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Continuous synthesis method for 2-ethylhexyl nitrate

A technology of isooctyl nitrate and a synthesis method, applied in the field of continuous synthesis of isooctyl nitrate, can solve the problems of weakened adsorption and dehydration ability, easy agglomeration of anhydrous sodium sulfate, high investment and operating costs, and achieves elimination of flying temperature explosion. Dangerous, improved process safety, fast mass and heat transfer effects

Inactive Publication Date: 2019-01-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, alkali washing and water washing are usually carried out in a reaction kettle, which has low efficiency and a large amount of waste water; drying and dehydration methods include vacuum drying and dehydration, adsorbent dehydration, and dehydration using lipophilic and hydrophobic materials.
CN1031525A discloses a method for vacuum drying and dehydration, this method needs special vacuum equipment, and the investment and operation costs are high
CN1045773A discloses a dehydration process utilizing lipophilic and hydrophobic materials. The dehydration material is mainly linoleum, which has poor dehydration ability and needs further adsorption and dehydration
CN1903829A discloses a dehydration method using anhydrous sodium sulfate as an adsorbent. In this method, anhydrous sodium sulfate absorbs water and is easy to agglomerate, which affects fluid flow; regeneration and disassembly are troublesome, and the waste sodium sulfate formed after using for a certain period of time needs to be treated separately
CN101696168B discloses a method of using silica gel for rough dehydration and molecular sieve for fine dehydration. In this method, silica gel and molecular sieves have weakened adsorption and dehydration capabilities with prolonged use. additional processing

Method used

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  • Continuous synthesis method for 2-ethylhexyl nitrate

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Experimental program
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Embodiment 1

[0029] See attached figure 1 , the reactor is heated and refrigerated by a heating and cooling circulator, and the reaction temperature is controlled at 4°C. At a certain temperature, concentrated nitric acid, concentrated sulfuric acid and isooctyl alcohol are pumped into the microchannel reactor, and the flow rate of the pump is controlled to maintain The molar ratio of sulfuric acid and nitric acid is 3.0, and the molar ratio of isooctyl alcohol to nitric acid is 1.08; The solution time is 5 minutes, and the crude product of the upper layer of acidic isooctyl nitrate enters the crude product storage tank of acidic isooctyl nitrate; the reaction acid of the lower layer goes to the reaction acid storage tank.

[0030] Put the crude isooctyl nitrate into the static mixer at 200ml / min and liquid caustic soda at 8ml / min, mix in the static mixer and then enter the oil-water liquid device, stay for 5 minutes, let it stand for stratification and then flow out continuously, the uppe...

Embodiment 2

[0032] Process is with embodiment 1, and sulfuric acid and nitric acid mol ratio are changed into 2.5.

[0033] Isooctyl nitrate is light yellow and transparent, with a purity of 99.23%, a yield of 99.14%, and a water content of 40ppm.

Embodiment 3

[0035] Process is with embodiment 1, and sulfuric acid and nitric acid mol ratio are changed into 3.5.

[0036] Isooctyl nitrate is colorless and transparent, with a purity of 99.65% and a yield of 99.43%.

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Abstract

The invention provides a continuous synthesis method for 2-ethylhexyl nitrate. 2-ethylhexanol, sulfuric acid, and nitric acid are sent to a microchannel reactor by utilizing pumps; during a reaction,the flow rate of the two pumps is controlled, the molar ratio of the sulfuric acid to the nitric acid is maintained to be 3.5-2.5:1, the molar ratio of the nitric acid to the 2-ethylhexanol is 1.5-1.0:1, the residence time is 1-5 s, the reaction temperature is 0-5 DEG C; and a reaction liquid is subjected to continuous liquid separation, neutralization, and membrane filtration to obtain a productof the 2-ethylhexyl nitrate. The method has the following characteristics of utilizing a microreactor as an esterification reactor, utilizing a static mixer as a neutralization reactor, and utilizinga membrane filter as a desalination dehydration reactor. The method is continuous in operation and stable in process, is high in safety and high in production efficiency, is free of solid waste and isless in amount of waste water.

Description

technical field [0001] The invention relates to a continuous synthesis method of isooctyl nitrate, in particular to a continuous synthesis method for producing isooctyl nitrate products with a microchannel reactor. Background technique [0002] Isooctyl nitrate is an important diesel oil cetane number improver, as an additive to diesel oil, it can greatly reduce the activation energy of diesel spontaneous combustion, improve the ignition performance, and increase the cetane number. [0003] Isooctyl nitrate is an important diesel cetane number improver. Isooctyl nitrate is thermally decomposed to generate active free radicals, triggering a series of oxidation chain reactions. Adding it to diesel as an additive can greatly reduce the activation energy of diesel spontaneous combustion, improve ignition performance, and increase cetane number. [0004] Isooctyl nitrate is usually produced by reacting nitric acid with sulfuric acid and isooctyl alcohol. The reaction speed is fa...

Claims

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Application Information

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IPC IPC(8): C07C201/02C07C203/04B01J19/00
CPCB01J19/0093C07C201/02C07C203/04
Inventor 金钢任磊黄伟何志勇陶建青
Owner CHINA PETROLEUM & CHEM CORP
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