Method for TORTNB etherification synthesis in microreactor

A technology of microreactor and chemical synthesis, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. It can solve the problems of cumbersome operation, low efficiency of chemical reaction, and bumping of volatile gas, so as to improve work efficiency , Improve the reaction efficiency, the effect of mass transfer speed

Active Publication Date: 2019-03-19
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In round bottom flasks and batch reactors, as the fluid approaches the agitator, it will cause convection, resulting in turbulent and chaotic flow, and the shear force that causes convection will be weakened from the agitator to the surrounding area, resulting in localized mixing inside the reactor. Inhomogeneous, resulting in concentration gradients, limited mass transfer and ultimately inefficient chemical reactions
At the same time, the reaction temperature is high and the raw materials are all organic substances with poor thermal conductivity. Uneven mixing will cause the reaction temperature to run out of control and local heating will be too fast, resulting in a sharp rise in the temperature of volatile gases and resulting in bumping. In severe cases, it may even cause explosions, posing a major safety hazard. And the operation is cumbersome

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  • Method for TORTNB etherification synthesis in microreactor
  • Method for TORTNB etherification synthesis in microreactor

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Experimental program
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Effect test

Embodiment 1

[0022] 10g (40mmol) TNPG was dissolved in 76g (720mmol) xylene, and the solution and etherification reagent triethyl orthoformate were simultaneously pumped into the intermittent flow microreactor in a continuous and constant form by a high-pressure constant flow pump, in which they were immiscible The fluid is saturated saline, which can inhibit the hydrolysis of the orthoester after dissolving the generated alcohol. At the same time, the saturated saline can reduce the solubility of organic matter in water. The reaction is carried out in an oil bath at 120°C. The flow rate of the pumped liquid is controlled to make the two raw materials The material ratio is maintained at a constant value of 1:4, the collected liquid is separated, the ethanol and ethyl formate remaining in the camera are evaporated, and the remaining reaction liquid in the reactor is washed twice at 80°C with sodium carbonate (10%) solution , retain the upper organic phase, distill off the solvent to obtain a...

Embodiment 2

[0024] 10g (40mmol) of TNPG was dissolved in 76g (720mmol) of xylene, and the solution and the etherification reagent trimethyl orthoformate were simultaneously pumped into the intermittent flow microreactor in a continuous and constant form by a high-pressure constant-flow pump, where they were immiscible The fluid is saturated saline, which can inhibit the hydrolysis of the orthoester after dissolving the generated alcohol. At the same time, the saturated saline can effectively reduce the solubility of organic matter in water. The reaction is carried out in an oil bath at 120°C. By controlling the flow rate of the pumped liquid, the materials of the two raw materials The ratio was maintained at a constant value of 1:4, the collected liquid was separated, and the methanol and methyl formate remaining in the camera were evaporated. The remaining reaction solution in the reactor was washed twice at 80° C. with sodium carbonate (10%) solution, the upper organic phase was kept, an...

Embodiment 3

[0026] 18g (72mmol) of TNPG was dissolved in 76g (720mmol) of xylene, and the solution and the etherification reagent triethyl orthoformate were simultaneously pumped into the intermittent flow microreactor in a continuous and constant form by a high-pressure constant-flow pump, in which they were immiscible The fluid is saturated saline, which can inhibit the hydrolysis of the orthoester after dissolving the generated alcohol. At the same time, the saturated saline can effectively reduce the solubility of organic matter in water. The reaction is carried out in an oil bath at 120 ° C. By controlling the flow rate of the pumped liquid, the two raw materials The ratio was maintained at a constant value of 1:4, the collected liquid was separated, the ethanol and ethyl formate remaining in the camera were evaporated, and the remaining reaction liquid in the reactor was washed twice at 80°C with sodium carbonate (10%) solution. Keep the upper organic phase, distill off the solvent t...

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Abstract

The invention discloses a method for TORTNB etherification synthesis in microreactor. The method includes steps: dissolving a nitrification product TNPG into an organic solvent; simultaneously pumpingTNPG solution and an etherification into a micro mixer, performing micro-mixing reaction, and removing generated by-products namely alcohol and ester to obtain an etherified product TORTNB. By advantages of high mixed mass transfer speed, reaction uniformity, continuity, stability and the like of a microfluid technique, TORTNB etherification reaction is realized, and problems of difficulty in process control, risks caused by local overheating, proneness to side reaction and the like of a conventional tank reactor are avoided. By adoption of the method, the TORTNB yield reaches 93.3%, and thepurity reaches 98.9%.

Description

technical field [0001] The invention relates to a method for synthesizing TORTNB through etherification in a microreactor, belonging to the technical field of microfluidics and organic synthesis. Background technique [0002] TNPG (1,3,5-trihydroxy-2,4,6-trinitrobenzene, referred to as trinitrophloroglucinol), is the product of phloroglucinol after nitration, and can form a strong combustion with a variety of Or metal salts with explosive properties, among which trinitrophloroglucinol lead is an important priming agent. Dry TNPG has high friction and impact sensitivity and low burst point, while wet TNPG has almost zero friction and impact sensitivity and high burst point temperature. Acidic phenolic hydroxyl group and adjacent strong electron-withdrawing group -NO in TNPG 2 , both the inductive effect and the conjugation effect make the negative charge on the hydroxyl oxygen better delocalized and move to the benzene ring, generating a more stable 2,4,6-trinitro-1,3,5-phe...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/37C07C201/16
CPCC07C201/12C07C201/16C07C205/37
Inventor李斌栋刘康黄瑶
OwnerNANJING UNIV OF SCI & TECH