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Purification method of crude hydroxyethyl hydrazine nitrate

A technology of hydroxyethylhydrazine and purification method, which is applied in the preparation of hydrazine, organic chemistry, etc., can solve the problems of high time consumption, discoloration, restriction of synthesis production process efficiency and product quality, and achieve product color improvement, short evaporation time, Effect of storage stability improvement

Active Publication Date: 2021-10-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Therefore, the pre-synthesis process limits the dehydration and concentration temperature to less than 30°C, which leads to evaporation time as long as several hours to more than ten hours
[0007] The time-consuming and discoloration problems in the dehydration and concentration process of hydroxyethylhydrazine nitrate products have seriously restricted the efficiency of its synthesis production process and product quality

Method used

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  • Purification method of crude hydroxyethyl hydrazine nitrate
  • Purification method of crude hydroxyethyl hydrazine nitrate
  • Purification method of crude hydroxyethyl hydrazine nitrate

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Embodiment 1-6

[0033] Embodiment 1-6, continuous reaction-intermittent extraction-separation-evaporation

[0034] Continuous synthesis of hydroxyethylhydrazine nitrate crude product: two metering pumps are used to continuously feed concentrated nitric acid (mass concentration 66.6%) and 99% hydroxyethylhydrazine raw materials into the microchannel reactor according to the reaction molar ratio of 1:1. Control the reaction temperature and reaction time during the reaction to obtain the crude product of hydroxyethylhydrazine nitrate.

[0035] Extraction, separation and evaporation of the crude product of hydroxyethylhydrazine nitrate: weigh the crude product, add absolute ethanol according to the mass ratio required by the process, and make the two form a mixed system in the container at room temperature, and the absolute ethanol and the aqueous phase of the crude product (comprising water in raw material concentrated nitric acid and unreacted trace nitric acid) combined to complete the mixed e...

Embodiment 7

[0039] Embodiment 7, continuous reaction-continuous extraction-continuous separation

[0040] Use two metering pumps to continuously feed concentrated nitric acid (66.6% mass concentration) and 99% hydroxyethylhydrazine raw materials into the first microchannel reactor at a reaction molar ratio of 1:1 for reaction, and control the reaction temperature and reaction time during the reaction , the product reacted by the first microchannel reactor flows through the first microchannel heat exchanger and is cooled to normal temperature to obtain a colorless crude product, which is continuously passed into the microchannel mixer 10 with the extractant absolute ethanol to form a mixed system , carry out the extraction and mass transfer process at normal temperature, the flow rate of the extraction agent is controlled by the third metering pump according to the set ratio; then, the mixed system is continuously passed into the second microchannel heat exchanger 11 for cooling, and then l...

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Abstract

The invention discloses a method for purifying a product in a process of synthesizing hydroxyethyl hydrazine nitrate in a micro-reactor. The method involves extraction, cooling separation and evaporation operation and specifically comprises the following steps of: pre-evaporating and dehydrating crude hydroxyethyl hydrazine nitrate synthesized by reaction of hydroxyethyl hydrazine and nitric acid in a micro-reactor or directly mixing the crude hydroxyethyl hydrazine nitrate with absolute ethyl alcohol at room temperature, extracting nitric acid therein by using absolute ethyl alcohol to form a mixed system, cooling, separating and settling the mixed system to form an extraction phase and a raffinate phase, and separating the raffinate phase at low temperature; and evaporating the raffinate phase at 30-70 DEG C under a vacuum condition, and removing water and ethanol in the raffinate phase to obtain a main product. According to the invention, the evaporation temperature is increased from 30 DEG C to 50-70 DEG C, and the evaporation time is greatly shortened; after purification, the concentration of the main product in the hydroxyethyl hydrazine nitrate product is increased to 97.5% or above, and the concentration of nitric acid is reduced from 0.6%-1.5% to 0.2%-0.3%; the product loss rate is lower than 3.5%; the product is lighter in color or colorless; and the extracting agent absolute ethyl alcohol is low in boiling point and is not left in the product.

Description

technical field [0001] The invention relates to a treatment method for a product of a synthesis process of hydroxyethylhydrazine nitrate, a functional component of a high-energy propellant, in particular to a method for purifying a product of hydroxyethylhydrazine nitrate synthesized in a microreactor. Background technique [0002] Hydroxyethylhydrazine nitrate (β-HEHN) is one of the important components of the new liquid propellant. It has the characteristics of low saturated vapor pressure, high density, good thermal stability, green and non-toxic, and is the mainstay of the new generation of liquid propellant technology. Functional components are focused on development by major space powers. [0003] Hydroxyethylhydrazine nitrate is prepared by the reaction of Hydroxyethylhydrazine and concentrated nitric acid. The existing preparation technology is a batch operation, which is carried out in an inert polar solvent. The U.S. Patent (US6218577B1) discloses the method in det...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14
CPCC07C241/02C07C243/14
Inventor 陈光文焦凤军韩梅尧超群杨梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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