°C for 24 hours, and then calcined in air at 400°C for 3 hours to obtain a porous manganese oxide catalyst.

[0021] Add 400mg of the above-mentioned catalyst into 6g of ethylbenzene, fill with 3MPa oxygen, react at 160°C for 24 hours, the conversion rate of ethylbenzene is 57.9%, and the selectivity of acetophenone and DL-1-phenylethanol is >99%.

Embodiment 2

[0023] Mix 10.0g of manganese chloride tetrahydrate (10g including the mass of water in the hydrate, the same below), 30.0g of water, 30g of ethanol, 10g of oxalic acid, and 10g of 1,2-propanediol in a beaker, stir well, and place at 50 ℃ in an oil bath with heating and stirring until expansion and foaming, the foamed material was dried in an oven at 80 ℃ for 24 hours, and then calcined in air at 400 ℃ for 3 hours to obtain a porous manganese oxide catalyst.

[0024] Add 400 mg of the above catalyst into 6 g of ethylbenzene, fill with 3 MPa oxygen, react at 160° C. for 24 hours, the conversion rate of ethylbenzene is 54.1%, and the selectivity of acetophenone and DL-1-phenylethanol is >99%.

Embodiment 3

[0026] Mix 10.0g manganese sulfate monohydrate, 30.0g water, 30g ethanol, 10g oxalic acid, 10g 1,2-propanediol in a beaker, stir evenly, heat and stir in an oil bath at 50°C until it expands and foams. The material was dried in an oven at 80°C for 24h, and then calcined in air at 400°C for 3h to obtain a porous manganese oxide catalyst.

[0027] Add 400mg of the above-mentioned catalyst to 6g of ethylbenzene, fill with 3MPa oxygen, react at 160°C for 24 hours, the conversion rate of ethylbenzene is 48.9%, and the selectivity of acetophenone and DL-1-phenylethanol is >99%.

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Abstract

The invention relates to a preparation technology of a catalytic material, and aims to provide a method for preparing a porous manganese oxide catalyst. The method comprises the following steps: carrying out foaming treatment by using manganese salt, a hydrate of the manganese salt or an aqueous solution of the manganese salt as a precursor and a lipid polymer prepared from organic acid and alcohols in situ as a foaming agent, uniformly stirring after mixing the precursor, the organic acid, the alcohols used for carrying out esterification reaction with acid, the water and ethanol which is used as a solvent according to a mass ratio of 10 to 10 to 10 to 30 to 30, and heating and stirring under 50 to 170 DEG C until expanding and foaming; carrying out drying and roasting treatment on a thick colloidal-state matter obtained through foaming, thus obtaining the porous manganese oxide catalyst. The porous manganese oxide catalyst prepared by the invention has a porous structure and has excellent performance aiming at C-H bond activation reaction. Even under a solvent-free condition, the porous manganese oxide catalyst prepared by the invention is still capable of realizing efficient activated oxidation on ethylbenzene C-H bonds.

Description

technical field [0001] The invention relates to a preparation technology of catalytic materials, in particular to a method for preparing a porous manganese oxide catalyst. Background technique [0002] Nowadays, in most industrial and fine chemical production processes, it is of great significance to obtain high value-added products through the catalytic oxidation of saturated C–H bonds. In many catalytic systems, molecular oxygen is used to achieve efficient and high selectivity for sp 3 The catalytic oxidation of the C–H bond is a key challenge, because the inertness of the C–H bond generally requires a high operating temperature and a huge energy consumption (for example, the dehydrogenation of propane requires 400~ at 700°C). The use of molecular oxygen as an oxidant also often causes over-oxidation, resulting in low product selectivity and easy carbon deposition. Therefore, catalytic materials with better catalytic performance are designed and prepared to achieve effi...

Claims

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Application Information

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IPC IPC(8): B01J23/34B01J37/08C07C49/78C07C45/36C07C33/22C07C29/50
CPCB01J23/34B01J37/0018B01J37/082B01J37/088C07C29/50C07C45/36C07C49/78C07C33/22
Inventor 王亮王海肖丰收
Owner ZHEJIANG UNIV
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