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Preparation method of dimethyl sulfone and solid catalyst for same

A solid catalyst, dimethyl sulfone technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of unsuitability for industrialization, difficult product separation, high cost, etc., and achieve easy separation and high catalytic activity , low cost effect

Inactive Publication Date: 2013-11-27
GENIFARM LAB INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1397533A adds a transition metal complex catalyst immobilized by the sol-gel method in the oxidation reaction, and uses air as an oxidant, so that the reaction can be carried out under very mild conditions, and the yield of alkyl sulfide can reach 95%. However, this method needs to add 3 equivalents of isovaleraldehyde as a reducing agent. The introduction of isovaleraldehyde leads to high cost. At the same time, isovaleraldehyde is oxidized to bring new impurities, which are difficult to separate from the product. Therefore, this method is not suitable. industrialization
[0003] At present, there is no method for catalytically synthesizing alkyl sulfones with mild reaction conditions, high efficiency, and low cost using air or oxygen as the oxidant.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 25.5g MnSO 4 ·H 2 O, 4.8g CoCl 2 ·6H 2 O, 25.6g CuCl 2 2H 2 O, 1.8gPdCl 2 with 2.1g RuCl 3 Mixed, added to 200ml of deionized water and stirred evenly, slowly added dropwise the obtained slurry into 500ml of 10% NaOH solution by mass, stirred at 100°C for 2 hours after the dropwise addition, cooled to room temperature, filtered, and used Wash with ionic water until neutral, activate at 300°C for 12 hours, cool to room temperature and grind to obtain Mn 1.5 co 0.2 Cu 1.5 PD 0.1 Ru 0.1 o 3.45 22.0 g of black solid catalyst powder.

Embodiment 2

[0026] 51.0g MnSO 4 ·H 2 O, 9.6g CoCl 2 ·6H 2 O, 5.1g CuCl 2 2H 2 O, 1.8gPdCl 2 with 2.1g RuCl 3 Mixed, added to 200ml of deionized water and stirred evenly, slowly added dropwise the obtained slurry into 500ml of 10% NaOH solution by mass, stirred at 100°C for 2 hours after the dropwise addition, cooled to room temperature, filtered, and used Wash with ionic water until neutral, activate at 300°C for 12 hours, cool to room temperature and grind to obtain Mn 3 co 0.4 Cu 0.3 PD 0.1 Ru 0.1 o 3.95 20.5 g of black solid catalyst powder.

Embodiment 3

[0028] 25.5g MnSO 4 ·H 2 O, 4.8g CoCl 2 ·6H 2 O, 3.0g CuCl, 3.5g PdCl 2 with 0.21gRuCl 3 Mixed, added to 200ml of deionized water and stirred evenly, slowly added dropwise the obtained slurry into 500ml of 5% NaOH solution by mass, stirred at 100°C for 2 hours after the dropwise addition, cooled to room temperature, filtered, and used Wash with ionic water until neutral, activate at 300°C for 12 hours, cool to room temperature and grind to obtain Mn 1.5 co 0.2 Cu 0.3 PD 0.2Ru 0.01 o 2.06 11.4 g of black solid catalyst powder.

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PUM

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Abstract

The invention discloses a preparation method of dimethyl sulfone and a solid catalyst for the preparation method. The solid catalyst has a molecular formula of MnvCowCuxPdyRuzOo, wherein Mn, Co and Pd are bivalent, Cu is monovalent or bivalent, Ru is trivalent, v, w, x, y and z are selected from 0.01-5, and o is selected from 0.05-27.5. The preparation method of dimethyl sulfone comprises the steps of: mixing dimethyl sulfide, a solvent and the solid catalyst, and reacting in 1-30atm air oxygen atmosphere at reaction temperature of 40-150 DEG C for 1-48h, wherein the weight ratio of dimethyl sulfide to the solid catalyst to the solvent is 1:(0.0001-1):(0-10). According the invention, oxygen or air is used as an oxidant; and compared with traditional method, no any harmful substances are generated in the preparing process, no any side reaction products are generated, and no any environmental pollution is caused; the preparation method has the advantages of simpleness and convenience in operation, short flow, mild reaction conditions, low cost, high efficiency and the like; and at the same time, the used solid catalyst is easy to separate, and can be recycled multiple times.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a preparation method of dimethyl sulfone and a solid catalyst thereof. Background technique [0002] Dimethyl sulfone is a human nutrient newly discovered abroad in recent years. It has therapeutic value and health care function for human diseases. It can be used in various industries and scientific researches such as medicine, food, feed additives, cosmetics, etc., so it has been valued by developed countries. , widely used and sold abroad. The synthesis of dimethyl sulfone is usually formed by the oxidation of dimethyl sulfide or dimethyl sulfoxide, and the method forms different routes according to the choice of oxidant. However, most of them use organic or inorganic salt oxidants, which are difficult to deal with after such reactions, or may cause pollution to the environment. Therefore, the preparation of dimethyl sulfone is promoted to a more environmentally friendly, safe a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07C317/04C07C315/02
Inventor 黄志鹏祝诗发王永东
Owner GENIFARM LAB INC