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Catalyst for CO gas phase synthesis of dimethyl oxalate and preparation method of catalyst

A gas-phase synthesis technology of dimethyl oxalate, which is applied in the direction of carbon monoxide or formate reaction preparation, etc., can solve the problems of not meeting the economic requirements of industrialization, increased side reactions, poor activity, etc., to improve catalytic activity and selectivity of target products , improve stability, improve the effect of active structure

Inactive Publication Date: 2015-07-01
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In industrial production, the reaction temperature of CO gas-phase synthesis of dimethyl oxalate is generally controlled at 130-160 ° C. Higher temperatures cause methyl nitrite to decompose too quickly, and side reactions increase. The by-products mainly include methanol, methyl formate, and dimethyl oxalate. Ether, methylal, dimethyl carbonate, etc., which affect the selectivity of MN and bring difficulties to subsequent processing
If the reaction temperature is lowered, the side reactions will be reduced, but the activity will be poor, the space-time yield will drop more, and the continuous operation time will be short, which cannot meet the economic requirements of industrialization
[0005] In the reported patent of CO gas-phase synthesis of dimethyl oxalate, the CH 3 The selectivity of ONO to generate dimethyl oxalate can be 95%, but the yield is low, which cannot meet the economic requirements of industrialization

Method used

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  • Catalyst for CO gas phase synthesis of dimethyl oxalate and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 100 grams of α-Al 2 o 3 Carrier, by 0.8wt%Pd / α-Al 2 o 3 (wherein, the percentage refers to the metal Pd accounted for the carrier α-Al 2 o 3 The percentage by weight, other embodiments are the same) content preparation catalyst, and its steps are as follows: select palladium nitrate for use, prepare the palladium nitrate impregnating solution that palladium ion concentration is 1.6wt% according to the load capacity of Pd, and adjust the pH=0.3 of impregnating solution with nitric acid . Set the specific surface area to 8m 2 / g, the pore volume is 0.09cm 3 / g, α-Al with an average pore size of 8nm 2 o 3 Put the carrier into the prepared impregnating solution and soak for 2 hours at 25°C, then take it out and let it dry in the air, dry at 120°C for 12 hours, and bake at 300°C for 2 hours in the air atmosphere to make an eggshell shape with a shell thickness of 0.1 -2mm Pd / α-Al 2 o 3 catalyst.

Embodiment 2

[0035] Weigh 100 grams of α-Al 2 o 3 Carrier, according to 0.6wt%Pd+0.5wt%Ti / α-Al 2 o 3 content to prepare the catalyst, the steps are as follows: prepare a titanium nitrate impregnation solution with a Ti ion concentration of 1.0wt% according to the loading amount of Ti; 2 / g, the pore volume is 0.25cm 3 / g, α-Al with an average pore diameter of 15nm 2 o 3Put the carrier into the prepared titanium nitrate impregnation solution and soak it at 35°C for 2 hours, then take it out and let it dry in the air, dry it at 120°C for 12 hours, and roast it at 600°C for 2 hours in the air atmosphere; then put it into the prepared Nitric acid adjusted pH = 0.3, palladium ion concentration of 1.2wt% palladium nitrate acidic dipping solution soaked at 35 ° C for 2 hours, then took it out and dried it in the air, dried at 120 ° C for 12 hours, and roasted at 300 ° C for 8 hours in an air atmosphere , step by step to make eggshell-shaped, shell thickness 0.1-2mm Pd-Ti / α-Al 2 o 3 cataly...

Embodiment 3

[0037] Weigh 100 grams of α-Al 2 o 3 Support, according to 0.6wt%Pd-0.4wt%Ti-0.4wt%Co / α-Al 2 o 3 Content preparation catalyst, its steps are as follows: According to Ti and Co load capacity preparation Ti and Co ion total concentration is 1.0wt% titanium nitrate and cobalt nitrate impregnation solution; Specific surface area is 20m 2 / g, the pore volume is 0.30cm 3 / g, α-Al with an average pore diameter of 25nm 2 o 3 Put the carrier into the titanium nitrate and cobalt nitrate impregnating solution prepared above and soak for 3 hours at 25°C, then take it out and dry it in the air, dry at 100°C for 12 hours, and bake at 600°C for 2 hours in an air atmosphere. Then put it into the palladium nitrate acidic impregnation solution adjusted with nitric acid to adjust pH=1 and palladium ion concentration to be 1.2wt% and soak for 2 hours, then take it out and put it in the air to dry, and dry it at 100°C for 12 hours. Calcined at 300°C for 8 hours in an air atmosphere, the eggs...

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Abstract

The invention relates to a catalyst for CO gas phase synthesis of dimethyl oxalate. The catalyst contains an active ingredient metal Pd, metal aids and a carrier, wherein the metal aids refer to one or two out of titanium, vanadium, manganese, iron, cobalt, nickel or copper; the carrier is selected from alpha-Al2O3 and has the specific surface area of 3-30m<2> / g, the pore volume of 0.01-0.5cm<3> / g and the mean pore size of 2-50nm; the content of the metal Pd accounts for 0.1-1.5 percent of the weight of the carrier; the content of the metal aids accounts for 0.05-0.8 percent of the weight of the carrier; and the catalyst is of an eggshell type structure. The catalyst has high activity and high space time yield under the low temperature condition of low than 110 DEG C, particularly the catalyst has high selectivity, the side reactions can be effectively reduced, and the catalyst can be used for realizing industrial synthesis of dimethyl oxalate.

Description

technical field [0001] The invention relates to a catalyst for CO gas-phase synthesis of dimethyl oxalate and a preparation method thereof, belonging to the field of catalysts. Background technique [0002] my country's oil resources are tight, and its dependence on foreign countries has remained high for a long time. With the rapid development of the national economy, the consumption of ethylene glycol products for polyester consumption has increased by leaps and bounds. In 2012, China's ethylene glycol consumption was 10.7 million tons, most of which came from petroleum routes, of which 8 million tons depended on imports from abroad. The development of coal-to-ethylene glycol technology starting from CO and improving the comprehensive utilization rate of coal resources can not only alleviate the tension of petroleum resources, but also help promote the development of coal chemical and C1 chemical technology. [0003] CO gas-phase synthesis of dimethyl oxalate and further...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/89C07C69/36C07C67/36
Inventor 朱燕杨菊群徐昌晶王之光顾卫忠
Owner SHANGHAI HUAYI ENERGY CHEM
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