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Copper metal-organic framework material based on metal copper and preparation method and application thereof

A technology of metal-organic frameworks and organic frameworks, applied in applications, chemical instruments and methods, and other chemical processes, can solve problems such as difficult removal and large molecular structure of sterols, and achieve small molecular structure, high cost, and high yield. Effect

Active Publication Date: 2021-05-04
HENAN AGRICULTURAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a copper metal-organic framework material based on metallic copper and its preparation method and application, so as to solve the problem that the sterol molecules in tobacco are difficult to be effectively removed from cigarettes due to their large and stable structure. technical problem

Method used

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  • Copper metal-organic framework material based on metal copper and preparation method and application thereof
  • Copper metal-organic framework material based on metal copper and preparation method and application thereof
  • Copper metal-organic framework material based on metal copper and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0029] Example 1: A preparation method of a copper-based metal-organic framework material

[0030] Add 10 mg (0.04 mmol) of benzimidazole diacid, 17 mg (0.1 mmol) of copper chloride dihydrate and 11 mg (0.1 mmol) of copper chloride dihydrate to a 23 mL polytetrafluoroethylene reactor at room temperature. ) l of sodium carbonate and 3 ml of N,N-dimethylformamide. After sealing, place it in an oven, raise the temperature to 100°C at a rate of 5°C per hour, react for 48 hours, and then gradually lower the temperature to room temperature at a rate of 2°C per hour. Then use 200 µL of dilute HCl with a concentration of 4 mol / L to adjust the pH, raise the temperature to 80 °C at a rate of 5 °C per hour, react for 48 hours, and then gradually lower the temperature to room temperature at a rate of 2 °C per hour. After washing with N,N-dimethylformamide solution for 3 to 4 times, green long crystals were filtered out; the yield was 80% based on copper.

[0031] The crystal structure w...

Embodiment 2

[0033] Solvent-exchange 100 mg of the metal-organic framework material obtained with 20 mL of methanol. The methanol solvent was replaced once a day. After soaking for three days, the solvent was exchanged again with 20 mL of dichloromethane. Drying was carried out in a 60 degree oven for 24 hours. Then, it was activated under vacuum at 50°C for 24 hours to obtain the metal-organic framework material after removing the solvent.

[0034]Then take 25 mg powder metal organic framework material and put it in a 50 mL round bottom flask, add 20 mg stigmasterol, 10 mL 95% ethanol, stir at room temperature for 10 min, 20 min, 30 min, 60 min, 90 min respectively , 120 min, 240 min. After filtration, the removal ability of metal-organic frameworks to stigmasterol at room temperature was tested by ferrophosphorus method, image 3 Show: this material is respectively 5%, 10%, 20%, 50%, 65%, 70% to the removal rate of stigmasterol in 10 min, 20 min, 30 min, 60 min, 90 min, 120min, 240min ...

Embodiment 3

[0035] Example 3: A preparation method of a copper-based metal organic framework material

[0036] At room temperature, add 10.2 mg (0.04 mmol) of benzimidazole diacid, 16.9 mg (0.1 mmol) of copper chloride dihydrate and 11.3 mg (0.1 mmol) to a 23 mL polytetrafluoroethylene reactor ) l of sodium carbonate and 3 ml of N,N-dimethylformamide. After sealing, place it in an oven, raise the temperature to 100°C at a rate of 5°C per hour, react for 48 hours, and then gradually lower the temperature to room temperature at a rate of 2°C per hour. Then use 200 µL of dilute HCl with a concentration of 4 mol / L to adjust the pH, raise the temperature to 80 °C at a rate of 5 °C per hour, react for 48 hours, and then gradually lower the temperature to room temperature at a rate of 2 °C per hour. Washed 4 times with N,N-dimethylformamide solution, and the green long crystals were filtered out; the yield was 83% based on copper.

[0037] The crystal structure was determined by a Supernova X-...

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Abstract

The invention discloses a copper metal-organic framework material based on metal copper. The molecular formula of the copper metal-organic framework material is C18H11N4O10.5 Cu2; the preparation method comprises the following steps: S1, adding copper chloride dihydrate, benzimidazole diacid and sodium carbonate into an N, N-dimethylformamide solution; s2, cooling the solution obtained in the step S1 to room temperature, adjusting the pH value, heating to 80 DEG C, and cooling to room temperature; s3, filtering the solution to obtain a precipitate, cleaning the precipitate with an N, N-dimethylformamide solution, and grinding after high-temperature drying to obtain a copper metal-organic framework material; s4, sequentially soaking the metal organic framework material obtained in the step S3 in methanol and dichloromethane for three days respectively; s5, activating the metal organic framework material obtained in the step S4 under a vacuum condition; and removing the solvent to obtain the metal organic framework material. The technical problem that sterol molecules in tobaccos are difficult to effectively remove from cigarettes due to large and stable structures is solved, and the material has the advantages of large pore diameter, mild reaction conditions, high yield and high adsorption.

Description

technical field [0001] The invention relates to the technical field of adsorption materials, in particular to a copper metal-organic framework material based on metallic copper and its preparation method and application. Background technique [0002] Sterols are important chemical components in tobacco, and the main sterols are stigmasterol, β-sitosterol, campesterol, and cholesterol, and ergosterol is also contained in moldy tobacco leaves. After the tobacco leaves are mature, the sterols do not contribute much to the quality of the tobacco. Studies have shown that a large number of condensed ring aromatics in the smoke tar are partly formed by the sterols during the smoking process. At present, many studies have shown that sterols are the most important precursor compounds of fused-ring aromatic hydrocarbons in smoke. Fused-ring aromatic hydrocarbons will not only affect the sensory quality of tobacco, but also have been recognized as a carcinogen. Sterol compounds can ob...

Claims

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Application Information

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IPC IPC(8): C08G83/00A24B15/38A24B15/18B01J20/22B01J20/30
CPCC08G83/008A24B15/18A24B15/385B01J20/226
Inventor 张晓平席高磊党炳俊张明月陈芝飞王清福赵旭冯颖杰
Owner HENAN AGRICULTURAL UNIVERSITY
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