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Metal organic framework forming body and preparation method thereof

A metal-organic framework and molding technology, applied in separation methods, chemical instruments and methods, dispersed particle separation, etc., can solve the problems of low MOFs content, low compressive mechanical strength, poor hydrophobic performance, etc. Abrasion resistance, good hydrophobicity and water stability, the effect of increasing the value of industrial applications

Active Publication Date: 2019-03-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Metal organic framework forming body and preparation method thereof
  • Metal organic framework forming body and preparation method thereof
  • Metal organic framework forming body and preparation method thereof

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 of HKUST-1 powder, 2.5g of alumina, 2.5g of methylcellulose and 14g of water were mixed, then added to the granulator for granulation, and the obtained pellets were dried at 100°C for 10h, Calcined for 10 hours, a spherical HKUST-1 molded body was obtained, with an average diameter of 1.0 mm.

[0036] (2) Add 50g of spherical HKUST-1 shaped body and 10g of polyvinylpyrrolidone into 500ml of ethanol, and ultrasonicate at 30kHz for 1h to obtain a feed solution containing modified spherical HKUST-1 shaped body.

[0037] (3) Slowly add 7g of methyltrimethoxysilane, 1g of nitric acid with a mass concentration of 1wt%, and 9g of water dropwise into the above-mentioned feed solution, after ultrasonication at 30kHz for 1.5h, age for 6h, filter and separate, wash until neutral, After drying at 100°C for 5 hours, it was fired at 200°C for 10 hours to obtain a spherical HKUST-1 molded body A w...

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 are mixed evenly, then added to a granulator for granulation, and the obtained pellets are dried at 100°C for 15h, and then calcined at 200°C for 8h to obtain Spherical HKUST-1 molded body with an average diameter of 2.0 mm.

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

[0043] (3) Slowly add 11g of dimethyldimethoxysilane, 0.5g of 1wt% hydrochloric acid and 10g of distilled water dropwise into the above-mentioned feed solution, after ultrasonication at 50kHz for 1.5h, age for 2h, filter and separate, and wash until Neutral, after drying at 100°C for 5 hours, calcining at 200°C for 12 hours, you can get spherical HKUST-1 shaped body B with a silico...

Embodiment 3

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

[0047] (2) Add 50g of spherical MOF-5 moldings and 20g of polyvinylpyrrolidone to 500ml of ethanol, and ultrasonicate at 50kHz for 3h to obtain a feed solution containing modified spherical MOF-5 moldings.

[0048] (3) Slowly add 11.5g of methyltriethoxysilane, 2g of acetic acid with a mass concentration of 3wt%, and 20g of distilled water dropwise into the above-mentioned feed liquid, after ultrasonication at 50kHz for 1.5h, age for 3h, filter and separate, and wash until medium After drying at 100°C for 5 hours, and then firing at 200°C for 10 hours, a spherical MOF-5 molded...

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Abstract

The invention relates to a metal organic framework forming body and a preparation method thereof. The preparation method comprises the following steps: blending an MOFs material, a binder, a shaping agent and water, adding the mixture in a granulator and granulating, and drying and roasting obtained pellet aggregates to obtain a spherical MOFs forming body; adding the spherical MOFs forming body and polyvinylpyrrolidone in an alcohol solvent, and carrying out ultrasonic treatment for a certain time to obtain feed liquid which contains a modified spherical MOFs forming body; and finally, slowlydropwise adding a hydrophobic silylating reagent, an acid catalyst and water in the feed liquid, carrying out ultrasonic treatment for a certain time, and ageing, filtering, washing, drying and roasting to obtain the MOFs forming body of which the surface is wrapped with a hydrophobic silicon dioxide film. The prepared metal organic framework foaming body 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 forming metal organic framework materials, in particular to a metal organic framework shaped body and a preparation method thereof. Background technique [0002] Metal-organic frameworks (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 channels, and chemical modification according to the target requirements, etc. 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 photoelectric performance applications. [0003] However, MOFs materials synthesized by conventional methods are usually powdery crystalline materials, which are easy to be blown away by gas and difficult to recycle, and will increase the resistance and pressur...

Claims

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Application Information

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Patent Type & Authority Applications(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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