Method for preparing m-dichlorobenzene by adopting microreactor

A micro-reactor, m-dichlorobenzene technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, halogenated hydrocarbon preparation, etc. Mixing, increasing contact, high content effect

Inactive Publication Date: 2020-12-29
江苏方圆芳纶研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has good catalytic activity and high selectivity of m-dichlorobenzene, but the pores of the catalyst are easily blocked to make it deactivated.
[0007] So far, there has been no report of a method for preparing m-dichlorobenzene by isomerizing p-dichlorobenzene in a microreactor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 250ml three-necked bottle equipped with a reflux condenser and a thermometer, add 4.5g of vacuum-dried fumed silica and anhydrous toluene, N 2 Protected, stirred at room temperature for 1h. Then add 2.3g (CH 3 O) 3 Si(CH 2 ) 5 SH, heated to reflux and stirred for 12h. Filter while hot, and dry in vacuum at 80°C for 12h. Then the dried sample was placed in a Soxhlet extractor, extracted with toluene for 12 hours to remove free organosilane, and dried in vacuum at 80° C. for 12 hours to obtain a solid powder. Add hydrogen peroxide, stir at room temperature for 12 hours, oxidize mercapto groups to obtain sulfonate groups, wash, filter, and vacuum dry to obtain a gas-phase silica catalyst with sulfonate groups immobilized. Marked as SiO 2 -SO 3 H, the loading capacity of sulfonate is 0.01mol / g.

Embodiment 2

[0029] In a 250ml three-necked bottle equipped with a reflux condenser and a thermometer, add 4.5g of vacuum-dried SBA-15 and anhydrous toluene, N 2 Protection, stirring at room temperature for 0.5h. Then add 6.3g (CH 3 O) 3 Si(CH 2 ) 4 SH, heated to reflux and stirred for 12h. Then it was filtered while it was hot, and dried under vacuum at 80°C for 12h. Then the dried sample was placed in a Soxhlet extractor, extracted with toluene for 12 hours to remove free organosilane, and dried in vacuum at 80° C. for 24 hours to obtain a solid powder. Join H 2 o 2 , stirred at room temperature for 12 hours to oxidize mercapto groups to obtain sulfonate groups, wash, filter, and vacuum dry to obtain a mesoporous silica catalyst loaded with sulfonate groups. Marked as SBA-15-SO 3 H, the loading capacity of sulfonate is 0.03mol / g.

Embodiment 3

[0031] In a 250ml three-necked bottle equipped with a reflux condenser and a thermometer, add 4.5g of vacuum-dried MCM-41 and anhydrous toluene, N 2 Protection, stirring at room temperature for 0.5h. Then add 9.8g (CH 3 O) 3 Si(CH 2 ) 3SH, heated to reflux and stirred for 12h. Then it was filtered while it was hot, and dried under vacuum at 80°C for 12h. Then the dried sample was placed in a Soxhlet extractor, extracted with toluene for 12 hours to remove free organosilane, and then vacuum-dried at 80° C. for 12 hours to obtain a solid powder. Join H 2 o 2 , stirring at room temperature for 12 hours to oxidize the mercapto groups to obtain sulfonate groups, wash, filter and dry in vacuum to obtain a mesoporous silica catalyst loaded with sulfonate groups. Marked MCM-41-SO 3 H, the loading capacity of sulfonate is 0.05mol / g.

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Abstract

The invention discloses a method for preparing m-dichlorobenzene from p-dichlorobenzene in a microreactor by using a solid acid catalyst, wherein the solid acid catalyst is a catalyst in which sulfonate radicals are immobilized on a carrier, and the carrier is fumed silica or mesoporous silica. The method is continuous in reaction, high in m-dichlorobenzene selectivity and easy in quality control.

Description

[0001] field of invention [0002] The invention relates to the field of chemical synthesis, in particular to a preparation method for m-dichlorobenzene using a microreactor. Background technique [0003] m-dichlorobenzene is an important intermediate, mainly used in the synthesis of pesticides, pharmaceuticals, dyes and pigments. In terms of pesticides, m-dichlorobenzene is mainly used to synthesize fungicides and herbicides; in medicine, m-dichlorobenzene is used to synthesize imidazole antifungal drugs, anti-inflammatory analgesics, etc.; Benzene is used in the synthesis of ASITR, naphthol AS-LG and pigment solid magenta FB, etc., and its development prospect is very broad. [0004] At present, there are two main methods for the preparation of m-dichlorobenzene, m-dinitrobenzene method and isomerization method. The m-dinitrobenzene method is that m-dinitrobenzene directly undergoes free radical substitution reaction with chlorine gas under catalyst or light conditions to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/358C07C25/08B01J31/02B01J19/00B01J35/10C07C1/26C07C15/08
CPCC07C17/358B01J31/0274B01J31/0275B01J19/0093B01J35/1004C07C1/26Y02P20/52
Inventor 王农跃张启俊沙艳松陈莉李斌
Owner 江苏方圆芳纶研究院有限公司
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