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A metal-organic framework shaped body and its preparation method

A technology of metal-organic frameworks and moldings, applied in separation methods, chemical instruments and methods, products, etc., can solve the problems of low MOFs content, low compression mechanical strength, poor hydrophobicity, etc., and achieve improved mechanical strength and wear resistance Good hydrophobicity and water stability, the effect of increasing industrial application value

Active Publication Date: 2021-06-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of MOFs in the MOFs molded body prepared by the in-situ growth method is low, the specific surface area is relatively small, the adsorption capacity is much lower than that of MOFs powder, and it is easy to drop powder
[0006] CN103170315A discloses a hydrophobic honeycomb metal-organic framework for waste gas treatment. By adding auxiliary raw material organic binder and water to MOFs powder and extrusion molding, the specific surface area of ​​the prepared honeycomb metal-organic framework is as high as 1570-3760m 2 / g, the contact angle with water is greater than 120°, but the compression mechanical strength is low, the positive pressure mechanical strength is only 2.8-7.4MPa, and the lateral compression strength is 1.1-3.7 MPa
However, the MOFs prepared by this method are powder materials with low mechanical strength and wear resistance, and poor hydrophobic properties.

Method used

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  • A metal-organic framework shaped body and its preparation method
  • A metal-organic framework shaped body and its preparation method
  • A metal-organic framework shaped body and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) The specific surface area of ​​50g is 1623 m 2 / g, the pore volume is 0.71 cm 3 / g HKUST-1 powder, 2.5g alumina, 2.5g methylcellulose and 14g water were mixed, then added to a granulator for granulation, and the obtained pellets were dried at 100°C for 10h, and then dried at 200°C for 10 hours. After calcination for 10 hours, spherical HKUST-1 shaped bodies were obtained, with an average diameter of 1.0 mm.

[0036] (2) 50g spherical HKUST-1 molded body and 10 g polyvinylpyrrolidone were added to 500 ml of ethanol, and ultrasonicated for 1 h at 30 kHz to obtain a feed liquid containing modified spherical HKUST-1 molded body.

[0037] (3) 7g of methyltrimethoxysilane, 1g of nitric acid with a mass concentration of 1wt% and 9g of water were slowly added dropwise to the above-mentioned feed solution, after 1.5h of 30kHz ultrasonic, aged for 6h, filtered and separated, washed to neutrality, After drying at 100 °C for 5 h, and calcining at 200 °C for 10 h, spherical HK...

Embodiment 2

[0041] (1) The specific surface area of ​​50g is 1623 m 2 / g, the pore volume is 0.71 cm 3 / g of HKUST-1 powder, 2g of alumina, 5g of starch and 20g of water were mixed, and then added to a granulator for granulation. Spherical HKUST-1 shaped bodies with an average diameter of 2.0 mm.

[0042] (2) Add 30 g spherical HKUST-1 molded body and 10 g polyvinylpyrrolidone to 500 ml of ethanol, and ultrasonicate at 50 kHz for 2 h to obtain a feed liquid containing modified spherical HKUST-1 molded body.

[0043] (3) 11g of dimethyldimethoxysilane, 0.5g of hydrochloric acid with a mass concentration of 1wt% and 10g of distilled water were slowly added dropwise to the above-mentioned feed solution, after 1.5h of 50kHz ultrasonic, aged for 2h, filtered and separated, and washed until Neutral, after drying at 100°C for 5h, and calcining at 200°C for 12h, the spherical HKUST-1 molded body B coated with silica film on the surface can be obtained.

[0044] The average diameter of the mold...

Embodiment 3

[0046] (1) The specific surface area of ​​50g is 1057m 2 / g, the pore volume is 0.45 cm 3 / g MOF-5 powder, 10g alumina, 2g methylcellulose and 40g water were mixed, then added to a granulator for granulation, and the pellets were dried at 80°C for 2h, and then calcined at 200°C for 12h. , a spherical MOF-5 molded body with an average diameter of 1.51 mm was obtained.

[0047] (2) 50 g of spherical MOF-5 molded body and 20 g of polyvinylpyrrolidone were added to 500 ml of ethanol, and sonicated at 50 kHz for 3 hours to obtain a feed liquid containing modified spherical MOF-5 molded body.

[0048] (3) 11.5g methyltriethoxysilane, 2g acetic acid with a mass concentration of 3wt% and 20g distilled water were slowly added dropwise to the above-mentioned feed solution, after 1.5h of 50kHz ultrasonic, aged for 3h, filtered and separated, washed to medium After drying at 100 °C for 5 h, and calcining at 200 °C for 10 h, the spherical MOF-5 molded body C with a silica film on the sur...

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Abstract

The invention relates to a metal-organic framework molding and a preparation method thereof. First, after mixing MOFs materials, binders, plasticizers and water, they are added to a granulator for granulation, and the obtained pellets are dried , roasting to obtain spherical MOFs moldings; then spherical MOFs moldings and polyvinylpyrrolidone are added to the alcohol solvent, and ultrasonic treatment is performed for a certain period of time to obtain a feed solution containing modified spherical MOFs moldings; finally, the hydrophobic silanization reagent , acid catalyst and water are slowly added dropwise to the above feed liquid, ultrasonically treated for a certain period of time, aged, filtered, washed, dried and roasted to obtain a MOFs molded body coated with a hydrophobic silicon dioxide film on the surface. The metal organic framework molded body prepared by the invention has the advantages of high mechanical strength, good water stability, large specific surface area and the like.

Description

technical field [0001] The invention relates to the technical field of metal-organic framework material molding, in particular to a metal-organic framework molded body and a preparation method thereof. Background technique [0002] Metal-Organic Frameworks (MOFs) are a new family of microporous / mesoporous materials in recent years, with huge specific surface area, developed pore structure, good stability, adjustable pore channels, and chemical modification according to target requirements. Therefore, it has broad application prospects in many fields such as gas storage, gas adsorption and separation, selective and chiral catalysts, microreactors, molecular recognition, drug delivery, and optoelectronic performance applications. [0003] However, MOFs synthesized by conventional methods are usually powdered crystalline materials, which are easily blown away by gas and are not easy to be recovered, and will increase the resistance and pressure drop in the transfer process. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L87/00C08L39/06C08L1/28C08L3/02C08K3/22C08K3/36C08K7/26B01D53/02
CPCB01D53/02C08K2003/2227C08K2201/013C08L87/00C08L2205/03C08L2205/18C08L39/06C08L1/28C08K3/22C08K3/36C08L3/02C08K7/26Y02P20/151
Inventor 马蕊英张英孙兆松王刚
Owner CHINA PETROLEUM & CHEM CORP
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