Preparation method of sandwich-shaped heterostructured MOF having multiple amino functional groups used for efficiently separating C2H2/CH4

A polyamino-functional, C2H2 technology, applied in separation methods, dispersed particle separation, chemical instruments and methods, etc., to achieve good application prospects, simple steps, and improved gas selectivity.

Inactive Publication Date: 2020-12-01
朱婷婷
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of synthesizing MOF materials, if the number of amino functional groups is increased on the organic ligands during the synthesis of ligands, it will be difficult to further increase the gas selectivity of MOF materials.

Method used

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  • Preparation method of sandwich-shaped heterostructured MOF having multiple amino functional groups used for efficiently separating C2H2/CH4
  • Preparation method of sandwich-shaped heterostructured MOF having multiple amino functional groups used for efficiently separating C2H2/CH4
  • Preparation method of sandwich-shaped heterostructured MOF having multiple amino functional groups used for efficiently separating C2H2/CH4

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] S1: 0.059g Liuheshui zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 0.033g terephthalic acid, 0.011g 1,4-diazabicyclooctane were placed in a 10ml DMF beaker and ultrasonically dissolved for 10 minutes, and then moved to a polytetrafluoroethylene reactor at 120°C for reaction In two days, transparent seed crystal A was obtained;

[0028] S2: Filter the transparent MOF crystal A obtained in the previous step, and then move the crystal A to dichloromethane (CH 2 Cl 2 ) in the solution for 60 minutes for solvent exchange, filtered, and vacuum activated at 30°C to obtain activated MOF seed crystal A;

[0029] S3: 0.059g Liuheshui zinc nitrate (Zn(NO 3 ) 2 ·6H 2(2), 0.041g 2,3,5,6-tetraaminoterephthalic acid, 0.011g 1,4-diazabicyclooctane were added into a 8ml DEF beaker and ultrasonically dissolved for 3 minutes, then it was transferred To a polytetrafluoroethylene reactor, add 0.01 mmol of the activated MOF seed crystal A obtained in the previous step, and react at 120°C for t...

Embodiment 2

[0033] S1: 0.059g Liuheshui zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 0.033g terephthalic acid, 0.011g 1,4-diazabicyclooctane were placed in a 10ml DMF beaker and ultrasonically dissolved for 10 minutes, and then moved to a polytetrafluoroethylene reactor at 120°C for reaction Two days later, the activated MOF seed crystal A was obtained;

[0034] S2: The transparent crystal A obtained in the previous step is filtered, and then the crystal A is moved to dichloromethane (CH 2 Cl 2 ) in the solution for 60 minutes for solvent exchange, filtered, and vacuum activated at 30°C to obtain activated MOF seed crystal A;

[0035] S3: 0.059g Liuheshui zinc nitrate (Zn(NO 3 ) 2 ·6H 2 (2), 0.041g 2,3,5,6-tetraaminoterephthalic acid, 0.022g 1,4-diazabicyclooctane were added into a 8ml DEF beaker and ultrasonically dissolved for 3 minutes, then it was transferred To a polytetrafluoroethylene reactor, add 0.01 mmol of the activated MOF seed crystal A obtained in the previous step, and react...

Embodiment 3

[0038] S1: 0.059g Liuheshui zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 0.033g terephthalic acid, 0.011g 1,4-diazabicyclooctane were placed in a 10ml DMF beaker and ultrasonically dissolved for 10 minutes, and then moved to a polytetrafluoroethylene reactor at 120°C for reaction Two days later, the activated MOF seed crystal A was obtained;

[0039] S2: The transparent crystal A obtained in the previous step is filtered, and then the crystal A is moved to dichloromethane (CH 2 Cl 2 ) in the solution for 60 minutes for solvent exchange, filtered, and vacuum activated at 30°C to obtain activated MOF seed crystal A;

[0040] S3: 0.059g Liuheshui zinc nitrate (Zn(NO 3 ) 2 ·6H 2 (2), 0.041g 2,3,5,6-tetraaminoterephthalic acid, 0.006g 1,4-diazabicyclooctane were added into a DEF beaker with 8ml and ultrasonically dissolved for 3 minutes, then it was removed To a polytetrafluoroethylene reactor, add 0.01 mmol of the activated MOF seed crystal A obtained in the previous step, and reac...

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Abstract

The invention provides a preparation method of a sandwich-shaped heterostructured MOF crystal material having multiple amino functional groups and application of the sandwich-shaped heterostructuredMOF crystal material having multiple amino functional groups to separation of C2H2 / CH4 mixed gas. The preparation method of the MOF crystal material is characterized by comprises the following steps:firstly, synthesizing an MOF crystal A through a hydrothermal method; and removing high-boiling-point solvent molecules in the pores of the crystal A through solvent exchange and vacuumizing; with thecrystal A as a seed crystal, growing a heterostructure MOF crystal B having a sandwich shape and multiple amino functional groups on the surface of the seed crystal A through a hydrothermal synthesismethod; and conducting separation through penetration experiments, and performing vacuum activation at 30 DEG C so as to obtain the sandwich-shaped heterostructured MOF crystal material having multiple amino functional group. The separation factor of the sandwich-shaped heterostructure MOF crystal material having multiple amino functional groups on C2H2 / CH4 / He (wherein a v / v / v ratio is 15: 15: 70, and the total flow of mixed gas is 6 ml / min) reaches 6.54, so the material is a solid adsorption material for efficiently separating C2H2 and CH4.

Description

technical field [0001] The invention belongs to the field of gas adsorption and separation, and relates to the synthesis of a sandwich-shaped multi-amino functional group heterostructure MOF (metal organic framework) material, which is used in the separation of C 2 h 2 / CH 4 in the application. Background technique [0002] Low-carbon hydrocarbons such as methane, ethylene, acetylene, propylene, etc. are extremely important basic raw materials for the petrochemical industry. Among them, acetylene will react with metals to form metal acetylides, hinder the flow of gas and may even cause explosions, so from some hydrocarbon mixtures such as C 2 h 2 / CH 4 ,C 2 h 4 / C 2 h 2 It is very important to separate acetylene from [0003] Metal-organic framework (MOF) materials are an attractive class of materials assembled by organic and inorganic (metal ions and clusters) units through coordination bonds (network synthesis). Due to their ultra-high porosity, specific surface...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01D53/02B01J20/30
CPCB01D53/02B01J20/226
Inventor 朱婷婷
Owner 朱婷婷
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