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MOFs material capable of effectively separating acetylene mixed gas and preparation method of MOFs material

A technology of mixing gas and acetylene, applied in the field of chemistry, can solve the problems of waste, increased cost, low separation selectivity, etc.

Inactive Publication Date: 2016-02-10
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there are some shortcomings in these two methods: Method 1 needs to use noble metals as catalysts, and may cause some olefins to undergo hydrogenation reactions, which seriously increases the cost; while Method 2 needs to waste a large amount of organic solvents
There is only one case of amino-functionalized metal-organic framework UTSA-100 material to achieve this separation, but the separation selectivity is still relatively low

Method used

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  • MOFs material capable of effectively separating acetylene mixed gas and preparation method of MOFs material
  • MOFs material capable of effectively separating acetylene mixed gas and preparation method of MOFs material
  • MOFs material capable of effectively separating acetylene mixed gas and preparation method of MOFs material

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preparation example Construction

[0043] A preparation method of MOFs material for effectively separating acetylene / ethylene and acetylene / carbon dioxide mixed gas, comprising the following steps:

[0044] 1) Add a certain proportion of mixed solvent of DMA and water into the glass bottle, and then dissolve 5-(4-hydrogen-1,2,4-triazol-4-yl)-1,3-phthalic acid in the above Add a certain amount of copper salt to the mixture of DMA and water, and ultrasonicate for 5 to 15 minutes;

[0045] Among them, the volume ratio of DMA and water is 1:0.5~2,5-(4-hydrogen-1,2,4-triazol-4-yl)-1,3-benzenedicarboxylic acid, DMA and water mixed solvent The ratio of the amount of substance is 1:1433~3656, the ratio of the amount of copper salt to 5-(4-hydrogen-1,2,4-triazol-4-yl)-1,3-benzenedicarboxylic acid 1:1~4;

[0046] 2) Screw the cap on the glass bottle to seal it, then place it in an oven, and heat it from room temperature to 75-100°C;

[0047] 3) At the above-mentioned temperature of 75-100°, keep warm for 24-36 hours, ...

Embodiment 1

[0051] 1. [Cu(5TIA)]·(DMA)(H 2 O) 1.5 Preparation of materials:

[0052] (1) Dissolve 0.023 g of 5-(4-hydrogen-1,2,4-triazol-4-yl)-1,3-benzenedicarboxylic acid in N,N-dimethylacetamide (DMA) and Add 0.0095g of cuprous iodide to the water mixture (5mL, v:v=3:2), and sonicate for 10 minutes;

[0053] (2) Screw the cap on the glass bottle to seal it, then place it in an oven and heat it from room temperature to 85°C;

[0054] (3) Maintain 85°C, keep warm for 24 hours, take out the glass bottle, and cool to room temperature;

[0055] (4) Filter the solution in the glass bottle, wash the product with N,N-dimethylacetamide, and dry the product naturally at room temperature to obtain green blocky crystals;

[0056] 2. [Cu(5TIA)]·(DMA)(H 2 O) 1.5 Preparation of FJU-22 material by activation:

[0057] The prepared crystals were exchanged several times with methanol and dichloromethane respectively, and placed under the conditions of 60°C and 5μmHg to remove the solvent molecules...

Embodiment 2

[0059] 1. [Cu(5TIA)]·(DMA)(H 2 O) 1.5 Preparation of materials:

[0060] (1) Dissolve 0.023 g of 5-(4-hydrogen-1,2,4-triazol-4-yl)-1,3-benzenedicarboxylic acid in N,N-dimethylacetamide (DMA) and Add 0.017g of copper chloride dihydrate to the water mixture (5mL, v:v=3:3), and ultrasonicate for 15 minutes;

[0061] (2) Screw the cap on the glass bottle to seal it, then place it in an oven and heat it from room temperature to 75°C;

[0062] (3) Maintain 75°C for 24 hours, take out the glass bottle, and cool to room temperature;

[0063] (4) Filter the solution in the glass bottle, wash the product with N,N-dimethylacetamide, and dry the product naturally at room temperature to obtain green blocky crystals;

[0064] 2. [Cu(5TIA)]·(DMA)(H 2 O) 1.5 Preparation of FJU-22 material by activation:

[0065] The prepared crystals were exchanged with methanol several times, and placed under the conditions of 60°C and 5 μmHg to remove solvent molecules, and the activated FJU-22 new m...

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Abstract

The invention discloses a MOFs (Metal-Organic Frameworks) material capable of effectively separating acetylene mixed gas and a preparation method of the MOFs material. The material has a one-dimensional rhombus-shaped channel hole structure, the distribution of a hole diameter is 8.0 angstroms, and the area of a rhombus-shaped window is 7.1*7.1 angstrom<2>. The preparation method of the MOFs material comprises the following steps: dissolving 5-(4-hydro-1,2,4-triazole-4-yl)-1,3-phthalic acid (5TIA) into a mixed solution of N,N-dimethylacetamide and water; adding cuprous iodide and uniformly mixing by ultrasonic waves; putting the mixture into a drying oven and heating the mixture to 75-100 DEG C and keeping the heat; cooling to a room temprature and filtering; washing the mixture with the N,N-dimethylacetamide and naturally drying at a room temprature to obtain a green block-shaped crystal; exchanging for a plurality of times by using an organic solvent; and removing solvent molecules to obtain the activated MOFs material. The MOFs material [Cu(5TIA)] prepared by the invention is named as FJU-22, and can be effectively used for separating acetylene / carbon dioxide mixed gas and acetylene / ethylene mixed gas at a room temperature and normal pressure.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a MOFs material for effectively separating acetylene mixed gas and a preparation method thereof. Background technique [0002] Because acetylene gas is the raw material of many petrochemical and electronic industrial products, and at the same time, acetylene gas is expected to be used in fuel cells, which makes the separation and purification of acetylene gas an extremely important industrial process. In the separation of acetylene mixed gas, the separation of acetylene / carbon dioxide mixed gas is very challenging, because: 1. Acetylene and carbon dioxide gas have close molecular size and shape, and the three-dimensional size of acetylene molecule is 332*334 *570pm, while the three-dimensional size of carbon dioxide molecules is 318.9*333.9*536.1pm; 2. The boiling points of the two are very close, the boiling point of acetylene is -84°C, and the boiling point of car...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01D53/02
CPCY02C20/40
Inventor 项生昌姚梓竹张章静王丽华
Owner FUJIAN NORMAL UNIV
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