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Method for preparing 2-bromo-2-methylpropane by brominating tert-butyl alcohol through microchannel reactor

A technology of microchannel reactor and brominated tert-butanol, which is applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., to achieve the effects of increasing conversion rate, avoiding serious corrosion of equipment, and excellent corrosion resistance

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

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Problems solved by technology

[0004] So far, there has been no research on the liquid-phase bromination of tert-butanol to synthesize tert-butane bromide in the Corning microchannel continuous flow mode. Process route for preparing bromo-tert-butane from butanol

Method used

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  • Method for preparing 2-bromo-2-methylpropane by brominating tert-butyl alcohol through microchannel reactor
  • Method for preparing 2-bromo-2-methylpropane by brominating tert-butyl alcohol through microchannel reactor
  • Method for preparing 2-bromo-2-methylpropane by brominating tert-butyl alcohol through microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) The device used: Corning high -throughput micro -channel reactor (Corning straight channel module+Corning heart -type channel module), refer to image 3 Determine the connection mode of the micro -channel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction stay time, and the heat exchange medium is the heating oil.

[0028] (2) Set the metering pump 4. Pump 5, pump 6 volume flow ratio is ol -limedol: hydrocelatic acid: concentrated sulfuric acid = 10: 17.5: 5.9, separate three materials into the preheating modules of the passage in each passage, respectivelySet the temperature of the heat exchanger at 60 ° C; the tanl butanol and hydride acid use the metering pump 4 and 5 into the microcosculator heart -shaped module 11 for mixing.The ratio is 1: 1.2.The mixed raw material is then entered into the lower heart -shaped mixed module 12, and the concentration sulfuric acid is mixed to react.In the end, the proportion of mol wit...

Embodiment 2

[0031] (1) The device used: Corning high -throughput micro -channel reactor (Corning straight channel module+Corning heart -type channel module), refer to image 3 Determine the connection mode of the micro -channel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction stay time, and the heat exchange medium is the heating oil.

[0032](2) Set the metering pump 4. Pump 5, pump 6 The volume flow rate ratio is ol -limedol: hydrocelatic acid: concentrated sulfuric acid = 10: 14.5: 5.9, and the three materials are separated into the preheating module of each direct channel, respectivelySet the temperature of the heat exchanger to 30 ° C; the tanl butanol and hydride acid use the metering pump 4 and 5 into the microcosculator heart -shaped hybrid module 11 for mixing.The ratio is 1: 1.The mixed raw material is then entered into the lower heart -shaped mixed module 12, and the concentration sulfuric acid is mixed to react.In the end, the prop...

Embodiment 3

[0035] (1) The device used: Corning high -throughput micro -channel reactor (Corning straight channel module+Corning heart -type channel module), refer to image 3 Determine the connection mode of the micro -channel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction stay time, and the heat exchange medium is the heating oil.

[0036] (2) Set the metering pump 4. Pump 5, pump 6 volume flow ratio is ol -liol: hydrocelatic acid: concentrated sulfuric acid = 10: 12.5: 5.9, separate three materials into the preheating modules of the passage in each passage, respectivelySet the temperature of the heat exchanger to 30 ° C; the tanl butanol and hydride acid use the metering pump 4 and 5 into the microcosculator heart -shaped hybrid module 11 for mixing.The ratio is 1: 0.8.The mixed raw material is then entered into the lower heart -shaped mixed module 12, and the concentration sulfuric acid is mixed to react.In the end, the proportion of mol...

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Abstract

The invention relates to a method for preparing 2-bromo-2-methylpropane by brominating tert-butyl alcohol through a microchannel reactor, belonging to the technical field of organic synthesis application. In the new process provided by the invention, tert-butyl alcohol and hydrobromic acid are used as raw materials, concentrated sulfuric acid is used as a catalyst, and 2-bromo-2-methylpropane is synthesized in a Corning microchannel reactor in a short reaction time of tens of seconds to several minutes. The method comprises the following steps: introducing three strands of materials into the Corning microchannel reactor through measuring pumps, preheating, mixing, and reacting to finally obtain the brominated product 2-bromo-2-methylpropane. The method is simple to operate and makes the high-yield continuous 2-bromo-2-methylpropane production possible. Besides, the environmental pollution caused by the process is greatly reduced. According to the invention, the tert-butyl alcohol conversion rate is up to 91-97%, and the 2-bromo-2-methylpropane selectivity is up to 92-97%.

Description

Technical field [0001] The present invention is an organic synthetic application technology field, which involves a method of preparing bromenocylcesertane with oste butanol as raw ingredients. More specifically, Corning (Corning) micro -channel in high -throughput microchannel flows continuously flows.In the reactor, the process of bromine is used to prepare the bromine -oxyl oxane. Background technique [0002] Cracratopatane is an important chemical raw material and an important organic intermediate. It can be used as an alkylated agent and intermediate when solvent and organic synthesis;) The raw materials and the raw materials used to synthesize the uncle's base benzene and to the second uncle. [0003] At present, the main preparation process in the industry is obtained by the reaction of cracium.Blobialization is generally used to use hydride-concentrated sulfate or bromide-concentrated sulfuric acid method. [0004] So far, no research on the form of cubidol synthetic bro...

Claims

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Application Information

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