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Metal-organic framework material mil-125 and its preparation method and application

A MIL-125, metal-organic framework technology, applied in the direction of organic chemistry, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of affecting the industrial scale-up process of the application of metal-organic framework materials MIL-125 , It is difficult to control the hydrolysis rate and other issues, to achieve uniform size, prevent precipitation, and large specific surface area

Active Publication Date: 2022-08-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are great difficulties in the synthesis of metal organic framework material MIL-125, because the titanium source is very easy to hydrolyze, it is difficult to control its hydrolysis rate during synthesis
Therefore, in the current synthesis methods, water must be strictly removed during the synthesis process, and most operations need to be carried out in a glove box, which seriously affects the application of the metal organic framework material MIL-125 and its industrial scale-up process

Method used

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  • Metal-organic framework material mil-125 and its preparation method and application
  • Metal-organic framework material mil-125 and its preparation method and application
  • Metal-organic framework material mil-125 and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0136] The specific batching process is as follows: add 5g of tetraethyl titanate and 10g of polyethylene glycol 200 into a three-necked flask and mix evenly, carry out a transesterification reaction under stirring, connect a distillation device, pass nitrogen protection, heat up to 175 ° C, and react Time 5 hours, the conversion rate of the transesterification reaction is 75%, connect the water pump to carry out vacuum distillation to make the transesterification reaction more complete, control the vacuum degree of the system at 3KPa, the reaction temperature is 200 ℃, the reaction time is 1 hour, the transesterification reaction The conversion rate was 92%, and the titanium polyethylene glycol ester polymer was obtained. 5 g of the obtained titanium polyethylene glycol ester polymer, 5 g of terephthalic acid, 18 ml of dimethylformamide, and 2 ml of methanol were stirred at room temperature for 2 hours, and then transferred to a stainless steel autoclave. The autoclave was se...

Embodiment 2

[0138] The specific batching process is as follows: add 5g of tetraethyl titanate and 3.13g of ethylene glycol into the three-necked flask and mix evenly, carry out the transesterification reaction under stirring, connect the distillation device, pass nitrogen protection, heat up to 100 ℃, the reaction time After 5 hours, the conversion rate of the transesterification reaction was 70%. The water pump was connected to carry out vacuum distillation to make the transesterification reaction more complete. The vacuum degree of the control system was 3KPa, the reaction temperature was 170°C, and the reaction time was 1 hour. The ratio is 90%, and the titanium glycol ester polymer is obtained. 3 g of the obtained titanium glycol ester polymer, 2 g of terephthalic acid, 9 ml of dimethylformamide, and 1.2 ml of methanol were stirred at room temperature for 2 hours, and then transferred to a stainless steel autoclave. The autoclave was sealed and put into an oven that has been raised to...

Embodiment 3

[0140] The specific batching process is as follows: add 5g of tetrabutyl titanate and 11.35g of terephthalic alcohol into a three-necked flask and mix evenly, carry out a transesterification reaction under stirring, connect a distillation device, pass nitrogen protection, heat up to 160 ° C, and react Time 5 hours, the conversion rate of the transesterification reaction is 80%, connect the water pump to carry out vacuum distillation to make the transesterification reaction more complete, control the vacuum degree of the system at 3KPa, the reaction temperature is 230 ℃, the reaction time is 1 hour, the transesterification reaction The conversion rate was 95%, and the titanium terephthalate polymer was obtained. 4 g of the obtained titanium terephthalate polymer, 6.2 g of terephthalic acid, 20 ml of dimethylformamide, and 2.3 ml of methanol were stirred at room temperature for 2 hours, and then transferred to a stainless steel autoclave. The autoclave was sealed and put into an...

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Abstract

The application discloses a metal-organic framework material MIL-125 and a preparation method and application thereof. The metal-organic framework material MIL-125 is a cake-shaped crystal block; the external specific surface area is 160-220 m 2 / g. The metal-organic framework material MIL-125 provided by this application has a large number of microporous structures, a large external specific surface area, and a higher catalytic activity in oxidation.

Description

technical field [0001] The present application relates to a metal-organic framework material MIL-125, a preparation method and application thereof, and belongs to the field of material preparation. Background technique [0002] Metal-organic framework material MIL-125 is a typical titanium-containing metal-organic framework material. It is the first titanium-doped carboxylic acid complex with crystal structure and pore structure. It is widely used in photocatalytic oxidation, adsorption and separation. . [0003] At present, there are great difficulties in the synthesis of metal organic framework material MIL-125. Since the titanium source is easily hydrolyzed, it is difficult to control its hydrolysis rate during synthesis. Therefore, in the current synthesis methods, it is necessary to strictly remove water during the synthesis process, and most of the operations need to be carried out in a glove box, which seriously affects the application of metal-organic framework mate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J31/22B01J35/10C07D301/12C07D303/04
CPCC08G83/008B01J31/1691B01J31/2239B01J35/1028B01J35/1057C07D301/12C07D303/04B01J2531/46B01J2231/72
Inventor 邢嘉成杨丽平袁丹华徐云鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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