Preparation method and application of nanometer Cu-organic complex crystal

A kind of organic complex and nanotechnology, which is applied in the preparation of organic compounds, amino hydroxyl compounds, organic compound/hydride/coordination complex catalysts, etc., can solve the problems of energy consumption and time consumption in the preparation of composite materials, and achieve good results. Industrial application prospects, low cost of raw materials, and the effect of large specific surface area

Inactive Publication Date: 2016-04-27
SHANDONG NORMAL UNIV
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  • Abstract
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Problems solved by technology

This patent has the following deficiencies: (1) in the preparation of Cu-MOFSiO 2 At 50-70°C and 100W ultrasonic conditions, ethyl orthosilicate needs to be added dropwise in 40-70min, which shows that the preparation of the composite material consumes energy and time; (2) the metal-organic complex prepared by the invention Cu-MOF needs to be coated with shell silica on its surface to be used for catalytic reduction of 4-nitrophenol to 4-aminophenol in aqueous medium

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  • Preparation method and application of nanometer Cu-organic complex crystal
  • Preparation method and application of nanometer Cu-organic complex crystal
  • Preparation method and application of nanometer Cu-organic complex crystal

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Experimental program
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Effect test

Embodiment 1

[0041] Example 1 Preparation of Ligand H 6 L

[0042] Ligand H 6 L is prepared by heating and reacting 5-aminoisophthalic acid and cyanuric chloride under alkaline conditions. The preparation steps are as follows:

[0043] Add 0.073mol of 5-aminoisophthalic acid, 0.117mol of sodium hydroxide and 0.085mol of sodium bicarbonate into 120mL of water; stir at room temperature for 30min, add 24mL of 1,4-cyanuric chloride containing 3.68g of cyanuric chloride dropwise within 5min Dioxane solution; heat the mixture to 100°C and continue to stir for 24 hours; after cooling to room temperature, neutralize the reaction solution to pH 5 with hydrochloric acid, filter with suction and wash with distilled water for 3 times, and dry to obtain the ligand H 6 L, the productive rate is 95%;

[0044] The ligand H 6 L, the construction formula is as follows:

[0045]

Embodiment 2

[0046] Example 2 Preparation of micron-sized Cu-organic complex crystals by solvothermal method

[0047] 0.030g of H 6 L and 2 mL DMF, 2 mL DMSO and 100 μL H 2 O shaking and blending, adding 0.164g of Cu(NO 3 ) 2 ·3H 2 O After shaking and blending, add 0.9mL HBF 4 , the mixed solution was sealed in a reaction kettle, heated at 85°C for 3 days, and after natural cooling, the product was centrifuged and washed three times with anhydrous EtOH to obtain blue Cu-organic complex crystals, which were observed under a scanning electron microscope as regular octagonal crystals. Hedral crystal, the average particle size is about 20um;

[0048] Single crystal diffraction analysis shows that the Cu-organic complex crystal has the chemical formula [Cu 3 L(H 2 O) 3 ]·10H 2 O·5DMF is a 3D porous metal-organic framework, one of which consists of three Cu 2+ , a L 6- , three H 2 O molecular composition; its XRD pattern as attached figure 1 As shown, its 2θ has characteristic absor...

Embodiment 3

[0049] Embodiment 3 A kind of preparation method of nano Cu-organic complex crystal

[0050] 0.17gCu(NO3) 2 and 0.02g Ligand H 6 L was added to the mixed solvent of 0.4mLDMF and 0.4mLDMSO respectively, and the two mixtures were blended and shaken for 6 seconds to obtain the Cu-organic complex gel; the Cu-organic complex gel was aged at 100°C 2 days, cooled to room temperature, washed 3 times with ethanol, dried to obtain nano Cu-organic complex crystals;

[0051] Described nanometer Cu-organic complex crystal, the XRD comparison of the Cu-organic complex crystal that obtains with solvent method sees attached figure 1 , the XRD pattern shows that: the nano-Cu-organic complex crystal has the same characteristic absorption peak as the Cu-organic complex crystal prepared by solvothermal method, and 2θ has characteristic absorption at 4.1, 6.6, 81, 10.4, 12.1 and 16.0, This shows that the nano-Cu-organic complex crystal has the chemical formula [Cu 3 L(H 2 O) 3 ]·10H 2 The c...

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Abstract

The invention relates to a preparation method and application of a nanometer Cu-organic complex crystal, belonging to the technical fields of metal organic complexes, material science, nano-materials, chemical industry, catalysis and the like. According to the invention, cupric nitrate and 5-aminoisophthalic acid are used as main raw materials, and a metal organic complex gel method is employed to prepare the nanometer Cu-organic complex crystal. The preparation method has the advantages of low cost for raw materials, easy process and operation and low energy consumption. The nanometer Cu-organic complex crystal can realize high-efficiency catalytic reduction of 4-nitrophenol into 4-aminophenol and has good application prospect in heterogeneous catalytic reduction.

Description

technical field [0001] The invention relates to a preparation method and application of a nano-Cu-organic complex crystal, and belongs to the technical fields of metal-organic complexes, material science, nanomaterials, chemical industry, and catalysis. Background technique [0002] Metal-organic complex crystals have shown good application prospects in the fields of drug carriers, gas adsorption storage, catalysis, magnetic materials, and optical materials. Compared with other porous materials (activated carbon, zeolite molecular sieve, carbon nanotubes), its high porosity and adjustable particle size, pore surface, pore size, uniform distribution, and good thermal stability have caused many years. It has received extensive attention and research and development from many scientific researchers at home and abroad. [0003] At present, the methods for preparing metal-organic complex crystals mainly include diffusion method and solvothermal method. The diffusion method refe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/70B01J31/22C07C213/02C07C215/76
CPCB01J31/2217B01J2231/641B01J2531/0205B01J2531/16C07C213/02C07D251/70C07C215/76
Inventor 匡芮石敬民郑鲁沂迟颜辉张程程陈雪雪
Owner SHANDONG NORMAL UNIV
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