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Preparation method of graphene-based composite solid base catalyst with 3D structure

A solid base catalyst, graphene-based technology, used in the preparation of carbon-based compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of complex product separation process, achieve green process energy saving, improve electron transfer rate, The effect of good catalytic performance

Inactive Publication Date: 2017-07-14
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, NaOH aqueous solution is generally used as a catalyst in the aldol condensation reaction. This traditional catalyst has disadvantages such as easy corrosion of experimental equipment and complicated product separation process. Therefore, some new solid base catalysts have been developed in recent years and have begun to be used in the aldol condensation reaction. , due to its simple preparation process and low production cost, it is expected to replace traditional catalysts. For example, in the literature Applied Clay Science, 2015, 118, 188-194, M.E.Manríquez et al. used transition metal ion-doped magnesium aluminum hydrotalcite as a solid base catalyst Used to catalyze the aldol condensation reaction of acetone

Method used

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  • Preparation method of graphene-based composite solid base catalyst with 3D structure
  • Preparation method of graphene-based composite solid base catalyst with 3D structure
  • Preparation method of graphene-based composite solid base catalyst with 3D structure

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Weigh 3.077g Mg(NO 3 ) 2 ·6H 2 O, 0.852g Al(NO 3 ) 3 9H 2 O and 0.40 g of citric acid were dissolved in 100 mL of deionized water, the above salt solution was mixed with 100 mL of graphene oxide solution with a concentration of 2 mg / mL, and stirred ultrasonically for 30 min to obtain a graphene oxide mixed solution. Weigh 1.60g NaOH and 1.27g NaOH 2 CO 3 Dissolve in 100mL deionized water to obtain a mixed alkali solution. The above two solutions were dropped into a 500ml four-necked flask at the same time, keeping the pH value at 10, and the temperature at 15°C. After the titration was completed, the crystallization was continued at 65°C for 16h. The magnesium aluminum hydrotalcite / reduced graphene oxide composite was prepared by centrifuging and washing to neutrality, and freeze-drying.

[0028] Under nitrogen condition, the temperature was raised to 500°C at 5°C / min and kept for 6h. After cooling, stir in deionized water at 25°C for 6h, wash with ethanol, and...

Embodiment 2

[0032] Weigh 2.051g Mg(NO 3 ) 2 ·6H 2 O, 0.852g Al(NO 3 ) 3 9H 2 O, and 0.40 g of citric acid were dissolved in 100 mL of deionized water, and the above-mentioned salt solution was mixed with 100 mL of graphene oxide solution having a concentration of 2 mg / mL, and stirred ultrasonically for 30 min to obtain a graphene oxide mixed solution. Weigh 1.20g NaOH and 0.63g NaOH 2 CO 3 Dissolve in 100mL deionized water to obtain a mixed alkali solution. The above two solutions were dropped into a 500ml four-necked flask at the same time, keeping the pH at 9 and the temperature at 25°C. After the titration was completed, continue to stir and crystallize at 75°C for 18h. The magnesium aluminum hydrotalcite / reduced graphene oxide composite was prepared by centrifuging and washing to neutrality, and freeze-drying.

[0033] Under nitrogen condition, the temperature was raised to 600°C at 2°C / min and kept for 8h. After cooling, stir in deionized water at 35°C for 7h, wash with etha...

Embodiment 3

[0036] Weigh 2.051g Mg(NO 3 ) 2 ·6H 2 O, 0.426g Al(NO 3 ) 3 9H 2 O and 0.40 g of citric acid were dissolved in 100 mL of deionized water, and the above salt solution was mixed with 100 mL of graphene oxide solution with a concentration of 2 mg / mL, and stirred ultrasonically for 30 min to obtain a mixed solution of graphene oxide; weigh 0.8 g of NaOH and 0.64 g Na 2 CO 3 Dissolve in 100mL deionized water to obtain a mixed alkali solution. The above two solutions were dropped into a 500ml four-neck flask at the same time, keeping the pH at 11 and the temperature at 35°C. After the titration was completed, the crystallization was continued at 85°C for 20h. The magnesium aluminum hydrotalcite / reduced graphene oxide composite was prepared by centrifuging and washing to neutrality, and freeze-drying.

[0037] Under nitrogen condition, the temperature was raised to 700°C at 10°C / min and kept for 10h. After cooling, stir in deionized water at 45°C for 8h, wash with ethanol, a...

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Abstract

The invention relates to a preparation method of a graphene-based composite solid base catalyst with a 3D structure. The method comprises the following steps: vertically growing magnesium aluminum hydrotalcite hexagonal crystal sheets on graphene oxide through adopting a one-step in situ growth technology, and carrying out high temperature calcination and hydration recovery to obtain the highly-active magnesium aluminum hydrotalcite / reduced graphene oxide solid base catalyst with a 3D array structure. The graphene oxide carrier with a high specific surface area facilitates the dispersion of the active sites of the marginal portion of the sheet structure of hydrotalcite to realize full exposure, and high interaction between a substrate and the sheet structure effectively improves the structural stability of the catalyst and improves the electron transfer rate in the catalytic reaction process. The graphene-based magnesium aluminum hydrotalcite solid base catalyst with a 3D composite structure has a good catalysis effect on the self-condensation reaction of acetone.

Description

technical field [0001] The invention belongs to the technical field of solid base catalysts, in particular to a preparation method of a graphene-based composite solid base catalyst with a 3D structure. Background technique [0002] Biomass has attracted much attention as a renewable resource. Biomass is chemically hydrolyzed to obtain lignin and sugars, which are further chemically converted into various organic compounds. Small organic molecules can achieve carbon chain growth through aldol condensation, which can be further processed to obtain biodiesel, realizing clean and renewable energy. At present, NaOH aqueous solution is generally used as a catalyst in the aldol condensation reaction. This traditional catalyst has disadvantages such as easy corrosion of experimental equipment and complicated product separation process. Therefore, some new solid base catalysts have been developed in recent years and have begun to be used in the aldol condensation reaction. , due to...

Claims

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Application Information

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IPC IPC(8): B01J21/18C07C45/72C07C49/17
CPCC07C45/72B01J21/18B01J35/50B01J35/615C07C49/17
Inventor 杨兰张艳花李峰范国利
Owner BEIJING UNIV OF CHEM TECH
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