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Preparation method of acid-base bifunctional MOFs material and method for synthesizing 3,4-dimethylfurazan by using acid-base bifunctional MOFs material as catalyst

A dimethylfurazan, dual-function technology, applied in the field of compound preparation, can solve the problems of low product yield, three wastes and the like, and achieves the effects of no three wastes, easy process, and solving the reduction of catalytic effect.

Active Publication Date: 2020-01-24
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of low product yield and easy generation of three wastes in the production of 3,4-dimethylfurazan, the present invention provides a preparation method of acid-base bifunctional MOFs material and its synthesis of 3,4-dimethylfuran as a catalyst. Methylfurazan method

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  • Preparation method of acid-base bifunctional MOFs material and method for synthesizing 3,4-dimethylfurazan by using acid-base bifunctional MOFs material as catalyst
  • Preparation method of acid-base bifunctional MOFs material and method for synthesizing 3,4-dimethylfurazan by using acid-base bifunctional MOFs material as catalyst
  • Preparation method of acid-base bifunctional MOFs material and method for synthesizing 3,4-dimethylfurazan by using acid-base bifunctional MOFs material as catalyst

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Experimental program
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Effect test

specific Embodiment approach 1

[0022] In 70mL ethanol solvent, add 10mmol of Cr(NO 3 ) 3 9H 2 O (4.0g), 15mmol of 5-aminoisophthalic acid (2.70g) and 1g of phosphotungstic acid were transferred to a 100mL autoclave after magnetic stirring for 4h, and after 10mmol of hydrofluoric acid was added dropwise and stirred for 2min, the Crystallization treatment at 220°C for 8 hours, after cooling down to room temperature, washing with deionized water and ethanol three times, filtering and drying, the obtained green powdery acid-base bifunctional MOFs material is NH 2 -PTA@MIL-101(Cr)(0.34) (where 0.34 represents 1g of NH 2 - PTA content in PTA@MIL-101 (Cr)).

[0023] NH 2 -The synthesis path of PTA@MIL-101(Cr) is as follows:

[0024]

[0025] The present invention can use chromium salt, 5-aminoterephthalic acid, and phosphotungstic acid as raw materials to synthesize and prepare acid-base functionalized bifunctional modified MOFs catalyst (NH 2 -PTA@MIL-101(Cr)) is because the size of the cage structure of...

specific Embodiment approach 2

[0030] In 70mL ethanol solvent, add 10mmol of Cr(NO 3 ) 3 9H 2 O (4.0g), 100mmol of 5-aminoisophthalic acid (18.0g) and 2g of phosphotungstic acid were transferred to a 100mL autoclave after magnetic stirring for 4h, and after adding dropwise 10mmol of hydrofluoric acid and stirring for 2min, the Crystallization treatment at 180°C for 8 hours, after cooling down to room temperature, washing with deionized water and ethanol three times, filtering, and drying to obtain green powdery acid-base bifunctional MOFs material, which is NH 2 -PTA@MIL-101(Cr)(0.07) (where 0.07 represents 1g of NH 2 - PTA content in PTA@MIL-101 (Cr)).

[0031] Will NH 2 -PTA@MIL-101(Cr)(0.07) and dimethylglyoxime were added to a flask with a distillation device at a mass ratio of 1:10, then 12ml of ethylene glycol solvent was added, and vigorously stirred for 10 minutes. After the flask was placed in an oil bath at 100°C for 10 minutes, the flask was raised to 120°C for distillation, and the heating ...

specific Embodiment approach 3

[0033] In 70mL ethanol solvent, add 10mmol of Cr(NO 3 ) 3 9H 2 O (4.0g), 10mmol of 5-aminoisophthalic acid (1.80g) and 2g of phosphotungstic acid were transferred to a 100mL autoclave after magnetic stirring for 4h, and were added dropwise with 10mmol of hydrofluoric acid and stirred for 2min. Crystallization treatment at 180°C for 8 hours, after cooling down to room temperature, washing with deionized water and ethanol three times, filtering, and drying to obtain green powdery acid-base bifunctional MOFs material, which is NH 2 -PTA@MIL-101(Cr)(0.54) (where 0.54 represents 1g of NH 2 - PTA content in PTA@MIL-101 (Cr)).

[0034] Will NH 2 -PTA@MIL-101(Cr)(0.54) and dimethylglyoxime were added to a flask with a distillation device at a mass ratio of 1:10, then 12ml of ethylene glycol solvent was added, and vigorously stirred for 10 minutes. After the flask was placed in an oil bath at 100°C for 10 minutes, the flask was raised to 220°C for distillation, and the heating was...

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Abstract

The invention discloses a preparation method of an acid-base bifunctional MOFs material and a method for synthesizing 3,4-dimethylfurazan by using the acid-base bifunctional MOFs material as a catalyst, belonging to the technical field of preparation methods of compounds. The invention aims to solve the problems of low product yield and easy generation of three wastes in conventional 3,4-dimethylfurazan production. According to the preparation method, a direct synthesis process is adopted, and a chromium salt, 5-aminoterephthalic acid and phosphotungstic acid are used as raw materials for one-step synthesis of the acid-base functionalized bifunctional modified MOFs catalyst; and 3,4-dimethylfurazan is prepared by catalyzing dehydration of dimethyl glyoxime via the acid-base functionalizedbifunctional modified MOFs catalyst. According to the invention, a synergistic catalytic mechanism of acid catalytic active sites and base catalytic active sites is utilized, so the designed and prepared MOFs catalyst realizes efficient catalysis of dimethyl glyoxime dehydration to synthesize dimethyl furazan; the yield of 3,4-dimethylfurazan can reach 60% or above; and the method is easy to operate, and overcomes the technical problem that the catalytic effect is reduced due to PTA loss in the traditional catalytic process.

Description

technical field [0001] The invention relates to a preparation method of an acid-base bifunctional MOFs material and a method for synthesizing 3,4-dimethylfurazan as a catalyst, belonging to the technical field of compound preparation methods. Background technique [0002] Furazan ring is a nitrogen-heterocyclic energy-containing group, which has the characteristics of high nitrogen content, high formation enthalpy, active oxygen in the ring and good thermal stability. Research hotspots in various countries. 3,4-Dimethylfurazan is one of the important monofurazan compounds, and it is an important precursor compound for the synthesis of furoxan-like energetic materials. [0003] 3,4-Dimethylfurazan is mainly prepared by catalytic intramolecular dehydration. Researchers at home and abroad mostly use dimethyl sulfoxide and thionyl chloride as dehydrating agents, and use acetaldehyde oxime and dimethylglyoxime as raw materials to prepare dimethyl furazan. Due to the large amoun...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/34C07D271/08
CPCB01J31/34B01J2531/0213B01J2531/62C07D271/08C08G83/008
Inventor 咸漠冯德鑫梁凤兵刘卫敏
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI