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Method for continuously synthesizing dimethyl sulfone

A technology of dimethyl sulfone and dimethyl sulfoxide, which is applied in the field of reaction to generate dimethyl sulfone, can solve the problems of high requirements for reaction equipment, long reaction time, low efficiency, harsh reaction conditions, etc., so as to improve the reaction rate and raw materials The utilization rate, the shortening of process production time, and the effect of improving operability

Inactive Publication Date: 2018-11-20
CHANGZHOU UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] The above method has optimized and improved the synthesis method of dimethyl sulfone from different angles, but there are still some problems to be solved: firstly, batch production is still mainly adopted in large-scale production, and the reaction efficiency is low. It is relatively complicated and produces more industrial waste. Secondly, in the above method, there are still a series of problems such as poor mass and heat transfer effects, high requirements for reaction equipment, low safety factor, harsh reaction conditions, long reaction time and low efficiency.

Method used

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  • Method for continuously synthesizing dimethyl sulfone
  • Method for continuously synthesizing dimethyl sulfone
  • Method for continuously synthesizing dimethyl sulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] refer to figure 2 Determine the reactor connection mode, the channel type is (4e+4a) cylindrical straight channel and diamond microchannel structure, the channel volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0028] 50% hydrogen peroxide is used as the oxidant system, and dimethyl sulfoxide is used as the raw material system. The two systems are injected into the reactor by a metering pump at a flow rate of 11.76ml / min and 10.24ml / min, at this time n(DMSO):n(H 2 o 2 )=1:1, using figure 2 In a microchannel reactor, the temperature is controlled at 140°C, and the residence time is 600s. The reaction solution is quantitatively collected, concentrated and crystallized by cooling to obtain white crystals. The product yield is 84.2% according to weighing calculation, and the purity of the product detected by chromatography is 97.8%.

Embodiment 2

[0030] refer to figure 2 Determine the reactor connection mode, the channel type is (4e+4b) cylindrical straight channel and heart-shaped microchannel structure, the channel volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0031] 50% hydrogen peroxide is used as the oxidant system, and dimethyl sulfoxide is used as the raw material system. With the two systems respectively, the two systems are injected into the reactor by metering pumps with the flow rate of 27.17ml / min and 10.33ml / min respectively, at this moment n(DMSO):n(H 2 o 2 )=1:2, using figure 2 In a microchannel reactor, the temperature is controlled at 130° C., and the residence time is 480 s. The reaction solution is quantitatively collected, concentrated and crystallized by cooling to obtain white crystals. The product yield is 87.9% by weighing, and the purity of the product detected by chromatography is 99.3%.

Embodiment 3

[0033] refer to figure 2 Determine the reactor connection mode, the channel type is (4e+4c) cylindrical straight channel and triangular microchannel structure, the channel volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0034] 50% hydrogen peroxide is used as the oxidant system, and dimethyl sulfoxide is used as the raw material system. With the two systems respectively, the two systems are injected into the reactor by a metering pump at a flow rate of 12ml / min and 10ml / min, at this time n(DMSO):n(H 2 o 2 )=1:1.5, using figure 2 In a microchannel reactor, the temperature was controlled at 140°C, and the residence time was 600s. The reaction solution was collected quantitatively, concentrated and crystallized by cooling to obtain white crystals. The product yield was 83.9% by weighing, and the purity of the product was 97.8% as determined by chromatography.

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Abstract

The invention discloses a method for continuously synthesizing dimethyl sulfone, and belongs to the technical field of organic synthesis. According to the method provided by the invention, dimethyl sulfone is prepared in a continuous flow microchannel reactor by using dimethyl sulfoxide as a raw material and using the aqueous solution of hydrogen peroxide as an oxidant. The method has the advantages of mild condition, short reaction time and high utilization of raw materials, can realize effective control in the reaction process, is safe and stable, realizes continuous operation and has high production efficiency.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and relates to a method for preparing dimethyl sulfone from dimethyl sulfoxide in a continuous flow microchannel reactor, more specifically, using dimethyl sulfoxide as a substrate, Hydrogen aqueous solution is used as an oxidant, and it reacts in a continuous flow microchannel reactor to generate dimethyl sulfone. Background technique [0002] Dimethyl sulfone (MSM) is an organic sulfide that is necessary for the synthesis of collagen in the human body. Human skin, hair, nails, bones, muscles and various organs contain MSM. The human body consumes 0.5mg of MSM every day. Once lacking, it will cause health disorders or diseases. Because it is a newly discovered human nutrient substance, it has therapeutic value and health care function for human diseases, is an essential drug for human survival and health protection, and is also a raw material for many pharmaceutical interme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/02C07C317/04
CPCC07C315/02C07C317/04
Inventor 张跃薛鹏博丁晓丹刘浩沈禹凡严生虎刘建武沈介发辜顺林马晓明
Owner CHANGZHOU UNIV
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