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Method for preparing 1,2,4-butanetriol trinitrate in continuous flow microchannel reactor

A technology of butanetriol trinitrate and microchannel reactor, which is applied in nitrate preparation, organic chemistry and other directions, can solve problems such as high safety hazards, and achieve the effects of avoiding leakage, high production efficiency and reducing waste acid generation.

Active Publication Date: 2019-06-11
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the stability of nitrated 1,2,4-butanetriol is relatively good, it is also an explosive itself, and there are high safety hazards

Method used

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  • Method for preparing 1,2,4-butanetriol trinitrate in continuous flow microchannel reactor
  • Method for preparing 1,2,4-butanetriol trinitrate in continuous flow microchannel reactor
  • Method for preparing 1,2,4-butanetriol trinitrate in continuous flow microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (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.

[0030] (2) Raw material tanks 1 and 2 are equipped with 1,2,4-butanetriol solution and nitric acid-concentrated sulfuric acid solution with a mass concentration of 10%. Set the flow control of each metering pump 3 and pump 4 to change the 1,2,4-butanetriol solution: nitric acid molar ratio = 1:3, put the materials into the preheating modules of each straight channel respectively, and control the reaction temperature to 10°C; 1,2,4-butanetriol solution and nitric acid-concentrated sulfuric acid are pumped into the heart-shaped mixing module by metering pumps 3 and 4 respectively for mixing and reaction....

Embodiment 2

[0033] (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.

[0034] Raw material tanks 1 and 2 are equipped with 1,2,4-butanetriol solution and nitric acid-concentrated sulfuric acid solution with a mass concentration of 30%. Set the flow control of each metering pump 3 and pump 4 to change the 1,2,4-butanetriol solution: nitric acid molar ratio = 1:3.5, put the materials into the preheating modules of each straight channel respectively, and control the reaction temperature to 40°C; 1,2,4-butanetriol solution and nitric acid-concentrated sulfuric acid are pumped into the drop-shaped mixing module by metering pumps 3 and 4 respectively for mixing and reaction. The reaction residence time i...

Embodiment 3

[0037] (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.

[0038](2) Raw material tanks 1 and 2 are equipped with 1,2,4-butanetriol solution and nitric acid solution with a mass concentration of 100%. Set the flow control of each metering pump 3 and pump 4 to change the 1,2,4-butanetriol solution: nitric acid molar ratio = 1:4, put the materials into the preheating modules of each straight channel respectively, and control the reaction temperature to 100°C; 1,2,4-butanetriol solution and nitric acid-concentrated sulfuric acid are pumped into the ball-type baffle-type mixing module with metering pumps 3 and 4 respectively for mixing and reaction. The reaction residence...

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Abstract

The invention discloses a method for preparing 1,2,4-butanetriol trinitrate in a continuous flow microchannel reactor, and belongs to the technical field of organic synthesis application. The method is a novel process of taking a 1,2,4-butanetriol solution and nitric acid-sulfuric acid as raw materials to synthesize the 1,2,4-butanetriol trinitrate within a reaction time from dozens of seconds toseveral minutes in the continuous flow microchannel reactor. After the materials are introduced into the continuous flow microchannel reactor through a metering pump, preheating, mixing and reacting are carried out to finally obtain the target product. The method has simple and safe operation, high-yield continuous production of the 1,2,4-butanetriol trinitrate becomes possible, and environmentalpollution of the process is small.

Description

technical field [0001] The invention belongs to the field of organic synthesis application technology, and specifically relates to a method for preparing 1,2,4-butanetriol trinitrate by nitration of 1,2,4-butanetriol as a raw material. A process for preparing 1,2,4-butanetriol trinitrate in a microchannel continuous flow reactor. Background technique [0002] 1,2,4-Butanetriol trinitrate, referred to as BTTN, is an energetic plasticizer, which is currently mainly used in high-performance NEPE propellants. Because of its excellent low-temperature performance, it is not prone to freezing problems. It can effectively avoid the low-temperature embrittlement of the solid propellant and is widely used. [0003] At present, the production of 1,2,4-butanetriol trinitrate in the industry mainly includes the following methods: intermittent tank-type nitration, tank-type continuous nitration and spray nitration. Although the stability of nitrated 1,2,4-butanetriol is relatively good,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C203/04C07C201/02
Inventor 王丹丹保宇刘益含高犇张雨哲竺赛冲邹文洁杨遇春陈婧林陈代祥张跃
Owner CHANGZHOU UNIV
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