Method for preparing bromo-2-methylpropane through bromination of tertiary butanol in continuous flow micro-channel reactor

A technology of microchannel reactor and channel reactor, which is applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve the problems of large consumption of concentrated sulfuric acid, large consumption of raw materials, environmental pollution, etc., to avoid Severely corroded equipment, reduced generation of waste acid, and excellent corrosion resistance

Active Publication Date: 2013-01-16
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method produces a large amount of waste acid, which has serious environmental pollution, a large amount of catalyst, and generally low yield of bromo-tert-butane
In addition, metal bromide salts are often used in industry to react with concentrated sulfuric acid and catalyze bromination of tert-butanol to prepare brominated tert-butane. In this method, concentrated sulfuric acid is used as both a catalyst and a reactant, and the reaction is violent and exothermic. It is easy to cause volatilization of raw materials and products, and the consumption of concentrated sulfuric acid is large, the utilization rate is low, and the amount of waste acid produced is large
Since the reaction is car

Method used

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  • Method for preparing bromo-2-methylpropane through bromination of tertiary butanol in continuous flow micro-channel reactor
  • Method for preparing bromo-2-methylpropane through bromination of tertiary butanol in continuous flow micro-channel reactor
  • Method for preparing bromo-2-methylpropane through bromination of tertiary butanol in continuous flow micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Device used: continuous flow microchannel reactor (straight channel functional module + "heart-shaped" structural functional module), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0029] (2) Set the volume flow rate ratio of each metering pump 4, pump 5, and pump 6 as tert-butanol: hydrobromic acid: concentrated sulfuric acid = 10: 14.5: 5.9, and put the three streams of materials into each straight channel preheating module respectively , set the temperature of the heat exchanger to 60°C; after preheating, pour them into the "heart-shaped" structural functional module for mixing and then react. Finally, the molar ratio of tert-butanol, hydrobromic acid and concentrated sulfuric acid is 1:1:1. The reaction residence time is 95s, the pressure is 1.2bar, and the reaction product ...

Embodiment 2

[0032] (1) Device used: continuous flow microchannel reactor (straight channel functional module + droplet channel), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0033] (2) Set the volume flow rate ratio of each metering pump 4, pump 5, and pump 6 as tert-butanol: hydrobromic acid: concentrated sulfuric acid = 10: 17.5: 5.9, and put the three streams of materials into the functional modules of each straight channel for pre-treatment. Heat, set the temperature of the heat exchanger to 30°C; after preheating, pour them into the drop-shaped channel of the micro-mixer for mixing and then react. Finally, the molar ratio of tert-butanol, hydrobromic acid and concentrated sulfuric acid is 1:1.2:1. The reaction residence time is 86s, the pressure is 1.6bar, and the reaction product flows out of ...

Embodiment 3

[0036](1) The device used: continuous flow microchannel reactor (straight channel functional module + spherical baffle plate channel), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0037] (2) Set the volume flow rate ratio of each metering pump 4, pump 5, and pump 6 as tert-butanol: hydrobromic acid: concentrated sulfuric acid = 10: 21.8: 5.9, and put the three streams of materials into the functional modules of each straight channel for pre-treatment. Heat, set the temperature of the heat exchanger to 30 ° C; after preheating, put them into the spherical channel of the micro-mixer with baffle plate for mixing and then react. Finally, the molar ratio of tert-butanol, hydrobromic acid and concentrated sulfuric acid is 1:1.5:1. The reaction residence time is 76s, the pressure is 2bar, and t...

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Abstract

The invention discloses a method for preparing bromo-2-methylpropane through bromination of tertiary butanol in a continuous flow micro-channel reactor, belonging to the technical field of organic synthesis application. The method is a new process in which the tertiary butanol and hydrobromic acid are used as raw materials and concentrated sulfuric acid is used as a catalyst to synthesize the bromo-2-methylpropane in the reaction time of scores of seconds to several minutes in the continuous flow micro-channel reactor. Three steams of materials are led into the continuous flow micro-channel reactor through a metering pump and are preheated, mixed and reacted to finally obtain a bromination product, i.e., the bromo-2-methylpropane. The method is easy and convenient to operate, so that high-yield continuous production of the bromo-2-methylpropane becomes possible, and the process has low environment pollution. The conversion rate of the tertiary butanol reaches 78-95 percent, and the selectivity of the bromo-2-methylpropane reaches 92-97 percent.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, and in particular relates to a method for preparing brominated tert-butane by bromination of tert-butanol as a raw material, more specifically, in a continuous flow microchannel reactor, using hydrobromic acid to brominate A process for preparing tert-butane bromide from tert-butanol. Background technique [0002] Bromo-tert-butane is an important chemical raw material and an important organic intermediate, which can be used as a solvent and an alkylating agent and intermediate in organic synthesis; it can also be used as a spice (such as methyl amyl ketone ) and the raw materials used to synthesize tert-butylbenzene and p-di-tert-butylbenzene. [0003] At present, the main industrial preparation process is to obtain tert-butanol through bromination reaction. Bromination is generally carried out by hydrobromic acid-concentrated sulfuric acid method or bromide salt-concentr...

Claims

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Application Information

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IPC IPC(8): C07C19/075C07C17/16
Inventor 张跃郭欣桐严生虎刘建武沈介发
Owner CHANGZHOU UNIV
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