Method for low-temperature atmosphere-pressure hydrothermal synthesis of stephanoporate metal-organic framework

A porous metal and organic framework technology, applied in the direction of cadmium organic compounds, zinc organic compounds, etc., can solve the problems of high gas phase pressure and long synthesis time, and achieve the effects of avoiding hydrolysis, excellent thermal stability and simple method

Inactive Publication Date: 2009-05-13
CHONGQING UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] The existing hydrothermal synthesis methods for the synthesis of porous metal-organic frameworks generally need to be carried out at a temperature greater than 100°C, and the generated gas phase pressure is higher than atmospheric pressure, so a pressure-resistant reactor is required, and the synthesis takes a long time

Method used

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  • Method for low-temperature atmosphere-pressure hydrothermal synthesis of stephanoporate metal-organic framework
  • Method for low-temperature atmosphere-pressure hydrothermal synthesis of stephanoporate metal-organic framework

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: [Cd(t-FA)(NH 3 )(H 2 O)] n

[0027] 1) 1.85g (6mmol) cadmium nitrate (Cd(NO 3 ) 2 4H 2 O) be dissolved in 10ml distilled water;

[0028] 2) Put 0.696g (6mmol) of fumaric acid into 10ml of distilled water and add 5ml of ammonia water (30%, w / w) dropwise while stirring;

[0029] 3) Mix the two solutions obtained in the above step 1) and step 2), and adjust the pH value of the mixed solution to 7-10 with ammonia water (30%, w / w), and then adjust the volume of the solution to about 30ml with distilled water;

[0030] 4) After reacting at 100°C for 24 hours, it was naturally cooled to room temperature at ambient temperature to obtain a porous metal-organic framework MOF crystal product;

[0031] 5) Collect MOF crystals, wash the crystals in the solution with distilled water and absolute ethanol, and dry naturally to obtain the product.

[0032] [Cd(t-FA)(NH 3 )(H 2 O)] n Orthorhombic, P bca space group. Each t-FA molecule has 6 coordination bonds and 4 ...

Embodiment 2

[0033] Embodiment 2: [Cd 2 (NA) 4 (H 2 O) 2 ] n Synthesis

[0034] 1) 1.85g (6mmol) cadmium nitrate (Cd(NO 3 ) 2 4H 2 O) be dissolved in 10ml distilled water;

[0035] 2) Put 1.48g (12mmol) of niacin (NA) into 10ml of distilled water, and add 8ml of ammonia water (30%, w / w) dropwise while stirring;

[0036] 3) Mix the two solutions obtained above, and adjust the pH value of the mixed solution to 7-10 with ammonia water (30%, w / w), and adjust the solution volume to about 30ml with distilled water;

[0037] 4) After reacting at 80-100°C for 12 hours, naturally cool to room temperature at ambient temperature to obtain a porous metal-organic framework MOF crystal product;

[0038] 5) Collect MOF crystals, wash the crystals in the solution with distilled water and absolute ethanol, and dry naturally to obtain the product.

[0039] [Cd 2 (NA) 4 (H 2 O) 2 ] n Orthorhombic, P bca space group. its center Cd 2+ It is a distorted seven-coordination pentagonal bipyramida...

Embodiment 3

[0040] Embodiment 3: ([Zn(BDC)(NH 3 ) 2 ] n )Synthesis

[0041] 1) 1.78g (6mmol) zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) be dissolved in 10ml distilled water;

[0042] 2) 0.996g H 2 Put BDC (6mmol) (terephthalic acid) into 10ml distilled water, add ammonia water (30%, w / w) 6ml;

[0043] 3) Mix the two solutions obtained above, and adjust the pH value of the mixed solution to 7-10 with ammonia water (30%, w / w), and adjust the solution volume to about 30ml with distilled water;

[0044] 4) reacting the mixed solution obtained in step 3) at 100° C. for 4 hours, and then naturally cooling to room temperature at ambient temperature to obtain a porous metal-organic framework MOF crystal product;

[0045] 5) Collect MOF crystals, wash the crystals in the solution with distilled water and ethanol respectively, and dry naturally to obtain the product.

[0046] [Zn(BDC)(NH 3 ) 2 ] n For monoclinic crystals, each Zn 2+ by and respectively from the two BDC 2- The two carboxyl oxy...

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Abstract

The invention discloses a method for hydrothermally synthesizing a porous metal-organic framework under low temperature and normal pressure, which comprises the following steps: 1) bivalent transition metal salt is put into proper amount of distilled water to be dissolved; 2) a multidentate organic ligand is put into proper amount of distilled water, and ammonia (30 percent, W/W) is added into the solution until the organic ligand is dissolved; 3) solutions obtained in step 1) and step 2) are mixed, and diluted by the distilled water; 4) the solution obtained in step 3) reacts for 4 to 24h at a temperature of between 80 and 100 DEG C, and is naturally cooled to room temperature at an environmental temperature to obtain an MOF crystal product; and 5) the MOF crystal product obtained in step 4) is filtered, MOF crystals are colleted and washed by the distilled water and absolute ethyl alcohol respectively, and the product is obtained after the natural drying. By performing a hydrothermal reaction in an ammonia solution, the method has mild conditions needed by the synthesis, less energy consumption and time consumption, and does not need a voltage resistant reactor. Therefore, the method is simpler and has lower cost; and a porous crystal material obtained by the synthesis has potential application value in the fields of gas separation, gas storage and heterogeneous catalysis.

Description

technical field [0001] The invention relates to the field of preparation of porous crystal materials, in particular to a method for hydrothermally synthesizing a porous metal-organic coordination polymer (MOF) under low temperature and normal pressure. Background technique [0002] Porous metal-organic coordination polymer or porous metal-organic framework (Metal-Organic Framework-MOF) is a new type of functional material, which can adjust the size and shape of holes through the combination of its building blocks (metal ions and organic ligand molecules). and surface properties, thus endowing it with unique structure and characteristics, in shape-selective catalysis, enantiomer separation, gas storage, microelectronics, optoelectronics, sensors, enzyme simulation, microreactors, medical diagnosis and molecular recognition etc. have attractive application prospects. For the emergence of the application possibility of this new material in large-scale applications, such as gas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/08C07F3/06
Inventor 杨明莉鲜晓红鲜学福周元敬张新涛
Owner CHONGQING UNIV
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