Method for preparing 3-amino-4-amidoxime furazan by using micro-flow field reaction technology

An amidoxime-based and reaction technology, applied in the field of chemical synthesis, can solve the problems of uncontrollable safety, cumbersome operation process, violent reaction, etc., and achieve the effects of good material mixing effect, high reaction conversion rate and simple operation.

Active Publication Date: 2021-02-09
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Purpose of the invention: the present invention aims to solve the problems of cumbersome operation, violent reaction, strong heat release, uncontrollable safety, and large amount of waste water in the traditional synthetic method. The present invention provides a method for preparing 3-amino -4-Amidoxime Furazan (AAOF) Method

Method used

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  • Method for preparing 3-amino-4-amidoxime furazan by using micro-flow field reaction technology
  • Method for preparing 3-amino-4-amidoxime furazan by using micro-flow field reaction technology
  • Method for preparing 3-amino-4-amidoxime furazan by using micro-flow field reaction technology

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Experimental program
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Embodiment 1

[0036] Weigh 1.32g of malononitrile (20mmol, 1.0equiv) and add it to 5% v / v acetic acid aqueous solution to prepare a 20mL solution as material I; weigh 2.76g of NaNO 2(40mmol, 2.0equiv) was added to water to prepare a 10mL solution as material II; 2.76g of hydroxylamine hydrochloride (40mmol, 2.0equiv) was weighed and added to water to prepare a 10mL solution as material III; 1.6mL 25mol / L of sodium hydroxide (40mmol, 2.0equiv) solution, as material IV. Material I and material II are simultaneously transported to the microchannel reactor for mixing, and then transported to the low-temperature module for reaction after mixing. Among them, the flow rate of material I is 5.0mL / min, the flow rate of material II is 2.5mL / min, the inner diameter of the low temperature module microchannel reactor is 1.0mm, the length is 20m, and the volume is 15.7mL. The reaction temperature is 10°C, and the residence time of the reaction is 2.1 min. Then pump in material III and material IV in s...

Embodiment 2

[0038] Weigh 1.32g of malononitrile (20mmol, 1.0equiv) and add it to 5% v / v acetic acid aqueous solution to prepare a 20mL solution as material I; weigh 2.76g of NaNO 2 (40mmol, 2.0equiv) was added to water to prepare a 10mL solution as material II; 2.76g of hydroxylamine hydrochloride (40mmol, 2.0equiv) was weighed and added to water to prepare a 10mL solution as material III; 1.6mL 25mol / L of sodium hydroxide (40mmol, 2.0equiv) solution, as material IV. Material I and material II are simultaneously transported to the microchannel reactor for mixing, and then transported to the low-temperature module for reaction after mixing. Among them, the flow rate of material I is 5.0mL / min, the flow rate of material II is 2.5mL / min, the inner diameter of the low temperature module microchannel reactor is 1.5mm, the length is 20m, and the volume is 35.3mL. The reaction temperature was 10°C, and the residence time of the reaction was 4.7 minutes. Then pump in material III and material ...

Embodiment 3

[0040] Weigh 1.32g of malononitrile (20mmol, 1.0equiv) and add it to 5% v / v acetic acid aqueous solution to prepare a 20mL solution as material I; weigh 2.76g of NaNO 2 (40mmol, 2.0equiv) was added to water to prepare a 10mL solution as material II; 2.76g of hydroxylamine hydrochloride (40mmol, 2.0equiv) was weighed and added to water to prepare a 10mL solution as material III; 1.6mL 25mol / L of sodium hydroxide (40mmol, 2.0equiv) solution, as material IV. Material I and material II are simultaneously transported to the microchannel reactor for mixing, and then transported to the low-temperature module for reaction after mixing. Among them, the flow rate of material I is 5.0mL / min, the flow rate of material II is 2.5mL / min, the inner diameter of the low temperature module microchannel reactor is 0.8mm, the length is 20m, and the volume is 10.0mL. The reaction temperature was 10°C, and the residence time of the reaction was 1.3 minutes. Then pump in material III and material ...

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Abstract

The invention discloses a method for preparing 3-amino-4-amidoxime furazan by using a micro-flow field reaction technology. The method comprises the following steps: (1) respectively pumping a malononitrile solution and a sodium nitrite aqueous solution into a first micro-mixer in a micro-flow field reaction device at the same time, mixing, and introducing into a first module to carry out a firstreaction; (2) while the step (1) is carried out, respectively and simultaneously pumping the hydroxylamine hydrochloride aqueous solution and the effluent of the first module into a second micro-mixerin the micro-flow field reaction device for mixing; and (3) while the step (2) is carried out, respectively pumping the sodium hydroxide aqueous solution and the effluent of the second micro-mixer into a third micro-mixer in the micro-flow field reaction device at the same time, mixing, and introducing into a second module to carry out a second reaction, thereby obtaining the reaction liquid containing the 3-amino-4-amidoxime furazan. The problems that a traditional feeding process is tedious, the reaction time is long, and ice bath energy consumption is high are solved.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing 3-amino-4-amidoxime furazan by using a microflow field reaction technology. Background technique [0002] Furazan compounds are important types of high-energy-density compounds and high-nitrogen-containing compounds, which have the advantages of high energy density, stew, and high nitrogen content. Furazan ring is a five-membered ring planar structure containing 2 carbon atoms, 2 nitrogen atoms and 1 oxygen atom, and the molecular formula is C 2 N 2 Oh 2 , also known as oxadiazole ring, its nitrogen content is 37%, carbon content is 34%, oxygen content is 23%, and six electrons on the ring form a conjugated large π bond, which has a certain aromaticity. Its energy source is based on the large number of carbon-nitrogen and nitrogen-nitrogen bonds in the molecule; for the design of high-energy-density compounds containing C, H, O, and N atoms,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D271/08B01J19/00
CPCC07D271/08B01J19/0093
Inventor 郭凯孙蕲覃龙州邱江凯袁鑫段秀
Owner NANJING UNIV OF TECH
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