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Method for continuously preparing UiO series metal framework material through mother liquor dehydration circulation

A metal framework material and mother liquor technology, applied in the field of materials and chemical technology research, can solve the problems of inability to recycle multiple times, affect the reaction rate, and no reports of MOFs synthesis mother liquor, reduce the amount of DMF used, improve economic benefits, The effect of improving atom utilization

Active Publication Date: 2021-08-13
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (1) At present, there is no report on the synthesis mother solution of UiO series MOFs
[0008] (2) There will be a small amount of water accumulation in the mother liquor circulation, which will affect the reaction rate and make it impossible to recycle multiple times

Method used

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  • Method for continuously preparing UiO series metal framework material through mother liquor dehydration circulation
  • Method for continuously preparing UiO series metal framework material through mother liquor dehydration circulation
  • Method for continuously preparing UiO series metal framework material through mother liquor dehydration circulation

Examples

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Effect test

Embodiment 1

[0028] Mother liquor dehydration and recycling process for synthesizing UiO-66: adopting continuous flow method with ZrOCl ratio as raw material 2 ·8H 2 O:H 2 BDC:HAC:DMF=1:1:100:750 (molar ratio) synthesize UiO-66, collect mother liquor (the water content in mother liquor is 8.46g / L), add acetic anhydride in mother liquor, acetic anhydride and the water in synthetic mother liquor The molar ratio is 2, the mother liquor treatment time is 4h, the mother liquor treatment temperature is 60°C, the water content in the dehydrated mother liquor is 4.11g / L, and ZrOCl is added to the dehydrated mother liquor 2 ·8H 2 O, H 2 BDC and DMF, keep the ratio of reaction raw materials in the mother liquor as ZrOCl 2 ·8H 2 O:H 2 BDC:HAC:DMF=1:1:100:750 (molar ratio), after uniform mixing, use a pump to continuously pass into the coil reactor (700mL) through the T-type mixer, the reaction temperature is 140°C, the residence time is 30min, and the reaction After the end, the UiO-66 solid a...

Embodiment 2

[0034] Synthesis of UiO-66-NH by dehydration and recycling of mother liquor 2 Process: The continuous flow method is adopted, and the reaction raw material ratio is ZrOCl 2 ·8H 2 O:H 2 BDC-NH 2 :HAC:DMF=1:0.9:90:100 (molar ratio) to synthesize UiO-66-NH 2 , Collect the mother liquor (the water content in the mother liquor is 8.79g / L), add acetic anhydride to the mother liquor, the molar ratio of acetic anhydride to water in the synthesis mother liquor is 0.5, the mother liquor treatment time is 1h, the mother liquor treatment temperature is 30°C, and the mother liquor is dehydrated by acetic anhydride After the water content is 3.42g / L, in the mother liquor after dehydration, add ZrOCl 2 ·8H 2 O, H 2 BDC-NH 2 and DMF, keep the reaction raw material ratio in the mother liquor as ZrOCl 2 ·8H 2 O:H 2 BDC-NH 2 :HAC:DMF=1:1:90:100 (molar ratio), after uniform mixing, use a pump to continuously pass into the coil reactor (70mL) through the T-type mixer, the reaction tempe...

Embodiment 3

[0038] Synthesis of UiO-66-(COOH) by Dehydration and Recycle of Mother Liquor 2 Process: The continuous flow method is adopted, and the reaction raw material ratio is ZrOCl 2 ·8H 2 O:H 2 BDC-(COOH) 2 :HAC:DMF=1:1.1:160:350 (molar ratio) to synthesize UiO-66-(COOH) 2 , Collect the mother liquor (the water content in the mother liquor is 8.19g / L), add acetic anhydride to the mother liquor, the molar ratio of acetic anhydride to water in the synthesis mother liquor is 1, the mother liquor treatment time is 2h, the mother liquor treatment temperature is 50°C, and the mother liquor is dehydrated by acetic anhydride After the water content is 4.02g / L, in the mother liquor after dehydration, add ZrOCl 2 ·8H 2 O, H 2 BDC-(COOH) 2 and DMF, keep the reaction raw material ratio in the mother liquor as ZrOCl 2 ·8H 2 O:H 2 BDC-(COOH) 2 :HAC:DMF=1:1:160:350 (molar ratio), after uniform mixing, use a pump to continuously pass into the coil reactor (1000mL) through the T-type mixer...

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Abstract

The invention discloses a method for continuously preparing a UiO series metal framework material through mother liquor dehydration circulation. According to the method, acetic anhydride is added into the synthesis mother liquor of the UiO series metal framework material for dehydration, acetic anhydride reacts to form a regulator acetic acid, and then the mother liquor is continuously recycled to prepare the UiO series metal framework material, so that the problem of recycling of the mother liquor is solved, and the use amount of an organic solvent is greatly reduced; meanwhile, UiO series metal framework material products circularly synthesized by mother liquor have the same specific surface area and crystal morphology. The mother liquor can be recycled for multiple times, the use amount of the organic solvent is reduced, the operation cost is obviously reduced, and remarkable economic benefits and environmental benefits are achieved.

Description

technical field [0001] The invention relates to a process for reusing mother liquor for producing UiO series metal skeleton materials, that is, a method for continuously preparing UiO series metal skeleton materials in circulation after dehydration of the mother liquor, belonging to the research field of materials and chemical processes. Background technique [0002] UiO series metal-organic frameworks (MOFs) have high porosity, specific surface area, and rich topological structure, making them potential applications in the fields of gas storage, adsorption separation, drug delivery, and catalysis. Currently, most reports focus on the research on new material design, modification and performance development of new applications of UiO series MOFs. However, the core of transforming UiO-series MOFs into commercial materials lies in the ability to produce large-scale, high-purity, and low-cost materials. At present, the large-scale production of MOFs faces the problem of using ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 王海燕孙智聪崔群张林刘宗健陆新悦冀嵩林
Owner NANJING UNIV OF TECH
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