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Metal-organic framework material MIL-68 (Al), and preparation method and application thereof

A metal-organic framework and organic solvent technology, applied in the field of material science, can solve the problems of complex preparation and activation process, environmental pollution, and long time-consuming, and achieve the effect of good crystal shape, excellent performance, and short time-consuming

Active Publication Date: 2017-03-22
SOUTH CHINA UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation and activation process of this method is complicated, time-consuming, and a large amount of organic solvents are used in the subsequent processing of the material, which is costly and easy to cause environmental pollution.

Method used

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  • Metal-organic framework material MIL-68 (Al), and preparation method and application thereof
  • Metal-organic framework material MIL-68 (Al), and preparation method and application thereof
  • Metal-organic framework material MIL-68 (Al), and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: prepare MIL-68 (Al) material

[0029] Dissolve 4.40g of aluminum chloride hexahydrate and 0.61g of terephthalic acid in 21mL of propanol, place in a reaction kettle and stir evenly, and the resulting reaction solution rises from 60°C to 140°C at a rate of 20°C / h. Keep the temperature at 140°C for 5h, then cool down to room temperature naturally. The filtered product was washed 3 times with deionized water for 2 hours each time, and calcined at 300° C. for 5 hours in a tube furnace to obtain a sample labeled MIL-68(Al)-1. In addition, the MIL-68(Al) sample prepared by the synthesis method of MIL-68(Al) disclosed in WO2008 / 129051 is marked as MIL-68(Al)-2.

Embodiment 2

[0030] Embodiment 2: prepare MIL-68 (Al) material

[0031] Dissolve 4.40g of aluminum chloride hexahydrate and 1.53g of terephthalic acid in 21mL of propanol, place in a reaction kettle and stir evenly, and the resulting reaction solution rises from 60°C to 140°C at a rate of 15°C / h. Keep the temperature at 140°C for 10h, then cool down to room temperature naturally. The filtered product was washed 3 times with deionized water for 2 hours each time, and calcined at 300°C for 10 hours in a tube furnace to obtain a sample labeled MIL-68(Al)-3.

Embodiment 3

[0032] Embodiment 3: prepare MIL-68 (Al) material

[0033] Dissolve 4.40g of aluminum chloride hexahydrate and 0.38g of terephthalic acid in 21mL of isopropanol, place in a reaction kettle and stir evenly, and the resulting reaction solution rises from 60°C to 130°C at a rate of 20°C / h , 130 ℃ constant temperature 10h, naturally cooled to room temperature. The filtered product was washed 3 times with deionized water for 2 hours each time, and calcined at 300° C. for 10 hours in a tube furnace to obtain a sample labeled MIL-68(Al)-4.

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Abstract

The invention discloses a preparation method of a metal-organic framework material MIL-68 (Al). The method comprises the following steps: (1) dissolving a soluble aluminum salt and an organic ligand in a low boiling point organic solvent to obtain a reaction mixture solution; (2) carrying out uniform stirring and ultrasonic dispersion on the reaction mixture solution obtained in step (1) in order to obtain a reaction dispersion, carrying out gradient heating to 130-150 DEG C, carrying out a constant temperature reaction for 5-12 h, cooling the obtained reaction product to room temperature, and filtering the cooled reaction product to obtain a metal-organic framework material MIL-68 (Al) head product; and 3, washing the metal-organic framework material MIL-68 (Al) head product obtained in step (2), and heating the washed head product for activating the head product in order to obtain the purified MIL-68 (Al) material. The preparation method has the advantages of simplicity, easiness in operation, short time and easiness in large-scale production; and the prepared metal-organic framework material has good crystal form and excellent performances, and can be used as an adsorbent in the removal of azo dye molecules from water.

Description

technical field [0001] The invention belongs to the field of material science, and in particular relates to a preparation method of a metal organic framework material MIL-68 (Al) and an application of the material in the aspect of adsorbing azo dyes. Background technique [0002] Azo dyes are widely used in industries such as textile, paper, printing, food, and cosmetics. The discharge of high-chroma dye wastewater into the environment not only seriously affects water quality, but also has toxic effects on organisms and even "three-caused" effects. At present, the types of azo dyes are becoming more and more complex, and the ability of anti-photolysis, anti-oxidation, and anti-biodegradation is continuously enhanced, and the difficulty of azo dye wastewater treatment is also increasing. For the treatment of high-concentration azo dye wastewater in water, existing methods include coagulation, biodegradation, precipitation and chemical oxidation. In comparison, the adsorption...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C02F1/28C02F101/30C02F101/38C02F103/30
CPCB01J20/223C02F1/288C02F2101/308C02F2101/38C02F2103/30
Inventor 程建华武士川张鹏郑华生
Owner SOUTH CHINA UNIV OF TECH
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