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Continuous flow micro-channel reactor and method for preparing imidazole by using same

A channel reactor and channel technology, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical processes, etc., can solve problems such as unfavorable concentration and rectification separation of imidazole, unfavorable safety production, etc. , to achieve the effects of improving selectivity and yield, reducing reaction time, and mild reaction conditions

Inactive Publication Date: 2020-06-09
NINGXIA JOIE MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Patent CN109422693A discloses a method for continuously preparing imidazole using micro-reaction technology, using microchannel reaction continuous flow to prepare imidazole, but the reaction temperature of this invention exceeds 100°C, which will produce a large number of by-products, which is not conducive to the subsequent concentration and rectification of imidazole. ; and the invention reacts as a stress response and is unfavorable for safe production

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  • Continuous flow micro-channel reactor and method for preparing imidazole by using same
  • Continuous flow micro-channel reactor and method for preparing imidazole by using same

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Embodiment 1

[0031] Such as figure 1 Shown, a kind of continuous flow microchannel reactor comprises the first reaction group and the second reaction group, and the first reaction group comprises the first material mixing channel 1, and the first material mixing channel 1 is provided with the first and the second Two feed channels (3 and 4), connect the second material mixing channel 2 of the second reaction group through the straight tube micro channel 6, the first straight tube micro channel 6 is connected with the third feeding channel 5, the second material mixing channel 2 is provided with a material outlet connected to the storage tank 8, and the first material mixing channel 1 and the second material mixing channel 2 are provided with micro channels. Temperature sensors are provided inside the first and second material mixing channels, and heat exchange pipelines are provided outside the channels, and both the temperature sensors and the heat exchange pipelines are connected to an i...

Embodiment 2

[0033] Embodiment 2 adopts the method for preparing imidazoles by continuous flow microchannel reactor

[0034] The formaldehyde solution with a mass fraction of 25% and the glyoxal solution with a mass fraction of 31% enter the first reaction group through the 3rd and 4th metering pumps according to the molar ratio n (formaldehyde): n (glyoxal)=1:1, The mixed aldehyde flow rate is set to 7ml / min, and the mass fraction is 15% ammonia solution and catalyst ammonium sulfate according to the molar ratio n (catalyst):n (ammonia water)=1:15 and enters the second reaction group through the third feeding channel 5 , the feed flow rate is set at 8ml / min, the temperature of the first reaction group temperature channel is set to 30°C, the temperature of the second and third reaction group channels is set to 70°C, and the residence time of the reaction in the first material mixing channel is controlled to be 30s, control the residence time of the material in the second material mixing ch...

Embodiment 3

[0036] Embodiment 3 adopts the method for preparing imidazoles by continuous flow microchannel reactor

[0037] The formaldehyde solution with a mass fraction of 27% and the glyoxal solution with a mass fraction of 32% enter the first reaction group through the 3rd and 4th metering pumps according to the molar ratio n (formaldehyde):n (glyoxal)=1:1.2, The mixed aldehyde flow rate is set at 5ml / min, and the mass fraction is 15% ammonia solution and catalyst ammonium sulfate according to the molar ratio n (catalyst):n (ammonia water)=1:20 and enters the second reaction group through the third feeding channel 5 , the feed flow rate is set at 10ml / min, the temperature of the first reaction group temperature channel is set to 30°C, the temperature of the second and third reaction group channels is set to 60°C, and the residence time of the reaction in the first material mixing channel is controlled to be 30s, control the residence time of the material in the second material mixing ...

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Abstract

The invention provides a continuous flow micro-channel reactor. The reactor comprises a first reaction group and a second reaction group. The first reaction group comprises a first material mixing channel. A first feeding channel, a second feeding channel and a second material mixing channel are arranged outside the first material mixing channel, and the second material mixing channel is connectedwith the second reaction group through a straight pipe micro-channel. The straight pipe micro-channel is connected with a third feeding channel. The second material mixing channel is provided with amaterial outlet which is connected with a storage tank. The invention also provides a process for preparing imidazole by adopting the continuous flow micro-channel reactor. The micro-channel reactor can reduce the reaction time from more than ten hours of the traditional intermittent reaction to less than several minutes by accurately controlling the flow rate and the retention time, so that the reaction time is greatly reduced. According to the method, high temperature and high pressure are not needed, reaction conditions are mild, the operation is easy, time consumption is low, the production efficiency is improved, and therefore a basis is provided for industrial production of imidazole.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and in particular relates to a method for preparing imidazole by using a continuous flow microchannel reactor. Background technique [0002] Imidazole is mainly used as a raw material for medicines and pesticides. It is one of the main raw materials for azoles, econazoles, ketoconazoles, clotrimazoles and other drugs. In addition, it is also widely used in fruit and vegetable preservatives. Oxygen resin curing agent, accounting for more than 90%, is a very important organic synthesis intermediate. [0003] At present, the method of industrial production of imidazole at home and abroad mainly adopts α-dicarbonyl compound (glyoxal), ammonia and aldehyde as raw materials, and forms an imidazole ring through condensation reaction, and the reaction is usually carried out in an indirect tank reactor. In the batch tank reactor, it is carried out by dropping: under continuous stirring...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C07D233/58
CPCB01J19/0093C07D233/58
Inventor 沈健
Owner NINGXIA JOIE MATERIAL CO LTD