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A kind of preparation method and application of metal organic framework that catalyzes carbon dioxide to epoxy carbonate
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A technology of epoxy carbonate and organic framework, which is applied in chemical instruments and methods, organic chemistry, physical/chemical process catalysts, etc., and can solve problems such as high cost, immature technology, and high equipment requirements
Inactive Publication Date: 2020-10-30
NANKAI UNIV
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Problems solved by technology
In terms of chemical utilization of carbon dioxide, it mainly synthesizes urea, methanol, formic acid and its derivatives, etc., but requires high equipment, immature technology and high cost
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preparation example Construction
[0024] A kind of preparation method of manganese metal organic framework material, synthetic route is as follows figure 1 shown.
[0025] Take 2,4,6-tris[(p-carboxyphenyl)amino]-1,3,5-triazine, dissolve manganese chloride in N,N-dimethylacetamide, add distilled water, place in poly The reaction was carried out at 120°C for 72 hours in a tetrafluoroethylene-lined reactor, and the temperature was slowly lowered to room temperature at 5°C / h to obtain a colorless rod-shaped crystal "Mn-MOF" with a yield of 83%. The ratio of raw materials 2,4,6-tris[(p-carboxyphenyl)amino]-1,3,5-triazine, manganese chloride, nitrogen, nitrogen-dimethylacetamide and distilled water is 73.0mg:12.6mg :3mL:0.75mL, the volume of the polytetrafluoroethylene lining is 25mL.
[0026] The invention relates to a heterogeneous catalyst system. The preparation of the catalyst is an important index for evaluating the catalyst. The preparation method of the catalyst is simple, low in cost and easy for industri...
Embodiment 2
[0032] An application of the Mn-MOF prepared in Example 1 in catalyzing carbon dioxide as epoxy carbonate, the steps are as follows:
[0033] 1) In the glove box, weigh the Mn-MOF catalyst prepared in Example 1 and the cocatalyst tetrabutylammonium bromide in a Schlenk bottle. The dosage ratio of Mn-MOF and tetrabutylammonium bromide is 100mg:3.6mmol.
[0034] 2) Take the Schlenk bottle out of the glove box, connect the branch pipe of the Schlenk bottle to a vacuum line and degas it, and then connect a 1 atm carbon dioxide balloon to the branch pipe to fill the Schlenk bottle with carbon dioxide gas.
[0035] 3) Inject 5.0 mmol each of styrene oxide, 2-(chloromethyl)oxirane, 3-phenoxy-1,2-propylene oxide, 3-(1-naphthyloxy)-1 , 2-propylene oxide and benzyl glycidyl ether into the Schlenk bottle, put the Schlenk bottle in an oil bath at 60°C, and react for 24h.
[0036] 3) After the reaction is completed, the crude epoxy carbonate is obtained, and then the silica gel column is...
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Abstract
The invention relates to a preparation method of a metal organic framework for catalyzing carbon dioxide into epoxy carbonate under mild conditions and application thereof. The method includes the following catalysis steps that 1, Mn-MOF and tetrabutylammonium bromide as a co-catalyst are weighed and placed into a Schlenk flask; 2, a branch tube of the Schlenk flask is connected to a vacuum line and degassed, and a 1 atm carbon dioxide balloon is connected to the branch tube; 3, a substrate is added to the Schlenk flask and allowed to react in an oil bath at 60 DEG C for 24 h; 3, after the reaction is completed, a corresponding crude product is obtained, and the yield after purification is about 90%. Mn-MOF is filtered and used for a next cycle reaction. The method has the advantages thatthe metal organic framework is easy to prepare, has good structural stability and high catalytic activity, and can be recycled and used, so that the purpose of sustainable production is achieved; thepreparation process of the epoxy carbonate is simple, the requirement for equipment is low, sources of raw materials are extensive, the cost is low, and industrialized enlargement production is easy.
Description
technical field [0001] The invention relates to a metal-organic framework material for catalytic conversion of carbon dioxide, in particular to a preparation method and application of a manganese metal-organic framework material with superhigh catalytic activity for carbon dioxide. Background technique [0002] Metal-organic frameworks (MOFs) are widely used in catalytic reactions, drug sustained release, fluorescence, gas adsorption and separation, etc. due to their structural and functional diversity, porosity, large specific surface area, and unsaturated metal sites. . However, most MOFs have small pores and unstable structures, which limit their applications in the field of catalysis. [0003] Carbon dioxide is a nontoxic, renewable, and low-cost C1 resource that can be chemically used to deliver high-value products. Carbon dioxide emissions mainly come from the combustion of oil, natural gas and coal. However, in recent years, the level of carbon dioxide has increase...
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