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Method for preparing isooctyl nitrate in micro-channel reactor

A technology of microchannel reactor and isooctyl nitrate, which is applied in the preparation of nitrate esters and organic chemistry, can solve the problems of increased separation steps and rising raw material costs, and achieve the effects of simplifying the production process, reducing energy consumption, and saving materials

Inactive Publication Date: 2016-02-17
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above two methods all introduce additives, which increases the nitration reaction steps and the subsequent separation steps of the product, and the cost of raw materials increases

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the first step, mixed acid is prepared by using nitric acid with a mass fraction of 65% and concentrated sulfuric acid with a mass fraction of 90% (the temperature during the mixed acid preparation process is controlled below 20°C), wherein the molar ratio of nitric acid to sulfuric acid is 1:3.

[0022] In the second step, the two fluids of mixed acid and iso-octanol are continuously input into the two inlets of the microchannel reactor through two high-pressure constant-flow pumps, and the molar ratio of nitric acid and iso-octanol is controlled to be 2.2:1.

[0023] In the third step, the two liquids are mixed, contacted and reacted in the microchannel reactor. Under the condition of a constant temperature water bath at 25°C, the liquid flows out from the outlet of the reactor into the receiving bottle, and the reaction product is collected.

[0024] The fourth step is to transfer the product to a separatory funnel and let it stand for stratification. The upper est...

Embodiment 2

[0026] The process is the same as in Example 1, only changing the mol ratio of nitric acid and isooctyl alcohol to 2.3:1, reacting under this condition, and detecting by gas chromatography, the yield of isooctyl nitrate is 99.3%, and the purity is 99.5%.

Embodiment 3

[0028] The process is the same as in Example 1, only changing the mass fraction of nitric acid to 75%, reacting under this condition, and detecting by gas chromatography, the yield of isooctyl nitrate is 99.1%, and the purity is 99.2%.

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Abstract

The invention discloses a method for preparing isooctyl nitrate in a micro-channel reactor. Isooctanol and nitric-sulfuric acid are taken as raw materials, no inert solvents or additives are used, and the reaction raw materials have a reaction in the micro-channel reactor. The problem of overheating of local parts during the reaction is solved through superhigh heat exchange capacity of the micro-channel reactor, a large-scale cooling system is not required to be used, and accordingly, the energy consumption is reduced; nitric-sulfuric acid obtained after the reaction can be treated simply and recycled; the problems of addition of the inert solvents or stabilizers and the like during the reaction and separation after the reaction are avoided, the production process is simplified, raw materials are saved, the energy consumption problem caused by separation is further solved, and the purity of the prepared isooctyl nitrate products can reach more than 99.0% under the condition that no purification means such as evaporation is adopted.

Description

technical field [0001] The invention relates to a method for synthesizing isooctyl nitrate in a microchannel reactor, belonging to the field of fine chemicals. Background technique [0002] Isooctyl nitrate is mainly used as a diesel additive to increase its cetane number. The cetane number is an indicator of spontaneous combustion of diesel oil, and the higher the value, the better the combustion performance of diesel oil and the better the anti-knock and anti-shock effect. Isooctyl nitrate can be thermally decomposed under low temperature conditions to produce active free radicals, which can participate in the oxidative decomposition reaction of diesel combustion, and initiate an oxidation chain reaction centered on these free radicals, so that oxidation reactions can occur at lower temperatures, improving the quality of diesel fuel. The cetane number greatly reduces the activation energy of diesel combustion, improves its ignition performance, protects diesel engine and ...

Claims

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Application Information

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IPC IPC(8): C07C203/04C07C201/02
CPCC07C201/02C07C203/04
Inventor 李斌栋刘建华胡永柯陈磊常婷
Owner NANJING UNIV OF SCI & TECH
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