Method for continuously preparing 3, 4-bis(4'-aminofurazan-3'-yl) furoxan by adopting micro-channel reactor

A microchannel reactor, aminofurazan technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, organic chemistry, etc., can solve the problems of uncontrollable large-scale production safety, difficult engineering applications, " There are many problems such as the discharge of three wastes, etc., to achieve the effect of improving the conversion rate of raw materials, good mixing effect of materials, and improving reaction selectivity.

Active Publication Date: 2021-02-05
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the traditional process has a series of problems such as cumbersome operation process, uncontrollable safety o

Method used

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  • Method for continuously preparing 3, 4-bis(4'-aminofurazan-3'-yl) furoxan by adopting micro-channel reactor
  • Method for continuously preparing 3, 4-bis(4'-aminofurazan-3'-yl) furoxan by adopting micro-channel reactor
  • Method for continuously preparing 3, 4-bis(4'-aminofurazan-3'-yl) furoxan by adopting micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Weigh 1.43g (10mmol, 1.0equiv) of 3-amino-4-amidoxime furazan (AAOF), add 14mL water and 6mL concentrated hydrochloric acid (37%) respectively, stir and dissolve it fully, use it as material Ⅰ, and draw it with a syringe Then place it on the syringe pump; Weigh 0.69g of sodium nitrite (NaNO 2 , 10mmol, 1.0equiv) after adding appropriate distilled water and fully stirring to dissolve, it was prepared into a 10mL solution as material II, which was sucked with a syringe and placed on the syringe pump; next, 0.3mol / L Na 2 CO 316mL of the solution, as material III, was drawn up with a syringe and placed on the syringe pump. After the feed pump is set at an appropriate flow rate, it pumps in material I and material II at the same time, and after being fully mixed, the materials are transported to the microflow field reaction module 1 for reaction. Among them, the internal diameter of the pipeline used in the micro-flow field reaction module 1 is 1.5mm, the length is 10m, an...

Embodiment 2

[0042] Weigh 1.43g (10mmol, 1.0equiv) of 3-amino-4-amidoxime furazan (AAOF), add 14mL water and 6mL concentrated hydrochloric acid (37%) respectively, stir and dissolve it fully, use it as material Ⅰ, and draw it with a syringe Then place it on the syringe pump; weigh 0.69g NaNO 2 (10mmol, 1.0equiv) was dissolved with an appropriate amount of distilled water, and prepared into a 10mL solution as material II, which was sucked with a syringe and placed on a syringe pump; measure 0.3mol / L of Na 2 CO 3 16 mL of the solution was used as material III. After the feed pump is set at an appropriate flow rate, it pumps in material I and material II at the same time, mixes them and transports them to the microflow field reaction module 1 for reaction. Among them, the inner diameter of the pipeline of the micro-flow field reaction module 1 is 2.0mm, the length of the tube is 6m, and the volume is 18.4mL. / min, the reaction residence time is 2.5min. Then the material III is pumped in t...

Embodiment 3

[0044] Weigh 1.43g (10mmol, 1.0equiv) of 3-amino-4-amidoxime furoxan (AAOF), add 14mL of water and 6mL of concentrated hydrochloric acid (37%) to fully stir and dissolve respectively, and use it as material Ⅰ. Place it on the syringe pump; weigh 0.69g NaNO 2 (10mmol, 1.0equiv) was dissolved in appropriate distilled water to prepare a 10mL solution, as material Ⅱ, suck it up with a syringe and put it on the syringe pump; after sucking it up with a syringe, put it on the syringe pump; 2 CO 3 16mL of the solution, as material III, was drawn up with a syringe and placed on the syringe pump. After the feed pump is set at an appropriate flow rate, it pumps in material I and material II at the same time, mixes them and transports them to the microflow field reaction module 1 for reaction. Among them, the microflow field reaction module 1 has an inner diameter of 1.0mm, a length of 20m, a volume of 15.7mL, and a reaction temperature of 20°C; the flow rate of material I is 5.0mL / min,...

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Abstract

The invention discloses a method for continuously preparing 3, 4-bis(4'-aminofurazan-3'-yl) furoxan by adopting a micro-channel reactor The method comprises the following steps of (1) respectively pumping a 3-amino-4-amidoxime furazan solution and a sodium nitrite aqueous solution into a first micro-mixer in a micro-channel reactor device at the same time, mixing, and introducing into a first reaction module to carry out a first reaction, and (2) while the step (1) is carried out, respectively pumping the effluent of the first reaction module and a sodium carbonate solution into a second micro-mixer in the micro-channel reactor device at the same time, mixing, and introducing into the second reaction module to carry out a second reaction, thereby obtaining the effluent containing 3, 4-bis(4'-aminofurazan-3'-yl) furazan. The invention relates to an intermediate 3-amino-4-amidoxime furazan needing to be separated, and efficient and continuous preparation of 3, 4-bis(4'-aminofurazan-3'-yl) furoxan is realized through a one-pot two-step method.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for continuously preparing 3,4-bis(4'-aminofurazan-3'-yl)furazan oxide (DATF) by using a microchannel reactor. Background technique [0002] Furazan compounds have the characteristics of high standard formation enthalpy, rich in nitrogen and oxygen, high energy, high density, and good molecular thermodynamic stability. Zan group is a very effective structural unit and a class of energetic compounds with important development and application value. And 3,4-bis(4'-aminofurazan-3'-yl)furazan oxide (DATF) is an important furazan compound, which can be synthesized by using DATF as a precursor containing nitro and azido , azo group, azo oxide group and other series of excellent new compounds. [0003] At present, the common synthesis method of DATF is to use malononitrile as the initial raw material to prepare the key intermediate AAOF through nitrosation reacti...

Claims

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Application Information

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IPC IPC(8): C07D271/08B01J19/00
CPCC07D271/08B01J19/0093B01J2219/00867B01J2219/00871
Inventor 郭凯袁鑫邱江凯覃龙州孙蕲段秀
Owner NANJING UNIV OF TECH
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