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Method for enhancing activity of catalyst for preparing oxalic ester from CO

A technology for producing oxalate esters and catalysts, which is applied in the direction of catalyst regeneration/reactivation, molecular sieve catalysts, chemical instruments and methods, etc. It can solve the problems of low space-time yield of the target product oxalate esters and achieve good technical effects

Active Publication Date: 2012-08-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is that in the previous literature, in the process of producing oxalate with CO, there is a technical problem that the space-time yield of the target product oxalate is low, and a new method for improving the activity of the catalyst for producing oxalate with CO is provided. The method has the advantage of high space-time yield of the target product oxalate in the process of producing oxalate with CO

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Catalyst preparation:

[0024] Dissolve ferric nitrate in water, heat to 80 °C, and impregnate in 5 mm of α-Al by vacuum rotation 2 o 3 pellets, and then dried at 120°C for 4 hours. Dissolve potassium chloride and ammonium chloropalladate in water, adjust the solution with HCl to make the pH value about 4, then heat the solution to 80°C, impregnate it on the carrier again, and then dry it at 140°C for 4 hours, then Roasting at 450 DEG C for 4 hours, down to room temperature, to obtain the required catalyst, which is converted into metal (hereinafter the same), based on catalyst weight, its weight composition is: 0.41%Pd+0.20%K+0.25%Fe / α -Al 2 o 3 .

[0025] Take by weighing 10 grams of the above-mentioned prepared catalyst, and put it into a tube reactor with a diameter of 18 millimeters. Before driving, the catalyst is at 100 ml / min, the molar content of hydrogen is 20%, and the molar content of nitrogen is 80%. °C / min to 300 °C, constant temperature for 6 hours....

Embodiment 2

[0027] According to the same method of [Example 1], the composition is 0.16%Pd+0.15%Fe / α-Al 2 o 3 the required catalyst.

[0028] Take by weighing 10 grams of the above-mentioned prepared catalyst, and put it into a tube reactor with a diameter of 18 millimeters. Before driving, the catalyst is at 100 ml / min, the molar content of hydrogen is 20%, and the molar content of nitrogen is 80%. ℃ / min rises to 300 ℃, constant temperature for 6 hours, after that, the volume space velocity of the catalyst is 1500 hours -1, pressure is-0.05MPa, temperature is 130 ℃, methyl nitrite and CO molar ratio is 0.6: 1 after reacting 800 hours under the condition of molar ratio, as a result, the space-time yield rate of dimethyl oxalate is 810 grams / (hour .L), the selectivity of dimethyl oxalate is 98.1%. Afterwards, the reaction temperature was increased by 20° C., and kept for 10 hours, and then cooled to the original reaction temperature. At this time, the reaction result was: the space-time...

Embodiment 3

[0030] According to the same method of [Example 1], the composition is 0.34%Pd+1.0%K+0.46%Mn / α-Al 2 o 3 the required catalyst.

[0031] Take by weighing 10 grams of the above-mentioned prepared catalyst, and put it into a tube reactor with a diameter of 18 millimeters. Before driving, the catalyst is at 100 ml / min, the molar content of hydrogen is 20%, and the molar content of nitrogen is 80%. °C / min rises to 300 °C, after constant temperature for 6 hours, the volume space velocity of the catalyst is 3000 hours -1 , the pressure is 0.5MPa, the temperature is 135°C, and the molar ratio of methyl nitrite and CO is 0.8:1 after reacting for 2000 hours. The result is that the space-time yield of dimethyl oxalate is 900 g / (hour. liter), the selectivity of dimethyl oxalate is 98.5%. Afterwards, the reaction temperature was increased by 30°C and maintained for 10 hours, and then the temperature was lowered to the original reaction temperature. At this time, the reaction result was:...

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Abstract

The invention relates to a method for enhancing activity of catalyst for preparing oxalic ester from CO, which mainly solves the problem that the space time yield of aiming product oxalic ester is low during the process of preparing oxalic ester by CO in the traditional technology. The invention adopts the technical scheme that mixed gases containing nitrite ester and CO are used as raw materials, and a mole ratio of nitrite ester to CO is larger than (0-1.5):1, under the conditions that the volume space velocity is 500-10,000h -1, the pressure is -0.05-1.5MPa, and the temperature is 60-180 DEG C, the reaction temperature is higher than normal reaction temperature by 3-30 DEG C, and is maintained for 0.1-100 hours, then the temperature is lowered to normal reaction temperature, and raw materials are contacted with the catalyst containing palladium to generate effluent containing oxalic ester; and carrier of the catalyst containing palladium is at least one selected from aluminium oxide, silicon oxide, molecular sieve, magnesium oxide and calcium oxide, the content of palladium is 0.02-0.8 percent in percentage by weight of the catalyst. According to the technical scheme, the problem is better solved, and the method can be applied in the industrial production of oxalic ester prepared by CO.

Description

technical field [0001] The invention relates to a method for improving the activity of a catalyst for producing oxalate with CO, in particular to a method for improving the activity of a catalyst for producing dimethyl oxalate or diethyl oxalate with CO. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in the fine chemical industry to produce various dyes, medicines, important solvents, extractants and various intermediates. In the 21st century, oxalate, as a degradable and environmentally friendly engineering plastic monomer, has received extensive international attention. In addition, oxalic acid can be obtained by normal pressure hydrolysis of oxalate, and oxalamide can be obtained by normal pressure ammonia solution. Oxalate can also be used as a solvent to produce pharmaceutical and dye intermediates, etc., such as various condensation reactions with fatty acid esters, cyclohexylacetophenone, amino alcohols, and ...

Claims

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Application Information

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IPC IPC(8): B01J23/96B01J29/90B01J38/02C07C69/36C07C67/36
CPCY02P20/584
Inventor 杨为民刘俊涛刘国强李蕾
Owner CHINA PETROLEUM & CHEM CORP
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