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Method for synthesizing MIL-100Cr integral material by sol-gel method

A sol-gel method and monolithic technology, which is applied in the field of sol-gel synthesis of molding-free MIL-100Cr monolithic materials, can solve the problems of shortage of molding technology, large pollution, high risk, etc., and achieve green and efficient synthesis, large-scale industry The effect of applying the foreground

Active Publication Date: 2020-11-06
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems of the existing MIL-100Cr synthesis method, such as high risk, long time consumption, large pollution, and shortage of molding technology, the present invention discloses a method for synthesizing MIL-100Cr monolithic material without molding by sol-gel method. The sol-gel method is applied to the synthesis process of MIL-100Cr, not only the MIL-100Cr product is synthesized in a short time without fluorine, but also the synthesized MIL-100Cr monolithic material does not require secondary molding, and it is crushed and screened Can be filled directly into the adsorption column

Method used

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  • Method for synthesizing MIL-100Cr integral material by sol-gel method
  • Method for synthesizing MIL-100Cr integral material by sol-gel method
  • Method for synthesizing MIL-100Cr integral material by sol-gel method

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Experimental program
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Effect test

Embodiment 1

[0035]A kind of sol-gel method is synthesized the method for exempting molding MIL-100Cr integral material, and its steps are:

[0036] (1) 0.5329 g CrCl 3 ·6H 2 O, 0.22 g H 3 Add BTC and 30 mL deionized water to a 100 mL beaker in sequence, and stir at room temperature for 30 min at 700 r / min to obtain a clear solution;

[0037] (2) Transfer the clarified solution obtained in step (1) to a 100 mL polytetrafluoroethylene container, place it in a stainless steel reaction kettle, and seal it, then place the sealed reaction kettle in a constant temperature oven, and set the temperature of the oven to After heating at 220°C for 9 hours, the reactor was cooled to room temperature, and the reactor was opened to obtain a wet gel that no longer had fluidity. The heating rate and cooling rate were both 5°C / min;

[0038] (3) Transfer the wet gel obtained in step (2) to a 50mL beaker, and age at room temperature (25°C) for 7 days to obtain the MIL-100Cr dry gel precursor;

[0039] (4...

Embodiment 2

[0063] A kind of sol-gel method is synthesized the method for exempting molding MIL-100Cr integral material, and its steps are:

[0064] (1) 0.5595 g CrCl 3 ·6H 2 O, 0.24 g H 3 Add BTC and 27 mL of deionized water to a 100 mL beaker in turn, and stir at room temperature for 30 min at 700 r / min to obtain a clear solution;

[0065](2) Transfer the clarified solution obtained in step (1) to a 100 mL polytetrafluoroethylene container, place it in a stainless steel reaction kettle, and seal it, then place the sealed reaction kettle in a constant temperature oven, and set the temperature of the oven to After heating for 11 hours at 200°C, the reaction kettle was cooled to room temperature, and the reaction kettle was opened to obtain a wet gel that no longer had fluidity. The heating rate and cooling rate were both 5°C / min;

[0066] (3) Transfer the wet gel obtained in step (2) to a 50mL beaker, and age at room temperature (25°C) for 7 days to obtain the MIL-100Cr dry gel precurs...

Embodiment 3

[0069] A kind of sol-gel method is synthesized the method for exempting molding MIL-100Cr integral material, and its steps are:

[0070] (1) 0.5062 g CrCl 3 ·6H 2 O, 0.20 g H 3 Add BTC and 32 mL deionized water to a 100 mL beaker in sequence, and stir at room temperature for 30 min at 700 r / min to obtain a clear solution;

[0071] (2) Transfer the clarified solution obtained in step (1) to a 100 mL polytetrafluoroethylene container, place it in a stainless steel reaction kettle, and seal it, then place the sealed reaction kettle in a constant temperature oven, and set the temperature of the oven to After heating for 7 hours at 240°C, the reactor was cooled to room temperature, and the reactor was opened to obtain a wet gel that no longer had fluidity. The heating rate and cooling rate were both 5°C / min;

[0072] (3) Transfer the wet gel obtained in step (2) to a 50mL beaker, and age at room temperature (25°C) for 7 days to obtain the MIL-100Cr dry gel precursor;

[0073] (...

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Abstract

The invention belongs to the technical field of preparation and molding of metal organic framework materials, and discloses a method for synthesizing a forming-free MIL-100Cr integral material by a sol-gel method. Chromium chloride, trimesic acid and deionized water are mixed and stirred to be clear, a hydrothermal reaction is performed to obtain wet gel, aging is performed for 7 days to obtain anMIL-100Cr xerogel precursor, extraction is performed in ethyl alcohol, and room-temperature drying is performed to obtain compact MIL-100Cr xerogel. The MIL-100Cr integral material can be obtained within a short time under the fluoride-free condition, green and efficient synthesis of the material is achieved, the hardness of the synthesized MIL-100Cr monolithic material reaches 58.7 N / mm < 2 >, an adsorption column can be directly filled with the synthesized MIL-100Cr integral material through crushing and screening, and secondary forming is not needed; the synthesis and molding integration of MIL-100Cr is realized, and the method has certain guiding significance for the synthesis and molding of MOFs materials.

Description

technical field [0001] The invention relates to the field of preparation and molding of a metal organic framework material MIL-100Cr, in particular to a method for synthesizing a molding-free MIL-100Cr monolithic material by a sol-gel method. Background technique [0002] Metal-organic frameworks (MOFs) have attracted extensive attention from researchers due to their large specific surface area, adjustable pore size, functionalizable structure, and designability at the molecular scale. After more than 20 years of exploration, this type of material has shown good application prospects in various fields. Among them, MOFs as adsorbents can make good use of the porosity of the material to take advantage of the material. In recent years, many researchers have done a lot of research on MOFs adsorbents. This type of material has exposed many problems in the actual application process and faces many challenges. 1) Poor stability: Since coordination bonds are mainly used in MOFs, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 杨江峰张飞飞王闯李晋平
Owner TAIYUAN UNIV OF TECH
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