Bimetal organic framework material as well as preparation and application thereof

A metal-organic framework and organic framework technology are applied in the field of bimetallic adsorbents and their preparation, which can solve the problems of unsuitability for industrial application, little investigation of adjustment effect, high price, etc., so as to improve adsorption and separation performance, solve environmental problems, Efficient separation effect

Inactive Publication Date: 2017-05-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these adsorbents mainly change the properties of the structure by adjusting the organic ligands, and seldom investigate the adjustment effect of different metal ions and multiple metal ions on the channels.
Also expensive and not suitable for industrial applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: solvothermal synthesis of Ni 0.65 Mg 0.35 (HCOO) 2

[0027] (1) Weigh 4.362g Ni(NO 3 ) 2 ·6H 2 Dissolve O and 1.261g melamine in a mixed solvent of 30ml DMF and 6ml methanol, stir for 50min to form solution A; dissolve 3.1ml HCOOH in 30ml DMF, stir to form solution B, add solution B to solution A, continue stirring for 20min to obtain a mixed Solution C;

[0028] (2) 1.282g Mg(NO 3 ) 2 ·6H 2 O was added to the mixed solution C in batches, stirred for 1 h, then the mixed solution was transferred to a 120 ml autoclave with a polytetrafluoroethylene liner, sealed tightly, placed in an oven at 100°C for 36 h, and cooled naturally.

[0029] (3) Centrifuge, wash the solid with methanol (2×25 ml), and dry the solid powder at 100° C. for 10 h to obtain 3.273 g of light green powder.

[0030] N measured by Autosorb IQ-2 from Quanta Instruments 2 The specific surface area is 298.04m 2 / g (determined by Langmuir method), CH 4 / N 2 The separation factor ...

Embodiment 2

[0031] Embodiment 2: solvothermal synthesis of Ni 0.8 mn 0.2 (HCOO) 2

[0032] (1) Weigh 5.816g Ni(NO 3 ) 2 ·6H 2 O and 1.513g melamine were dissolved in a mixed solvent of 30ml DMF and 6ml methanol, stirred for 40min to form solution A; 5.6ml HCOOH was dissolved in 30ml DMF, stirred to form solution B, solution B was added to solution A, continued to stir for 20min to obtain a mixed Solution C;

[0033] (2) 1.000g Mn(NO 3 ) 2 4H 2 O was slowly added to the mixed solution C, and continued to stir for 30 minutes, then the mixed solution was transferred to a 120ml autoclave with a Teflon liner, sealed tightly, placed in a 120°C oven for 36 hours, and cooled naturally.

[0034] (3) Centrifuge, wash the solid with methanol (2×25 ml), and dry the solid powder at 100° C. for 10 h to obtain 4.132 g of light green powder.

[0035] N as measured by Autosorb IQ-2 2 The specific surface area is 313.53m 2 / g (determined by Langmuir method), CH 4 / N 2 The separation factor wa...

Embodiment 3

[0036] Embodiment 3: solvothermal synthesis of Ni 0.7 Fe 0.2 (HCOO) 2

[0037] (1) Weigh 5.816g Ni(NO 3 ) 2 ·6H 2 Dissolve O and 0.784g sodium cyanide in a mixed solvent of 40ml DMF and 12ml methanol, stir for 50min to form solution A; dissolve 3.8ml HCOOH in 20ml DMF, stir to form solution B, add solution B to solution A, and continue stirring for 20min Obtain mixed solution C;

[0038] (2) 1.616g Fe(NO 3 ) 3 9H 2 O was slowly added to the mixed solution C, and continued to stir for 30 minutes, then the mixed solution was transferred to a 120ml autoclave with a Teflon liner, sealed tightly, placed in an oven at 100°C for 48 hours, and cooled naturally.

[0039] (3) Centrifuge, wash the solid with methanol (2×25 ml), and dry the solid powder at 100° C. for 10 h to obtain 4.016 g of brick red powder.

[0040] N as measured by Autosorb IQ-2 2 The specific surface area is 265.14m 2 / g (determined by Langmuir method), CH 4 / N 2 The separation factor was 5.0.

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Abstract

The invention relates to a bimetal organic framework material adsorbent applied to methane/nitrogen separation and a preparation method thereof. The bimetal organic framework material adsorbent is a compound with super-molecular porous network structure, wherein the compound is formed by coordinating two metal ions with an organic ligand HCOOH under the action of an adjusting agent; at least one of the two metal ions is Ni(II); the coordination conditions of different metals are controlled by adjusting complexation of Ni(II) to obtain several bimetal organic framework materials with different metal ratios. The prepared adsorbent has rich micro-porous structures; the purpose of adjusting pore properties microscopically is achieved; the NH4/N2 separation effect is excellent; the material is simple to prepare and low in cost, and is extremely applicable to development and recycling of low-quality methane separated under low pressure.

Description

technical field [0001] The invention belongs to the technical field of chemical adsorbents, in particular to a bimetallic adsorbent for methane-nitrogen adsorption separation and a preparation method thereof. Background technique [0002] Energy shortage and environmental pollution are two major issues facing our country at present. Methane (CH 4 ) is an internationally recognized low-carbon clean energy. Its development and clean utilization have become one of the major strategies to solve the contradiction between energy supply and demand in my country, realize energy diversification, and maintain sustainable development of the economic environment. According to my country's energy plan, by 2020 the proportion of natural gas in primary energy consumption is planned to increase to 12%, which is equivalent to an annual consumption of 400 billion cubic meters, and the natural gas resource gap will reach 150 billion cubic meters, and the contradiction between supply and deman...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C53/06B01J20/22B01D53/02C10L3/10
CPCC07C51/418B01D53/02B01D2253/204B01J20/226C10L3/105C07C53/06
Inventor 王树东胡江亮孙天军刘小伟李德伏赵生生
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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