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Metal-organic frame material for absorbing and storing acetylene and preparation method thereof

A metal-organic framework, acetylene technology, applied in the directions of alkali metal compounds, copper organic compounds, zinc organic compounds, etc., to achieve the effects of mild reaction conditions, high specific surface area, high acetylene adsorption and storage capacity

Active Publication Date: 2013-04-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when designing ligands, it is rare to introduce basic units that do not participate in coordination, such as pyridyl groups, etc.

Method used

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  • Metal-organic frame material for absorbing and storing acetylene and preparation method thereof
  • Metal-organic frame material for absorbing and storing acetylene and preparation method thereof
  • Metal-organic frame material for absorbing and storing acetylene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Dissolve 10g (50mmol) of 5-amino-isophthalic acid dimethyl ester in 225 mL of 15% hydrobromic acid solution, stir and cool to 0°C-5°C, add dropwise 23mL of molar Concentration is that the aqueous solution of sodium nitrite of 2.5mol / L carries out diazotization reaction, obtains diazonium salt solution;

[0026] (2) Dissolve 9.8g of cuprous bromide into 90mL of hydrobromic acid solution with a mass concentration of 15%, cool to 0°C, and add the diazonium salt solution obtained in step (1) dropwise to the solution while stirring , reacted at 0°C for 30 minutes, and then reacted at room temperature for 5 hours. After the reaction, the organic layer was separated by filtration and washed repeatedly with water. The organic layer was dissolved in dichloromethane and washed with anhydrous MgSO 4 After drying and filtering, use petroleum ether and ethyl acetate (volume ratio 8:1) as eluents to separate and purify by column chromatography to obtain 10.5 g of the product dime...

Embodiment 2

[0035] The implementation of steps (1) to (5) in this example is the same as the implementation of steps (1) to (5) in Example 1.

[0036] (6) 15 mg of 5,5'-(pyridine-2,5-diyl)-isophthalic acid and 30 mg of CuCl obtained in step (5) 2 (H 2 O) 2 Dissolve it in 8mL of N,N-dimethylacetamide (DMA) solution, then add 50μL of concentrated hydrochloric acid dropwise, place it in a 25ml seed bottle, seal it and place it in an oven at 80°C for 72 hours, take it out After repeated washing with DMA and drying, the metal-organic framework material was obtained, and the optical microscope showed rhombic crystals.

[0037] The metal-organic framework material obtained in this example is solvent-exchanged with acetone, and the solvent is exchanged at least 10 times every 15 minutes, and then activated at 0°C for 36 hours under vacuum conditions, and then activated at 100°C under vacuum conditions After 12 hours, a metal-organic framework material with unsaturated metal sites and open pore...

Embodiment 3

[0039] The implementation of steps (1) to (5) in this example is the same as the implementation of steps (1) to (5) in Example 1.

[0040] (6) 15 mg of 5,5'-(pyridine-2,5-diyl)-isophthalic acid obtained in step (5) and 30 mg of Zn(ClO 4 ) 2 (H 2 O) 6 Dissolve in a mixed solvent of N,N-diethylacetamide (DEF) and acetonitrile (8mL, 6:2, v / v), place in a 25ml seed bottle, seal and place in an oven at 80°C After reacting for 24 hours, take it out, wash it repeatedly with DMF, and dry it to obtain a metal-organic framework material, which is shown as a diamond-shaped crystal by an optical microscope.

[0041] The metal-organic framework material obtained in this example is solvent-exchanged with acetone, and the solvent is exchanged at least 10 times every 15 minutes, and then activated at 0°C for 36 hours under vacuum conditions, and then activated at 100°C under vacuum conditions After 12 hours, a metal-organic framework material with unsaturated metal sites and open pores wa...

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Abstract

The invention discloses a metal-organic frame material for absorbing and storing acetylene and a preparation method thereof. The metal-organic frame material adopts a three-dimensional network structure which is formed by transition metal ions and multitooth organic ligands 5,5'-(pyridine-2,5-dibase)-isophthalic acid through coordinate bonds or intermolecular forces. Bivalent copper, zinc, cobalt, nickel and cadmium ions are preferably selected as the transition metal ions. The metal-organic frame material has a simple preparation process and has higher specific surface area being 2000-2200m2 / g and pore volume being 1.0-1.3cm<3> / g. The multitooth organic ligands used by the material introduce an alkaline unit containing pyridine, so that the absorption and storage capacity of acetylene can be effectively increased. The materials has a higher acetylene absorption capacity under the 273-298K temperature condition, can be used under lower pressure, and can be used as a novel efficient acetylene absorption and storage material.

Description

technical field [0001] The invention relates to a metal organic framework material used for acetylene adsorption and storage and a preparation method thereof, belonging to the technical field of metal organic framework materials. Background technique [0002] As the simplest alkane containing unsaturated triple bonds, acetylene is widely used as a raw material in the fields of petrochemical, electronic industry and commercial products. At the same time, as a fuel gas, its oxyacetylene flame temperature is much higher than other fuel gases, so acetylene is also widely used in metal cutting, welding and other processing. However, acetylene is volatile, difficult to transport, and explosive (it may explode when compressed to about two atmospheres), which greatly limits its application. A common method of storing acetylene is to store it in gas cylinders containing acetone. The disadvantage of this method is that the stock is low, the extraction rate is low, and it cannot be s...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C07F1/08C07F3/06C07F3/08C07F15/06C07F15/04
Inventor 钱国栋饶兴堂蔡建锋郁建灿崔元靖杨雨王智宇樊先平王民权
Owner ZHEJIANG UNIV
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