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Preparation method of nanosheet magnesium oxide catalyst and method for preparing diethyl carbonate by adopting catalyst

A technology of diethyl carbonate and flakes, which is applied in the field of preparation of nano-flaky magnesium oxide catalysts, can solve the problems of low catalyst activity such as carbamate decomposition, achieve good catalytic activity and stability, and the process is simple and easy , the effect of convenient operation

Inactive Publication Date: 2015-09-23
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a preparation method of nano-flaky magnesia catalyst, the method is simple and easy, and can prepare nano-flaky magnesia with high specific surface area, which overcomes the low catalyst activity and carbamate in the existing technology. Serious problems such as acid ester decomposition, thus providing an efficient catalyst for the preparation of diethyl carbonate by alcoholysis of ethyl carbamate and ethanol

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  • Preparation method of nanosheet magnesium oxide catalyst and method for preparing diethyl carbonate by adopting catalyst
  • Preparation method of nanosheet magnesium oxide catalyst and method for preparing diethyl carbonate by adopting catalyst
  • Preparation method of nanosheet magnesium oxide catalyst and method for preparing diethyl carbonate by adopting catalyst

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Embodiment 1

[0031] Mg(NO 3 ) 2 ·6H 2 O dissolved in deionized water, configured as 1.5mol / L Mg 2+ aqueous solution. 100mL1.5mol / L Mg 2+ Aqueous solution at 20°C with 2mol / L Na 2 CO 3 The precipitant was added dropwise to 50 mL of deionized water at the same time, and the pH was controlled at 10. After the precipitation was completed, the stirring was continued at 65°C for 3 hours, and then hydrothermally heated at 120°C for 10 hours. After hydrothermal treatment, the precipitate is filtered, washed with water until neutral, and then dried at 120°C for 10 hours. After drying, it is ground, and then calcined at 450, 600, and 750°C for 3 hours in an air atmosphere to obtain white magnesium oxide. The powders are recorded as MgO-A-450, MgO-A-600, and MgO-A-750, respectively, where 450, 600, and 750 represent the calcination temperature.

[0032] XRD detection, nitrogen adsorption-desorption isothermal detection, scanning electron microscope detection, CO 2 Programmed temperature deso...

Embodiment 2

[0034] Mg(NO 3 ) 2 ·6H 2 O dissolved in deionized water, configured as 1.5mol / L Mg 2+ aqueous solution. In addition, the configuration contains Na 2 CO 3Mixed precipitant with NaOH, where Na 2 CO 3 The concentration is 1mol / L, and the NaOH concentration is 2mol / L. 200mL 1.5mol / L Mg 2+ The aqueous solution was added dropwise to 50 mL of deionized water simultaneously with the mixed precipitant at 40°C, and the pH was controlled at 9. Stirring was continued at 40°C for 2 hours after the precipitation was completed, and then hydrothermally heated at 100°C for 20 hours. After the hydrothermal treatment, the precipitate was filtered, washed with water until neutral, and then dried at 110°C for 12 hours. After drying, it was ground and then calcined at 450°C in vacuum for 3 hours. The product was recorded as MgO-B-450, of which 450 represents the firing temperature.

Embodiment 3

[0036] Dissolve magnesium acetate in deionized water to make 0.1mol / L Mg 2+ aqueous solution. Then 0.10mol / L Na at 50°C 2 CO 3 The precipitant was gradually added dropwise to 150mL 1mol / L Mg 2+ in aqueous solution until the pH reaches 10. Stirring was continued at 50°C for 3 hours after the precipitation, and then hydrothermally aged at 160°C for 10 hours. After hydrothermal treatment, the precipitate is filtered, washed with water until neutral, and then dried at 100°C for 24 hours. After drying, it is ground and then calcined at 300°C for 3 hours in a nitrogen atmosphere. The product is marked as MgO-C-300, where 300 represents the firing temperature.

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Abstract

The invention discloses a preparation method of nanosheet magnesium oxide catalyst and a method for preparing diethyl carbonate by adopting the catalyst. The preparation method of the magnesium oxide catalyst comprises the following steps: (1) mixing 0.1 to 2 mol / L magnesium salt aqueous solution and 0.1 to 12 mol / L metal salt aqueous solution precipitating agent, wherein the precipitation temperature is 20 to 80 DEG C, the pH value in the precipitation process is 9 to 12, and precipitating insoluble metal salt mixture; (2) after the precipitation is ended, continuously stirring for 0.1 to 3 hours at the temperature of 40 to 80 DEG C; (3) then hydrothermally aging for 10 to 20 hours, filtering and washing precipitates to be neutral, and drying the precipitates at the temperature of 100 to 120 DEG C for 6 to 24 hours; (4) then roasting the precipitates for 0.2 to 6 hours, and obtaining white magnesium oxide powder. The average thickness of nanosheet magnesium oxide is 20nm to 50nm, and the specific surface area is 200 to 500 m<2> / g. The catalyst is used for preparing diethyl carbonate by virtue of alcoholysis of ethyl carbamate and ethanol, the product yield is 80 percent or more, and the selectivity is 99 percent.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanometer materials and catalysts. Specifically, the invention relates to a preparation method of a nano-flaky magnesium oxide catalyst and a method for preparing diethyl carbonate by using the catalyst. Background technique [0002] Magnesium oxide materials are widely used in basic catalysts, refractory materials, rubber activators and accelerators, functional ceramics and other fields. Compared with bulk magnesium oxide, nano magnesium oxide has special optical, electrical, magnetic, and chemical properties due to its excellent small size effect, surface effect, and quantum size effect. In addition, the specific surface area of ​​ordinary commercial magnesia is relatively small, and the preparation of nano-magnesia with high specific surface area has become an important means to improve the performance of catalysts. At present, magnesium oxide can be prepared by mechanical crushing meth...

Claims

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Application Information

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IPC IPC(8): B01J21/10B01J35/02C01F5/06C07C68/00C07C69/96B82Y40/00
CPCY02P20/584
Inventor 王利国李会泉李凤姣曹妍贺鹏陈家强
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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