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Preparation method of amide keyed ferrocenyl nano-porous polymer

A ferrocene-based, nano-porous technology, which is applied in the field of preparing amide-bonded ferrocene-based nano-porous polymer materials, can solve the problems of ferrocene-based nano-porous polymer materials, and achieve good results. Effects of chemical and thermal stability, high specific surface area, and high pore volume

Active Publication Date: 2016-03-02
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no reports of ferrocene-based nanoporous polymer materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a 50mL three-neck flask equipped with an argon gas conduit, magnetic stirring and condenser, add 0.926g of 1,1'-ferrocene dichloride, 0.126g of melamine, and 20ml of dimethyl sulfoxide. Under the protection of inert gas, ultrasonically disperse for 30min. Slowly raise the temperature to 180°C within 2 hours and keep the temperature constant for 72 hours. After the reaction, cool to room temperature, filter, and wash with chloroform, distilled water, methanol, and acetone three times successively, then use methanol for Soxhlet extraction for 48 hours, and finally the product is dried in a vacuum oven at 70 degrees Celsius for 24 hours. The specific surface area of ​​the product is 455m 2 / g, the pore volume is 0.95cm 3 / g.

Embodiment 2

[0016] In a 100mL three-necked flask equipped with an argon gas conduit, a magnetic stirrer and a condenser, add 0.926g of 1,1'-ferrocene dichloride, 0.123g of 1,3,5-triaminobenzene, and 20ml of N-methylpyrrolidone. Under the protection of inert gas, ultrasonically disperse for 30min. Slowly raise the temperature to 180°C within 2 hours and keep the temperature constant for 72 hours. After the reaction, cool to room temperature, filter, and wash with chloroform, distilled water, methanol, and acetone three times successively, then use methanol for Soxhlet extraction for 48 hours, and finally the product is dried in a vacuum oven at 70 degrees Celsius for 24 hours. The specific surface area of ​​the product is 525m 2 / g, the pore volume is 1.08cm 3 / g.

Embodiment 3

[0018] In a 50mL three-necked flask with an argon conduit, magnetic stirring and condenser, add 0.926g of 1,1'-ferrocene dichloride, 0.126g of tetrakis(4-aminophenyl)methane, and 20ml of sulfolane. Under the protection of inert gas, ultrasonically disperse for 30min. Slowly raise the temperature to 180°C within 2 hours and keep the temperature constant for 72 hours. After the reaction, cool to room temperature, filter, and wash with chloroform, distilled water, methanol, and acetone three times successively, then use methanol for Soxhlet extraction for 48 hours, and finally the product is dried in a vacuum oven at 70 degrees Celsius for 24 hours. The specific surface area of ​​the product is 455m 2 / g, the pore volume is 0.95cm 3 / g.

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Abstract

Provided is a preparation method of an amide keyed ferrocenyl nano-porous polymer. The preparation method comprises the steps that 5% to 15% of first construction unit, 10% to 20% of second construction unit and 75% to 90% of dispersion medium are added to a container in sequence, ultrasonic dispersion is carried out for 30 min under inert gas shielding, the container is filled with inert gas, the temperature is slowly raised to 150 DEG C within 2 h, and constant-temperature reacting is carried out for 72 h; after reacting is finished, filtering is carried out, and washing is carried out four times through chloroform, distilled water, methyl alcohol and acetone; Soxhlet extraction is carried out for 48 hr through methyl alcohol, and then a product is subjected to vacuum drying for 24 hr at the temperature of 70 DEG C. The ferrocenyl nano-porous high polymer material is prepared through the one-step method, the material has the large specific surface area and pore volume and good chemical stability and thermal stability, and the material has potential application on the aspects of adsorption, gas storage, sewage treatment, catalysis, gas separation and fluorescence sensing.

Description

technical field [0001] The invention belongs to the field of polymer material preparation, and in particular relates to a method for preparing amide bonded ferrocene-based nanoporous polymer polymer material. Background technique [0002] In recent years, organic porous polymers have potential applications in gas adsorption and separation, gas storage, heterogeneous catalysis, and optoelectronic semiconductors due to their high specific surface area and high chemical stability. Chinese patent 102887991A discloses the preparation of an organic porous polymer with a specific surface area of ​​2-7000m2g-1, which can be used in hydrogen storage, methane storage, carbon dioxide capture and other gas adsorption, heterogeneous catalysis, optoelectronic semiconductor and other fields. US Patent 2010240781-A1 discloses a conjugated microporous polymer prepared by copolymerizing 1,3,5-triynylbenzene and 1,4-diiodobenzene. It has potential applications in gas adsorption, liquid adsorp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42
CPCC08G69/42
Inventor 刘清泉李根
Owner HUNAN UNIV OF SCI & TECH
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