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Method for synthesizing isooctyl nitrate and microchannel reactor

A microchannel reactor, the technology of isooctyl nitrate, which is applied in the directions of nitrate preparation, organic chemistry, etc., can solve the problems such as the increase of operation steps and subsequent separation steps, the increase of raw material costs, etc., so as to improve the space-time yield and save equipment costs. , the effect of avoiding production accidents

Active Publication Date: 2012-04-11
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

The above two methods of adding additives all have the problems of increased operation steps and subsequent separation steps, and rising raw material costs.

Method used

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  • Method for synthesizing isooctyl nitrate and microchannel reactor
  • Method for synthesizing isooctyl nitrate and microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048]98% nitric acid and 98% concentrated sulfuric acid are used to prepare a mixed acid with a molar ratio of nitric acid and sulfuric acid of 1:2, and the temperature during the preparation of the mixed acid can be controlled below 35°C. Under normal temperature conditions, the mixed acid and liquid isooctyl alcohol are continuously pumped into the microreactor by a micro advection pump and react in the microchannel, the molar ratio of nitric acid and isooctyl alcohol is controlled to be 1.3:1, and the liquid hourly space velocity of the reactor is 4000h -1 . The reaction product flows out of the reactor continuously, and is collected in the collector at normal temperature, and the layers are statically separated, and the acid solution is separated, and the ester layer is washed with water, alkali and water until neutral. The purity of the product isooctyl nitrate reaches 99.5%, and the yield is 98.9%.

Embodiment 2

[0050] Process is the same as embodiment 1, fixed nitric acid and sulfuric acid mol ratio are 1: 2, only change the mol ratio of nitric acid and iso-octanol: nitric acid and iso-octanol are fed by stoichiometric ratio i.e. 1:1. The purity of isooctyl nitrate reaches 99.5%, and the yield is 99.1%.

Embodiment 3

[0052] Process is with embodiment 1, only changes the mol ratio of nitric acid and sulfuric acid: nitric acid and sulfuric acid mol ratio are 1: 1. The purity of isooctyl nitrate reaches 99.7%, and the yield is 98.5%.

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Abstract

The invention relates to the synthesis of isooctyl nitrate; in particular to a synthesis method of isooctyl nitrate and a microchannel reactor. Isooctyl alcohol is taken as raw material and an acid mixture of nitric acid and sulphuric acid is taken as nitrating agent, and the raw material and the nitrating agent are pumped into the microchannel reactor at normal temperature and pressure to carry out direct esterification. The process needs no catalyst or solvent, makes full use of the efficient heat and mass transfer capability of the microchannel as well as the characteristic of direct amplification and adopts two microreactors, of which one is a single-channel microreactor and the other is a multichannel microreactor; liquid hourly space velocity in the microreactor is 3000-10000h<-1>, the once-through conversion ratio of isooctyl alcohol is higher than 99% and the yield coefficient of isooctyl nitrate is higher than 98%. The process has high operation safety and high selectivity and can realize approximate isothermal operation in the reaction. The reactor is small in volume, is easy to integrate and amplify and space-time productive rate is high, thus being significant for strengthening and guaranteeing the safe production of isooctyl nitrate.

Description

technical field [0001] The present invention relates to the synthesis of isooctyl nitrate (2-EHN), specifically a kind of synthetic method and microchannel reactor of isooctyl nitrate; Octyl esters. Background technique [0002] Isooctyl nitrate is an important additive to increase the cetane number of diesel oil. Under low temperature conditions, isooctyl nitrate is thermally decomposed to generate active free radicals, which can initiate a series of oxidation chain reactions. Therefore, after isooctyl nitrate is added to diesel as an additive, it can greatly reduce the activation energy of diesel spontaneous combustion, improve the ignition performance, and increase the cetane number. [0003] Using sulfuric acid as a catalyst, nitric acid and isooctyl alcohol undergo nitration reaction to generate isooctyl nitrate. The reaction equation is as follows: [0004] HNO 3 +CH 3 (CH 2 ) 3 CH(C 2 h 5 )CH 2 OH→CH 3 (CH 2 ) 3 CH(C 2 h 5 )CH 2 ONO 2 +H 2 o [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C203/04C07C201/02
Inventor 陈光文沈佳妮焦凤军赵玉潮袁权
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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