Method for continuously synthesizing 2-ethylhexyl nitrate in micro-reactors and extracting residual acid in 2-ethylhexyl nitrate

A technology of isooctyl nitrate and micro-reactor, which is applied in the field of synthesis and refining of isooctyl nitrate, can solve the problems of long time consumption, high energy consumption, high production cost, etc., and achieve the effect of avoiding difficult deacidification and low energy consumption

Active Publication Date: 2020-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are a series of problems and hidden dangers in this production technology: first, it takes a long time to add slowly, and the long production cycle limits its industrial application, so it is difficult to realize the synthesis of EHN quickly and efficiently; second, due to the addition of concentrated sulfuric acid or The conditions under which the mixed acid exists can reduce the initial decomposition temperature of isooctyl nitrate and increase the heat sensitivity. If it exceeds 30°C, there will be a danger of explosion. The local overheating phenomenon of the local overheating phenomenon cannot be completely avoided, and the side reactions and reaction out-of-control phenomena caused

Method used

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  • Method for continuously synthesizing 2-ethylhexyl nitrate in micro-reactors and extracting residual acid in 2-ethylhexyl nitrate
  • Method for continuously synthesizing 2-ethylhexyl nitrate in micro-reactors and extracting residual acid in 2-ethylhexyl nitrate

Examples

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Effect test

Embodiment 1

[0029] Isooctyl alcohol and sulfur / nitrate mixed acid are squeezed into the first microreactor by two metering pumps to react respectively, the mol ratio of described sulfur / nitrate mixed acid is 2, and the mol ratio of nitric acid and isooctyl alcohol is 1.1:1, reaction The temperature is a constant temperature of 55°C, and the residence time of the nitrification reaction is about 30s. Wait for about 25 minutes, after the liquid two-phase interface in the separator reaches a stable state, the EHN crude product separated from the b port of the separator and the 0.5mol / L NaOH aqueous solution are pumped into the second microreactor by two metering pumps respectively, The extraction flow rate of the EHN crude product and the flow rate of isooctyl alcohol are both 1ml / min, the flow rate of the NaOH aqueous solution is 2.5ml / min, the extraction residence time of the acid-base reaction in the second microreactor is 9s, and the sample is collected at the end of the reaction Carry ou...

Embodiment 2

[0031] The process is the same as in Example 1, except that the reaction temperature in the synthesis stage of isooctyl nitrate is changed to 45° C., and the yield of isooctyl nitrate is 92.7%.

Embodiment 3

[0033] The process is the same as in Example 1, except that the concentration of the NaOH aqueous solution in the extraction stage is changed to 1.0 mol / L, and the extraction rate of residual acid in EHN is 89%.

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Abstract

The invention relates to a method for continuously synthesizing 2-ethylhexyl nitrate in micro-reactors and extracting residual acid in the 2-ethylhexyl nitrate. The method for continuously synthesizing the 2-ethylhexyl nitrate in the micro-reactors and extracting the residual acid in the 2-ethylhexyl nitrate comprises the following steps: with isooctanol and a mixed acid, with a molar ratio of sulfuric acid to nitric acid ranging from 1.5 to 2.5, as raw materials, carrying out a nitration reaction in a first micro-reactor to generate 2-ethylhexyl nitrate and a waste acid, and separating out anacid-containing 2-ethylhexyl nitrate crude product through a liquid-liquid automatic separator; and mixing the crude product and a NaOH aqueous solution in a second micro-reactor, then carrying out areaction to extract the residual acid in the 2-ethylhexyl nitratecrude product, and conducting water-oil separation to obtain the 2-ethylhexyl nitrate with an ultra low acid content. The extraction efficiency is higher than 96%. By means of the method for continuously synthesizing the 2-ethylhexyl nitrate in the micro-reactors and extracting the residual acid in the 2-ethylhexyl nitrate, continuous operation of synthesis of the 2-ethylhexyl nitrate and acid removal is achieved, the danger level is lowered, and the consumed time of acid removal is shortened, so that the production efficiency is improved.

Description

technical field [0001] The invention relates to a method for synthesizing and refining isooctyl nitrate, in particular to a method for continuously synthesizing isooctyl nitrate and removing residual acid in isooctyl nitrate using micro-reaction technology. Background technique [0002] Isooctyl nitrate (referred to as EHN) molecular formula: (C 8 h 17 O)NO 2 , also known as 2-ethylhexyl nitrate, is an important liquid energetic material in nitrate ester compounds, and is the most widely used and cost-effective diesel cetane number improver, which can participate in the degradation branch reaction of fuel before ignition , shortening the chemical flame-delay period of the fuel is of great significance to improving the performance of the fuel. [0003] In the production technology of existing isooctyl nitrate, generally adopt nitric acid mixed acid method in tank reactor, in the mode of slow dropwise, under the condition of normal temperature or lower than normal temperatu...

Claims

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Application Information

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IPC IPC(8): C07C201/02C07C203/04
CPCC07C201/02C07C203/04
Inventor 陈光文张奇焦凤军尧超群
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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