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Preparation method and application of triphenylamino metal organic framework compound capable of catalyzing carbon dioxide-epoxy compound cycloaddition

A technology of epoxy compounds and organic skeletons, applied in organic compound/hydride/coordination complex catalysts, organic chemical methods, catalyst activation/preparation, etc., to achieve good industrialization prospects, simple synthesis, and easy to be popularized and applied on a large scale Effect

Active Publication Date: 2017-02-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it has not been reported that the exhaust gas simulated mixed gas after desulfurization and denitrification treatment in thermal power plants can be directly synthesized with epoxy compounds in a solvent-free one-pot method without separation and purification.

Method used

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  • Preparation method and application of triphenylamino metal organic framework compound capable of catalyzing carbon dioxide-epoxy compound cycloaddition
  • Preparation method and application of triphenylamino metal organic framework compound capable of catalyzing carbon dioxide-epoxy compound cycloaddition
  • Preparation method and application of triphenylamino metal organic framework compound capable of catalyzing carbon dioxide-epoxy compound cycloaddition

Examples

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Effect test

Embodiment 1

[0032] 5,5',5"-(4,4',4"-nitrilotritylamide)triisophthalic acid (17mg, 0.02mmol), Zn(NO 3 ) 2 ·6H 2 O (29.7mg, 0.1mmol) was dissolved in N,N'-diethylformamide (2mL) and ethanol (1mL) and stirred evenly, then the solution was placed in an oven, fired at 100°C for 72h, and the oven was closed. After cooling to room temperature, colorless to pale yellow cubic crystals were produced, filtered and dried to obtain the target material Zn-L with a yield of about 60%. Elemental analysis (%) for Zn 7 C 90 N 8 o 62.50 h 111 : C45.95, H 3.63, N 5.36%. Found: C 46.30, H3.70, N 5.19%. The structure of the obtained target material is as follows figure 1 As shown, the XRD pattern of the target material is shown in image 3 As shown, the thermal analysis diagram is shown as Figure 5 shown.

Embodiment 2

[0034] 5,5',5"-(4,4',4"-nitrilotritylamide)triisophthalic acid (17mg, 0.02mmol), Zn(NO 3 ) 2 ·6H 2 O (29.7mg, 0.1mmol) was dissolved in N,N'-diethylformamide (2mL) and ethanol (1mL) and stirred evenly, then the solution was placed in an oven, fired at 120°C for 72h, and the oven was closed. After cooling to room temperature, colorless to light yellow cubic crystals were produced, filtered and dried to obtain the target material Zn-L with a yield of about 56%.

Embodiment 3

[0036] 5,5',5"-(4,4',4"-nitrilotritylamide)triisophthalic acid (17mg, 0.02mmol), Cu(NO 3 ) 2 ·3H 2 O (24 mg, 0.1 mmol) was dissolved in N,N'-dimethylformamide (2 mL) and concentrated HNO 3 (300 μL) after stirring evenly, take the solution and place it in an oven, bake it at 60°C for 72 hours, turn off the oven, cool to room temperature, green octahedral block crystals are produced, filter, and dry to obtain the target material Cu-L, The yield is about 70%. Elemental analysis (%) for Cu 6 C 90 N 8 o 42.75 h 73.50 : C46.36, H 4.11, N 6.69%. Found: C 47.24, H4.13, N 6.64%. The structure of the obtained target material is as follows figure 2 As shown, the XRD pattern of the target material is shown in Figure 4 As shown, the thermal analysis diagram is shown as Image 6 The adsorption curves of nitrogen and carbon dioxide are shown in Figure 7 shown.

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Abstract

The invention belongs to the technical field of catalytic materials, and relates to a preparation method and application of a triphenylamino metal organic framework compound capable of catalyzing carbon dioxide-epoxy compound cycloaddition. The preparation method comprises the following steps: 1. adding a connection ligand L and a transition metal salt Tm in a mole ratio of 1:(3-5) into a mixed solvent composed of ethanol and N,N-diethyl formamide in a volume ratio of 1:(2-2.5) or a mixed solvent composed of concentrated nitric acid and N,N-dimethylformamide in a volume ratio of 1:(6-8), and uniformly stirring; and 2. putting the solution prepared in the step 1 into a drying oven, drying for 60-90 hours while controlling the temperature at 60-120 DEG C, shutting down the drying oven, cooling to room temperature to precipitate a crystal, filtering and drying to obtain the target material Tm-L. The catalyst synthesis process is simple and easy to operate, and has the advantages of low raw material price for the catalyst and catalytic reaction, and high yield. The obtained functional material has stable chemical properties, and can easily implement large-area popularization and application.

Description

technical field [0001] The invention relates to a preparation method and application of a triphenylamine-based metal-organic framework compound capable of catalyzing the cycloaddition of carbon dioxide and epoxy compounds, and belongs to the technical field of catalytic materials. Background technique [0002] With the advancement of science and technology and the rapid development of human society, global warming caused by the excessive emission of carbon dioxide caused by the extensive use of fossil fuels has become an environmental problem that seriously threatens the survival and development of human beings. carbon dioxide (CO 2 ) is currently the most important greenhouse gas on the earth, and it is also the cheapest and most abundant resource in the C1 family. On a global scale, CO 2 The carbon content is 10 times that of oil, coal and natural gas. Among the sources of carbon dioxide emissions, the carbon dioxide emitted by thermal power plants accounts for a large p...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/10B01J37/10C07D317/38
CPCC07D317/38B01J31/2217B01J37/10C07B2200/13B01J35/60
Inventor 段春迎郭向阳何成于浩王喆
Owner DALIAN UNIV OF TECH
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