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Preparation method and application method of iron-zirconium composite oxide catalyst

A technology of composite oxides and application methods, which is applied in the field of preparation of iron-zirconium composite oxide catalysts with adjustable dual functions and iron-zirconium composite oxide catalysts, which can solve the problems of difficult recycling, high cost of methyl iodide, and reduced catalyst activity And other issues

Inactive Publication Date: 2012-04-25
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Alkaline compounds require the addition of methyl iodide, an alkylating agent, which is costly, corrosive, and consumable
Cu-Ni metal activity is low, ZrO in metal oxide 2 Highest activity, especially ZrO impregnated with phosphoric acid 2 The highest activity, but ZrO impregnated with phosphoric acid 2 Phosphoric acid is easily lost during the use of the catalyst, which leads to a decrease in catalyst activity and is difficult to recycle

Method used

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  • Preparation method and application method of iron-zirconium composite oxide catalyst

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Experimental program
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Effect test

Embodiment 1

[0015] Accurately weigh Fe(NO 3 ) 3 .9H 2 O, 60.66g (0.15mol), Zr(NO 3 ) 2 .5H 2 O, 12.88g (0.03mol) was dissolved in deionized water, then weighed 45.39g of citric acid, dissolved in deionized water. Pour the aqueous solution of iron-zirconium into the aqueous solution of citric acid, stir, add 12ml of ethylene glycol, stir in a water bath at 60°C for 2 hours at a constant temperature, add ammonia water dropwise to adjust the pH value to 7, and stir at reflux at a constant temperature of 80°C for 2 hours until Sol. The sol was taken out, aged at room temperature for 12 hours, then placed in a vacuum drying oven, and dried at a constant temperature of 80° C. for 12 hours to obtain a catalyst precursor. Put the catalyst precursor into a muffle furnace for roasting, and roast at a constant temperature of 500° C. for 5 hours to prepare the desired iron-zirconium composite oxide catalyst.

[0016] Put 1 g of iron-zirconium composite oxide catalyst, 3 g of 4A molecular sieve...

Embodiment 2

[0024] According to the preparation method of the iron-zirconium composite oxide in Example 1, Fe: Zr molar ratios were respectively prepared as 10: 1, 5: 1, 2: 1 and 1: 1 catalysts, using a high-pressure reactor, according to the activity evaluation method of the catalyst , at CO 2 The reaction was carried out under the conditions of a pressure of 5 MPa (normal temperature), a reaction temperature of 150° C., and a reaction time of 24 hours. The obtained reaction liquids were quantitatively analyzed using the above-mentioned gas chromatography conditions. Experimental results such as figure 1 The results show that the catalytic activity of the Fe-Zr composite oxide catalyst increases first and then decreases with the addition of Fe. When the molar ratio of Fe:Zr is 5:1, the methanol conversion reaches the highest value.

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Abstract

The invention belongs to the technical field of chemical industry, relates to a preparation method and application method of an iron-zirconium composite oxide catalyst, and is used for solving the problems that at present, the catalyst has low activity and is difficult for separation, recovery and reutilization in a catalytic process for direct synthesis of dimethyl carbonate from carbon dioxide and methanol. The catalyst provided by the invention is composed of iron and zirconium oxides, wherein the molar ratio of iron to zirconium is (10:1)-(0.5:1); the catalyst is prepared by adopting a sol-gel method, is used for reaction between CO2 and CH3OH for direct synthesis of dimethyl carbonate at the reaction temperature of 80-180 DEG C and CO2 pressure of 3-7MPa ( room temperature); and compared with the existing ZrO2 catalyst and H3PO4-treated ZrO2 catalyst, both the activity and selectivity of the catalyst are greatly improved.

Description

Technical field: [0001] The invention belongs to the technical field of chemical industry, and relates to a method for preparing an iron-zirconium composite oxide catalyst and an application method for applying the catalyst to a reaction system for directly synthesizing dimethyl carbonate from carbon dioxide and methanol. Preparation and use method of functional iron-zirconium catalyst. technical background: [0002] Dimethyl carbonate (dimethyl carbonate, DMC) is an important "green" organic chemical intermediate, and its molecular structure contains carbonyl, methyl, methoxy and carbonylmethoxy, so it can be widely used in carbonylation, Organic synthesis reactions such as methylation, methoxylation and carbonylmethylation. It can replace highly toxic phosgene, methyl chloroformate, dimethyl sulfate, etc. as methylation reagents or carbonylation reagents to improve the safety of production operations and reduce environmental pollution. As a highly soluble solvent, DMC ca...

Claims

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Application Information

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IPC IPC(8): B01J23/745C07C69/96C07C68/04
CPCY02P20/141
Inventor 陈红萍梁英华苗建平郑小满
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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