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A kind of method that microreactor synthesizes methyl nitrite

A technology of methyl nitrite and microreactor, which is applied in nitrite preparation, chemical instruments and methods, chemical/physical/physical-chemical reactors, etc., can solve the problem of low reactor operation efficiency, increase reaction time and residence time Long and other problems, to achieve the effect of high gas-liquid mixing efficiency, simple capacity amplification, and low N2 content

Active Publication Date: 2020-04-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Therefore, the volume of the reactor equipment is often large to increase the reaction time, and the operating efficiency of the reactor is low
In addition, the residence time of the material in the tower reactor is long (Li et al. Ind.Eng.Chem.Res, 2013, 52:2814-2823), and it is easy to generate a large amount of nitric acid (2%~4% or even higher, CN201310416056), Serious corrosion to equipment

Method used

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  • A kind of method that microreactor synthesizes methyl nitrite

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Effect test

Embodiment 1

[0022] In the tubular reactor ① inlet NO / O 2 The molar ratio is 4, the gas phase N 2 The volume content is 40%, the pre-reaction temperature is normal temperature, and the reaction residence time is 10 minutes. Single-channel microreactor ②The hydraulic diameter is 1000 microns, and the gas phase space velocity is 13000h -1 , the methanol / NO molar ratio is 2, the microreactor reaction temperature is 50°C, and the system pressure is normal pressure, the gas phase outlet methyl nitrite volume content is 43%, based on O 2 The product yield was 84.6%.

Embodiment 2

[0024] In the tubular reactor ① inlet NO / O 2 The molar ratio is 5, the gas phase N 2 The volume content is 60%, the pre-reaction temperature is normal temperature, and the reaction residence time is 8 minutes. Single-channel microreactor ②The hydraulic diameter is 300 microns, and the gas phase space velocity is 50000h -1 , the methanol / NO molar ratio is 2, the reaction temperature of the microreactor is 30°C, and the system pressure is 0.2MPa, the volume content of methyl nitrite at the outlet of the gas phase is 27.3%, based on O 2 The product yield is 85.3%.

Embodiment 3

[0026] In the tubular reactor ① inlet NO / O 2 The molar ratio is 4, the gas phase N 2 The volume content is 60%, the pre-reaction temperature is 100°C, and the reaction residence time is 1.2s. Parallel multi-channel (parallel number 30) microreactor ②The hydraulic diameter is 1000 microns, and the gas phase space velocity is 50000h -1 , gas phase N 2 Volume content 60%, NO / O 2 =4, the methanol / NO molar ratio is 2, the reaction temperature of the microreactor is 30° C., and the system pressure is normal pressure, the volume content of methyl nitrite at the outlet of the gas phase is 31.6%, and the product yield based on oxygen is 80.2%.

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Abstract

The invention discloses a method for synthesizing methyl nitrite through a microreactor. The method is mainly characterized by comprising the following steps: (a) firstly pre-reacting NO and O2 in a shell and tube reactor to generate a mixed gas containing oxynitride; and (b) carrying out nitratlon reaction via the mixed gas and methyl alcohol in a micro-channel reactor which is a single-channel reactor or a multi-channel reactor, and generating the methyl nitrite, wherein the hydraulic diameter of each micro reaction channel is in a range of 100-3000 microns, the gas-phase space velocity in the microreactor is 2000-50000h<-1>, the content of N2 in a gas phase is 40-70%; the volume ratio of the NO to the O2 is 4-7; the mole ratio of the methyl alcohol to the feedstock NO is 1-2; the yieldof the product methyl nitrite based on the O2 is greater than 70% after reaction. According to the reaction process, the material residence time is short; the side reaction is effectively inhibited; the generation of HNO3 and the like is reduced; the corrosion to the equipment is low; meanwhile, the characteristics of efficient mass transfer and heat transfer of the micro-channel reactor are used;the process has high operability and safety.

Description

technical field [0001] The invention relates to a method for synthesizing methyl nitrite, in particular to using a micro-reactor to continuously synthesize methyl nitrite. Background technique [0002] As an important organic chemical raw material, ethylene glycol is mainly used in the production of polyester fibers, plastics and rubber, and is also widely used in solvents, lubricants, plasticizers and antifreeze. There is a large gap in the supply of ethylene glycol in my country, and the dependence on imports is as high as 70%, mainly from the Middle East and North America. In view of the strong demand of the polyester industry, it is expected that the demand for ethylene glycol in my country will further increase in the future. [0003] Ethylene glycol process routes are mainly divided into petroleum routes and coal-based routes. In recent years, the coal-based route has developed rapidly, and its economy has gradually improved. For example, the production cost of coal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C203/00C07C201/04B01J19/00
CPCB01J19/0093C07C201/04C07C203/00
Inventor 尧超群陈光文阎立军焦凤军刘宏博
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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