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MOF type hierarchical porous material IPD-mesonMOF-12

A multi-level pore and mesoporous technology, applied in the fields of alkali metal oxides/hydroxides, inorganic chemistry, water/sludge/sewage treatment, etc., can solve the problem of unfavorable mesopores of surfactants, clear clogging, and thermal stability No problem, etc., to achieve good lipophilic hydrophobicity, good thermal stability effect

Active Publication Date: 2016-06-15
BEIJING SIDAAN NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this patent has the following disadvantages: the so-called template agent (anionic surfactant) used for pore formation is used, which increases the production cost and the preparation process. At the same time, the use of complex surfactants is not conducive to the generation of mesopores, but because Difficult to remove completely and block some pores between particles
[0007] In the prior art, there is also a method of preparing porous MOF materials using hydrosol, which follows the synthesis method of inorganic mesoporous molecular sieves, but the obtained is still a hierarchical porous material dominated by mesoporous pores between ZIF-8 nanoparticles. The so-called template surfactant makes the pore size distribution of this material very wide, resulting in poor thermal stability and poor adsorption performance.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0039] 1.188 g (4mmol) Zn(NO 3 ) 2 6H2O and 0.656 g (8 mmol) of Hmim were added to 18 mL of absolute ethanol, and 8 mmol of sodium hydroxide was added to stir at room temperature, then transferred to a 20 mL capacity polytetrafluoroethylene reactor and sealed at 100 ° C for 6 hours. After cooling to room temperature, the jelly-like substance was dried at room temperature to form a dry gel, and then it was extracted and washed with absolute ethanol for 7 hours with a Soxhlet extractor. Remove the residual ethanol under vacuum (0.2mmHg) at 150°C to obtain the MOF-type hierarchical porous material of the present invention, with a yield of 96% (calculated by Hmim), figure 2 It is the X-ray diffraction pattern of the MOF type hierarchical porous material synthesized, and the nanoparticle particle size is less than 60nm, and Fig. 3 is the scanning electron microscope (SEM) picture of the MOF type hierarchical porous material synthesized, micropore (1.1nm) and mesoporous ( 35nm), ...

Embodiment 2

[0043] 1.188 g (4mmol) Zn(NO 3 ) 2 6H2O and 10mmol Hmim were added to 18mL of absolute ethanol, and 10mmol of sodium hydroxide was added, stirred evenly at room temperature, then transferred to a 20ml-capacity polytetrafluoroethylene reactor and sealed at 120°C for 6 hours. After cooling to room temperature, the jelly-like substance was dried at room temperature to form a dry gel, and then it was extracted and washed with absolute ethanol for 7 hours with a Soxhlet extractor. Remove the residual ethanol under vacuum (0.2mmHg) at 150°C to obtain the MOF type hierarchical porous material of the present invention, the yield is 97% (calculated by Hmim), the particle size of nanoparticles is less than 60nm, micropore (1.1nm) and mesoporous (35nm) , BET specific surface 1670M 2 / g, total pore volume 1.54cm 3 / g, mesopore volume 1.03cm 3 / g.

Embodiment 3

[0045] 1.188 g (4mmol) Zn(NO 3 ) 2 6H2O and 0.656 g (8 mmol) of Hmim were added to 15 mL of absolute ethanol, and 8 mmol of sodium hydroxide was added to stir evenly at room temperature, then transferred to a polytetrafluoroethylene reactor with a capacity of 20 mL and sealed at 120°C for 6 hours. After cooling to room temperature, the jelly-like substance was dried at room temperature to form a dry gel, and then it was extracted and washed with absolute ethanol for 7 hours with a Soxhlet extractor. Remove the residual ethanol under vacuum (0.2mmHg) at 150°C to obtain the MOF type hierarchical porous material of the present invention, the yield is 97% (calculated by Hmim), the particle size of nanoparticles is less than 60nm, micropore (1.1nm) and mesoporous (35nm) , BET specific surface 1660M 2 / g, total pore volume 1.47cm 3 / g, mesopore volume 0.97cm 3 / g.

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Abstract

The invention relates to an MOF type hierarchical porous material.The diameter of mesoporous ranges from 2 nm to 50 nm, the size of micropores is smaller than 2 nm, the BET specific surface ranges from 1300 M<2> / g to 1850 M<2> / g, the total pore volume ranges from 1.20 cm<3> / g to 2.80 cm<3> / g, and the pore volume of the mesoporous ranges from 0.5 cm<3> / g to 1.90 cm<3> / g.The preparation method comprises the following steps that 1, metal zinc salt, 2-methylimidazole, alkali and an organic solvent are stirred to be uniform and transferred into a reaction kettle to be subjected to a reaction for 2-12 h at the constant temperature of 80-130 DEG C; 2, the reaction is completed, cooling is performed to reach the room temperature, obtained gel materials are dried under the temperature of 20-50 DEG C to form a dry adhesive, and then extraction and washing are performed for 6 h or longer; 3, finally, heating is performed for 12 h or longer under the vacuum condition at the temperature of 130-150 DEG C, and then the hierarchical porous material is obtained.The micropores are from the ZIF-8 structure, the mesoporous is frame holes between particles, and the hierarchical porous material can be used for adsorbing and purifying organic pollutants.

Description

technical field [0001] The invention belongs to the technical field of porous material synthesis, and in particular relates to a MOF type hierarchical porous material and its preparation method and application. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOF), also known as metal-organic framework compounds, metal-organic coordination polymers, which use metal ions as the coordination center, and form a certain molecular structure through coordination with multidentate ligands. Space-structured complexes, also known as MOF porous materials, are a new type of inorganic-organic hybrid porous materials developed in the past 20 years. Due to its selective adsorption of some gases and organic molecules, it has been widely researched and applied in the world as a new type of porous adsorption material. [0003] Zeoliticimidazolateframework (Zeoliticimidazolateframework, ZIF) material is a new type of nanoporous material with zeolite topologic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01J20/28B01D53/02C02F1/28
CPCB01D53/02B01D2253/204B01J20/226B01J20/28066B01J20/28073B01J20/28076B01J20/2808B01J20/28083B01J2220/4812C02F1/285
Inventor 田运齐张敏刘春苗
Owner BEIJING SIDAAN NEW MATERIAL TECH
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