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Catalyst for synthesizing oxalic ester and preparation method thereof

A technology of catalyst and oxalate, which is applied in the direction of carbon monoxide or formate reaction preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low space-time yield and achieve stable reaction, long life and easy The effect of control

Active Publication Date: 2009-12-09
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Subsequently, many patents have successively reported that Mo, Ni, Ti, Fe, Ga, Cu, Na 2 O and SiO 2 Catalysts composed of other additives are used in the gas phase synthesis of oxalate from carbon monoxide and nitrite, but the space-time yield is still low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 10g α-Al 2 o 3 Place in an aqueous solution of ammonia water and sodium bicarbonate with a pH value of 9, treat in an autoclave at 150°C for 3 hours, then wash with distilled water until neutral, and dry at 120°C for 12 hours. According to 0.8wt%Pd+0.02La / α-Al 2 o 3 Content preparation catalyst. Treated α-Al 2 o 3 Immerse in 0.005M lanthanum nitrate solution for 12 hours, dry under infrared lamp after fully absorbed, then dry at 120°C for 12 hours, bake at 350°C for 4 hours, then place the solid in a concentration of 0.005 M PdCl 2 In the solution, soak for 12 hours, dry under infrared lamp after fully absorbed, then dry at 120°C for 12 hours, and bake at 350°C for 4 hours to make Pd-La / α-Al 2 o 3 catalyst.

[0017] Get 2 grams of the catalyst prepared in Example 1, put it in a reaction tube of quartz glass with an inner diameter of 18 mm, and reduce it through a hydrogen gas temperature program, and finally reduce it at 350° C. for 6 hours. The hydrogen ...

Embodiment 2

[0019] Weigh 10gα-Al 2 o 3 In an aqueous solution of ammonia water and sodium bicarbonate with a pH value of 9, it was treated in an autoclave at 250°C for 5 hours, then washed with distilled water until neutral, and dried at 120°C for 12 hours. According to 0.8wt%Pd+0.05La / α-Al 2 o 3 Content preparation catalyst. Treated α-Al 2 o 3 Immerse in 0.005M lanthanum nitrate solution for 12 hours, dry under infrared lamp after fully absorbed, then dry at 120°C for 12 hours, bake at 450°C for 4 hours, then place the solid in a concentration of 0.005 M PdCl 2 In the solution, soak for 12 hours, dry under infrared lamp after fully absorbed, dry at 120°C for 12 hours, and then bake at 450°C for 4 hours to make Pd-La / α-Al 2 o 3 catalyst.

[0020] Get 2 grams of the newly prepared catalyst of Example 2, and evaluate the catalyst according to the evaluation conditions of Example 1. After the evaluation, the space-time yield of dimethyl oxalate is 850g / L.h.

Embodiment 3

[0022] Weigh 10g α-Al 2 o 3 In an aqueous solution of ammonia water and sodium bicarbonate with a pH value of 9, it was treated in an autoclave at 250°C for 8 hours, then washed with distilled water until neutral, and dried at 120°C for 12 hours. According to 0.8wt%Pd+1.0La / α-Al 2 o 3 Content preparation catalyst. Treated α-Al 2 o 3 Immerse in 0.01M lanthanum nitrate solution for 12 hours, dry under infrared lamp after fully absorbed, then dry at 120°C for 12 hours, bake at 450°C for 4 hours, then place the solid in a concentration of 0.005 M PdCl 2 In the solution, soak for 12 hours, dry under infrared lamp after fully absorbed, then dry at 120°C for 12 hours, and then bake at 450°C for 4 hours to make Pd-La / α-Al 2 o 3 catalyst.

[0023] Get 2 grams of the catalyst prepared in Example 3, evaluate the catalyst according to the evaluation conditions of Example 1, and the space-time yield of dimethyl oxalate after the evaluation is 1020g / L.h.

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PUM

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Abstract

The invention relates to a catalyst for synthesizing oxalic ester and a preparation method thereof. The catalyst contains active components of palladium and lanthanum which respectively account for 0.3-1.5 percent and 0.01-8 percent of the weight of a carrier, and the carrier is Alpha-Al2O3. The preparation method comprises the following steps: placing the Alpha-Al2O3 into alkaline solution, and processing the Alpha-Al2O3 in a high-pressure kettle under a temperature of 150-350 DEG C; washing the Alpha-Al2O3 with distilled water to neutral; drying the Alpha-Al2O3 under the temperature of 100-200 DEG C; dipping the Alpha-Al2O3 in solution with the concentration of lanthanum being 0.003-0.02 M, drying and baking; and dipping the Alpha-Al2O3 in solution with the concentration of palladium being 0.003-0.02 M, drying and baking under a temperature of 300-700 DEG C. The catalyst is applied to a reaction for synthesizing dimethyl oxalate by carbon monoxide and methyl nitrite and has the advantages of higher reacting activity and selectivity, long service life, stable reaction and easy control; and the space time yield of the dimethyl oxalate is 830g / L.h-1130g / L.h.

Description

technical field [0001] The invention relates to a catalyst for synthesizing oxalate and a preparation method thereof. Background technique [0002] Oxalate is an important chemical raw material, which can be used as an intermediate of oxalic acid, ethylene glycol, oxamide, medicine and fuel. Especially along with the dwindling of oil resources, the preparation of oxalate from natural gas through synthesis gas is a pioneering C 1 The new process and new technology of chemical industry realize the strategic goal of "replacing petroleum ethylene with coal and natural gas, and indirect two-step synthesis of ethylene glycol", which has great development prospects and is the C 1 An important development direction of chemical industry. [0003] At present, oxalate esters are mainly produced by esterification and dehydration of oxalic acid and alcohol in toluene in China. The production of 1 ton of diethyl oxalate requires 1 ton of anhydrous oxalic acid, 780 kilograms of ethanol ...

Claims

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Application Information

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IPC IPC(8): B01J23/63C07C67/36C07C69/36
Inventor 马中义王宏伟周玮孟庆茹赵胤李正蒋海洋
Owner PETROCHINA CO LTD
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