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A kind of 5-isonicotinamide pyridyl isotitanic acid porous copper complex and its preparation method and application

A technology of isonicotinamide pyridyl and isotitanic acid, which is applied in the preparation of organic compounds, the preparation of carboxylic acid nitrile, copper organic compounds, etc., can solve the problems of long catalytic reaction time and low catalytic efficiency, and achieves good repeated use effect. , The effect of stable catalytic performance and high reaction conversion rate

Active Publication Date: 2016-02-03
HENGYANG NORMAL UNIV
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  • Claims
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Problems solved by technology

It has been reported that a new type of complex material made of 1,3,5-benzenetricarboxylic acid tris[N-(4-pyridyl)amide or 2-aminobenzoic acid has catalytic performance for partial heterogeneous Knovevenagel condensation However, the catalytic reaction time of the former is as long as 12 hours, and the catalytic efficiency of the latter is also lower than 70%.

Method used

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  • A kind of 5-isonicotinamide pyridyl isotitanic acid porous copper complex and its preparation method and application
  • A kind of 5-isonicotinamide pyridyl isotitanic acid porous copper complex and its preparation method and application
  • A kind of 5-isonicotinamide pyridyl isotitanic acid porous copper complex and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Dissolve 5-isonicotinamide pyridylisotitanic acid (28.7mg, 0.1mmol) and copper perchlorate (37.2mg, 0.1mmol) in DMAc (10mL), seal it in a 16mL reaction vessel, and heat at 10°C per hour Heating rate to 130°C, maintaining this temperature for 3 days, and then naturally cooling to room temperature, blue columnar crystals can be obtained, the crystals are separated, washed and dried successively to obtain the target product with a yield of about 42%. The main infrared absorption peaks are: 3214m, 2928m, 2361m, 1615s, 1546s, 1429m, 1356m, 1278s, 1227s, 1089s, 1025m, 940s, 913s, 845s, 778s, 702m.

[0030] The catalytic performance experiment of the prepared porous copper complex:

[0031] Its catalytic reaction step is as follows: add benzaldehyde (2.1mmol, 0.2229g) in round bottom flask, malononitrile (2.0mmol, 0.1321g), catalyst Cu-MOF (0.037g, 0.08mmol (4wt%)), wherein Benzene (6mL) was used as a solvent and reacted for 4h at 30°C. The conversion rate of the reaction was...

Embodiment 2

[0045] Dissolve 5-isonicotinamide pyridylisotitanic acid (43.1mg, 0.15mmol) and copper perchlorate (55.3mg, 0.15mmol) in DMAc (10mL), seal it in a 16mL reaction vessel, and heat at 10°C per hour Heating rate to 110°C, maintaining this temperature for 3 days, then naturally cooling down to room temperature, blue columnar crystals can be obtained, the crystals are separated, washed and dried successively to obtain the target product with a yield of about 51%.

[0046] The heterogeneous reaction of benzaldehyde and malononitrile catalyzed by 5-isonicotinamide pyridyl isotitanic acid porous copper complex is carried out according to the steps and conditions of Example 1, the conversion rate of benzaldehyde is 98.5%, the catalyst is circulated 3 times, and the benzene The conversion rate of formaldehyde did not drop significantly, and the catalyst was basically not lost.

Embodiment 3

[0048] Dissolve 5-isonicotinamide pyridylisotitanic acid (43.1mg, 0.15mmol) and copper chloride (25.4mg, 0.15mmol) in DMAc (10mL), seal it in a 16mL reaction vessel, and set the temperature at 10°C per hour Heating rate to 110°C, maintaining this temperature for 3 days, and then naturally cooling down to room temperature, blue columnar crystals can be obtained, the crystals are separated, washed and dried successively to obtain the target product with a yield of about 47%.

[0049] 5-isonicotinamide pyridyl isotitanic acid porous copper complex catalyzes the heterogeneous reaction steps and conditions of benzaldehyde and malononitrile according to the examples, the conversion rate of benzaldehyde is 98.6%, the catalyst is circulated 3 times, the benzaldehyde The conversion rate did not decrease significantly, and the catalyst was basically not lost.

[0050] Table 1 The main crystallographic data of the complex

[0051]

[0052] a R 1 (F)=||F o |-|F c || / S|F o |, wR ...

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Abstract

The invention discloses a 5-isonicotinamide-pyridyl-isophthalic acid porous copper complex, as well as a preparation method and application thereof. The porous copper complex comprises a (3,6) dual-node three-dimensional topology lattice structure; the chemical formula of the porous copper complex is [Cu(L)].DMAc.H2O, wherein L is 5-isonicotinamide-pyridyl-isophthalic acid radical ion. The preparation method comprises the following steps: solvent thermal reaction between 5-isonicotinamide-pyridyl-isophthalic acid and nantokite, washing, and drying to obtain the novel porous copper complex of which the structure is stable. The preparation method is simple in process, convenient to operate and high in productivity. The 5-isonicotinamide-pyridyl-isophthalic acid porous copper complex obtained according to the method can catalyze the Knovevenagel condensation reaction between benzaldehyde and malononitrile, is high in catalysis selectivity and catalytic activity, and can be effectively recycled and used repeatedly.

Description

technical field [0001] The invention relates to a porous copper complex of 5-isonicotinamide pyridyl isotitanate and its preparation method and application, belonging to the technical field of porous layer columnar materials. Background technique [0002] Porous MOFs material combines the characteristics of organic compound structure design, tailorability and easy functionalization of inorganic substances. Compared with traditional porous materials such as zeolites, carbon nanotubes, and activated carbon, the most significant advantage is that it can be modified by modifying organic ligands. The surface properties of the pores can be adjusted to achieve the purpose of increasing the selectivity of specific reactions. The ability of MOF to assemble well-defined molecular building blocks into a microporous framework is especially suitable for evenly distributing and immobilizing catalytically active organometallics in its open pores, making it highly efficient and easy to reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/08B01J31/22C07C255/34C07C253/30
CPCY02P20/50
Inventor 陈满生许金生张春华邓奕芳易正戟聂雪崔莺
Owner HENGYANG NORMAL UNIV
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