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A kind of preparation method of ferrocenyl conjugated microporous polymer

A conjugated microporous and ferrocene-based technology, which is applied in the field of preparing ferrocenyl-based conjugated microporous polymer polymer materials, can solve the problems of ferrocenyl-based conjugated microporous materials and achieve good results. Effects of chemical and thermal stability, high pore volume, and high BET surface area

Active Publication Date: 2017-11-28
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 is no report on ferrocene-based conjugated microporous materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 100mL three-necked flask equipped with an argon gas line, magnetic stirring and condenser, add 0.298g 1,3,6,8-tetraacetylene pyrene, 0.488g 1,1'-dibromoferrocene, 25mg tetra (Triphenylphosphine)palladium(0), 25mg cuprous iodide, 1.5ml N,N-dimethylformamide and 1.5ml triethylamine. After ultrasonic dispersion for 30 minutes, fill with nitrogen, freeze with liquid nitrogen for 10 minutes, pump air for 30 minutes with a vacuum pump, and thaw for 2 hours, and cycle three times. Slowly raise the temperature to 65°C within 2h and keep the temperature constant for 72h. After the reaction, it was cooled to room temperature, filtered, and washed three times with chloroform, distilled water, methanol, and acetone. Soxhlet extraction with methanol for 48h. The product was dried in a vacuum oven at 70°C for 24 h. The specific surface area of ​​the product is 585m 2 / g, the pore volume is 1.2cm 3 / g.

Embodiment 2

[0020] In a 100mL three-neck flask with an argon tube, magnetic stirring and condenser, add 0.57g 2,2´-bipyridine, 1g bis(1,5-cyclooctadiene)nickel(0), 0.45ml 1,5-cyclooctadiene, 0.488g 1,1'-dibromoferrocene, 0.517g 1,3,6,8-tetrabromopyrene, 36ml tetrahydrofuran and 24ml N,N-dimethylformamide. After ultrasonic dispersion for 30 minutes, fill with nitrogen, freeze with liquid nitrogen for 10 minutes, pump air for 30 minutes with a vacuum pump, and thaw for 2 hours, and cycle three times. Slowly raise the temperature to 65°C within 2h and keep the temperature constant for 72h. After the reaction, it was cooled to room temperature, filtered, and washed three times with chloroform, distilled water, methanol, and acetone. Soxhlet extraction with methanol for 48h. The product was dried in a vacuum oven at 70°C for 24 h. The specific surface area of ​​the product is 625m 2 / g, the pore volume is 1.35cm 3 / g.

Embodiment 3

[0022] In a 100mL three-neck flask with an argon tube, magnetic stirring and condenser, add 0.57g 2,2´-bipyridine, 1g bis(1,5-cyclooctadiene)nickel(0), 0.45ml 1,5-cyclooctadiene, 0.488g 1,1'-dibromoferrocene, 0.636g tetrakis(4-bromophenyl)methane, 10ml mesitylene, 26ml dioxane and 24ml N,N-dimethyl base formamide. After ultrasonic dispersion for 30 minutes, fill with nitrogen, freeze with liquid nitrogen for 10 minutes, pump air for 30 minutes with a vacuum pump, and thaw for 2 hours, and cycle three times. Slowly raise the temperature to 65°C within 2h and keep the temperature constant for 72h. After the reaction, it was cooled to room temperature, filtered, and washed three times with chloroform, distilled water, methanol, and acetone. Soxhlet extraction with methanol for 48h. The product was dried in a vacuum oven at 70°C for 24 h. The specific surface area of ​​the product is 515m 2 / g, the pore volume is 1.05cm 3 / g.

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PUM

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Abstract

The invention provides a preparation method of a ferrocene-based conjugated microporous polymer. The preparation method includes the steps that 1, 5-15% of a first construction unit, 10-20% of a second construction unit, 0.1-0.5% of a catalyst, and 75-85% of a dispersing medium are sequentially added into a container, ultrasonic dispersion is conducted for 30 minutes under the protection of inert gas, the inert gas is fed in a filled mode, freezing, air sucking and unfreezing are conducted and circulated three times, the temperature is slowly raised to 65 DEG C within 2 hours, and a thermostatic reaction is conducted for 72 hours; 2, after the reaction is ended, filtration is conducted, and washing is conducted with chloroform, distilled water, methyl alcohol and acetone four times; 3, Soxhlet extraction is conducted with methyl alcohol for 48 hours, and a product is subjected to vacuum drying for 24 hours at the temperature of 70 DEG C. A one-step method is adopted for preparing a ferrocene-based conjugated microporous polymer high molecular material, and the material has a high BET surface area and pore volume, good chemical stability and thermal stability and has potential application value on the aspects of adsorption, sewage treatment, catalyzing, gas separation, gas storage 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 a ferrocene-based conjugated microporous polymer polymer material. Background technique [0002] Porous materials have high specific surface area, large pore volume, and good thermal stability, and have potential applications in adsorption, sewage treatment, catalysis, gas separation, gas storage, and fluorescence sensing. In recent years, scientists have prepared various organic or inorganic porous materials, and some have been industrialized. [0003] Chinese patent 104817461 A discloses a dendritic conjugated microporous polymer film as a fluorescent probe for detecting TNT gas, Fe 3+ And benzene gas, high sensitivity, good repeatability, strong practicability. Chinese patent 104817461 A discloses a preparation of nitrogen-containing tridentate ligand organic polymer material, which is a kind of good adsorption material and catal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G61/12
CPCC08G61/121C08G2261/1529C08G2261/18C08G2261/312C08G2261/314C08G2261/94
Inventor 刘清泉李根
Owner HUNAN UNIV OF SCI & TECH