Cluster base heterocaryosis N-(phosphonic acid methyl) iminodiacetic acid trimesicate magnesium-nickel porous crystal and preparation method of porous crystal

A technology of iminodiacetic acid trimesic acid and iminodiacetic acid, which is applied in the direction of organic chemistry to achieve good adsorption performance

Inactive Publication Date: 2015-12-16
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still relatively few reports on the use of phosphonic acid and carboxylic acid as mixed ligands to construct heterometallic carboxyl coordination compounds. Using phosphonic acid and carboxylic acid as mixed ligands to synthesize carboxyl heterometallic MOFs materials is still a promising Challenging work with great significance

Method used

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  • Cluster base heterocaryosis N-(phosphonic acid methyl) iminodiacetic acid trimesicate magnesium-nickel porous crystal and preparation method of porous crystal
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  • Cluster base heterocaryosis N-(phosphonic acid methyl) iminodiacetic acid trimesicate magnesium-nickel porous crystal and preparation method of porous crystal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 0.125g (0.5mmol) nickel acetate tetrahydrate, 0.485g (1mmol) basic magnesium carbonate hexahydrate, 0.07g (0.3mmol) N- (phosphonic acid methyl) iminodiacetic acid, 0.042g (0.2mmol) 1 , 3,5-tribenzenetricarboxylic acid, 4mL distilled water were placed in 10mL polytetrafluoroethylene lining, stirred evenly at room temperature, the pH value was adjusted to 7.0 with ammonia water, and then the polytetrafluoroethylene lining was put into the stainless steel reaction shell In the oven, react at a constant temperature of 190°C for 5 days, and cool down to 30°C at a cooling rate of 10°C / min to obtain light green blocky N-(phosphonic acid methyl)iminodiacetic acid trimellitic acid magnesium nickel porous Crystal, its yield is 75%, molecular formula is [Mg 8 Ni 12 (OH) 12 (PMIDA) 4 (BTC) 4 (H 2 O) 16 ]·9H 2 O, belongs to the orthorhombic crystal system, the space group is Cmca, and the unit cell parameters β=90°, the unit cell volume is The hole size is Z=2. The p...

Embodiment 2

[0022] 0.125g (0.5mmol) nickel acetate tetrahydrate, 0.485g (1mmol) basic magnesium carbonate hexahydrate, 0.07g (0.3mmol) N- (phosphonic acid methyl) iminodiacetic acid, 0.042g (0.2mmol) 1 , 3,5-tribenzenetricarboxylic acid, 4mL distilled water were placed in 10mL polytetrafluoroethylene lining, stirred evenly at room temperature, the pH value was adjusted to 7.0 with ammonia water, and then the polytetrafluoroethylene lining was put into the stainless steel reaction shell In the oven, react at a constant temperature of 170°C for 5 days, and cool down to 30°C at a cooling rate of 10°C / min to obtain light green blocky N-(phosphonic acid methyl)iminodiacetic acid trimellitic acid magnesium nickel porous The yield of the crystal is 68%. The molecular formula, crystal structure parameters, unit cell volume and pore size are all the same as in Example 1.

Embodiment 3

[0024] 0.125g (0.5mmol) nickel acetate tetrahydrate, 0.485g (1mmol) basic magnesium carbonate hexahydrate, 0.07g (0.3mmol) N- (phosphonic acid methyl) iminodiacetic acid, 0.042g (0.2mmol) 1 , 3,5-tribenzenetricarboxylic acid, 4mL distilled water were placed in 10mL polytetrafluoroethylene lining, stirred evenly at room temperature, adjusted its pH value to 6.0 with ammonia water, and then put the polytetrafluoroethylene lining into the stainless steel reaction shell In the oven, react at a constant temperature of 190°C for 5 days, and cool down to 30°C at a cooling rate of 10°C / min to obtain light green blocky N-(phosphonic acid methyl)iminodiacetic acid trimellitic acid magnesium nickel porous Crystal, its yield is 60%, molecular formula, crystal structure parameters, unit cell volume and pore size are all identical with embodiment 1.

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Abstract

The invention discloses a cluster base heterocaryosis N-(phosphonic acid methyl) iminodiacetic acid trimesicate magnesium-nickel porous crystal and a preparation method of the porous crystal. The molecular formula of the porous crystal is [Mg<8>Ni<12>(OH)<12>(PMIDA)<4>(BTC)<4>(H2O)<16>] 9H<2>O, wherein the BTC represents negative trivalent 1,3,5-trimesic acid radicals; the PMIDA represents negative quadrivalent N-(phosphonic acid methyl) iminodiacetic acid radicals, the porous crystal has the molecular weight being 3298.102 and belongs to an orthorhombic crystal system; in a Cmca space group, the crystal cell parameters are as follows: a=28.0134(7)A, b=17.8914(4)A, c=12.7629(3)A, alpha=90 degrees, beta=90 degrees, gamma=90 degrees, the crystal cell volume is 6396.8(3)A<3>, the pore passage size is 10.81A*11.398A, and Z=2. Hydrothermal reaction is used for synthesizing the porous crystal material, and the obtained porous crystal material has good adsorption performance and has potential application prospects in the fields of petrochemical engineering, fine chemical engineering and the like.

Description

technical field [0001] The invention belongs to the technical field of crystal materials, and relates to an adsorbable carboxyl heteronuclear N-(phosphonic acid methyl) iminodiacetic acid trimesate magnesium nickel metal-organic framework porous crystal material and a preparation method thereof. Background technique [0002] Metal-organic frameworks (MOFs) are a new class of crystalline porous materials, which are mainly composed of metal ions or metal clusters and organic ligands linked by self-assembly coordination. Because of its many excellent properties, such as fluorescence, magnetism, catalytic activity, ion exchange and adsorption, etc., it has important applications in petrochemical, fine chemical and other fields. This kind of material also shows broad application prospects in molecular recognition, host-guest functional material assembly and so on. So far, the design, synthesis and development of MOFs porous materials with novel structures and different chemical ...

Claims

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Application Information

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IPC IPC(8): C07F19/00
Inventor 刘志宏张爱琴李飒英
Owner SHAANXI NORMAL UNIV
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