Method of synthesizing isooctyl nitrate

A technology of isooctyl nitrate and nitric acid, which is applied in the field of synthesis of isooctyl nitrate (2-EHN), can solve the problems of increasing operation steps and subsequent separation steps, increasing the cost of raw materials, etc., so as to simplify post-processing and facilitate recycling , high mass transfer effect

Inactive Publication Date: 2016-05-11
CHINA PETROLEUM & CHEM CORP +1
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above two methods of adding additives all have the problem of increasing the number of

Method used

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  • Method of synthesizing isooctyl nitrate
  • Method of synthesizing isooctyl nitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Use 98% sulfuric acid and 98% nitric acid to prepare a mixed acid with a molar ratio of sulfuric acid and nitric acid of 1.35:1.

[0027] Use a heating and cooling circulator to heat and cool the reactor. Set the temperature of the reactor at 10°C. After the temperature is stable, pump the mixed acid into the reactor at a flow rate of 32mL / min; pump isooctanol into the reactor In the process, the flow rate is controlled at 40mL / min, the material reacts in the microchannel reactor, the reaction residence time is 8s, and the reaction pressure is 0.5MPa. The phase is washed with water, alkali and washed with water until neutral, and dried to remove moisture. Isooctyl nitrate is colorless and transparent, with a purity of 98.70% and a yield of 96.50%.

Embodiment 2

[0029] Use 98% sulfuric acid and 98% nitric acid to prepare a mixed acid with a molar ratio of sulfuric acid and nitric acid of 1.80:1.

[0030] Use a heating and cooling circulator to heat and cool the reactor. Set the temperature of the reactor at 10°C. After the temperature is stable, pump the mixed acid into the reactor with a flow rate of 36mL / min; pump isooctanol into the reactor In the process, the flow rate is controlled at 36mL / min, the material reacts in the microchannel reactor, the reaction residence time is 8s, and the reaction pressure is 0.5MPa. The phase is washed with water, alkali and washed with water until neutral, and dried to remove moisture. Isooctyl nitrate is colorless and transparent, with a purity of 99.92% and a yield of 98.54%.

Embodiment 3

[0032] Use 98% sulfuric acid and 98% nitric acid to prepare a mixed acid with a molar ratio of sulfuric acid and nitric acid of 1.80:1.

[0033] Heating and refrigeration circulators are used to heat and cool the reactor. Set the temperature of the reactor to 20°C. After the temperature is stable, pump the mixed acid into the reactor with a flow rate of 36mL / min; pump isooctanol into the reactor In the process, the flow rate is controlled at 36mL / min, the material reacts in the microchannel reactor, the reaction residence time is 8s, and the reaction pressure is 0.5MPa. The phase is washed with water, alkali and washed with water until neutral, and dried to remove moisture. Isooctyl nitrate is colorless and transparent, with a purity of 98.51% and a yield of 96.54%.

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Abstract

The invention relates to a method of synthesizing isooctyl nitrate. The method comprises the steps that mixed acid obtained by mixing concentrated nitric acid and concentrated sulfuric acid and isooctyl alcohol are conveyed into a micro-channel reactor through conveying equipment for a reaction for 5-60 seconds in the reactor at the temperature of 5-50 DEG C, the reaction product stands for skimming, and the organic phase is washed and dried to obtain the isooctyl nitrate. According to the method, the reaction is performed in a triangular three-layer structure reaction plate, mass and heat transfer is quick, the reaction can be performed at constant temperature, and operation safety is high. In the process, the single-pass conversion rate of the isooctyl alcohol is 99% or above, and the yield is also 99% or above.

Description

technical field [0001] The invention relates to the synthesis of isooctyl nitrate (2-EHN), a method for synthesizing isooctyl nitrate in a "heart" microchannel reactor. Background technique [0002] 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. [0003] Concentrated sulfuric acid catalyzes the nitration reaction of nitric acid and isooctyl alcohol to generate isooctyl nitrate and water. The nitrification reaction speed is fast and the heat release is large, and the generated water dilutes the concentrated sulfuric acid to release a large amount of heat. If the heat is not removed in time, the reaction temperature will rise, causing side reactions such as oxidation, an...

Claims

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Application Information

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IPC IPC(8): C07C203/04C07C201/02
Inventor 金钢黄伟何志勇陶建青任磊
Owner CHINA PETROLEUM & CHEM CORP
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