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Catalyst used for gas-phase synthesis of oxalate ester and its preparation method

A gas-phase synthesis and catalyst technology, applied in the fields of carbon monoxide or formate reaction preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high price, high catalyst cost, influence on use, etc., and achieve a low amount of precious metals. , the effect of low catalyst cost

Active Publication Date: 2012-05-09
河南能源集团研究总院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of Pd in ​​these catalysts is generally high, and Pd is a noble metal, which is expensive, and the high loading makes the cost of the catalyst high, which affects its use in industry

Method used

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  • Catalyst used for gas-phase synthesis of oxalate ester and its preparation method
  • Catalyst used for gas-phase synthesis of oxalate ester and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh 10 grams of α-Al 2 o 3 Support, according to 0.01wt%Cu +1.0wt%Mo+0.5wt%Pd / α-Al 2 o 3 content to prepare the catalyst, the steps are as follows: take the calculated amount of copper nitrate and ammonium molybdate dissolved in water to form a solution, the specific surface area is 5.0 m 2 / g of α-Al 2 o 3 The carrier was soaked in the prepared impregnating solution for 4 hours, filtered, dried at room temperature, put into a reaction vessel, added an appropriate amount of water, and added dropwise 1mol / L K 2 CO 3Aqueous solution, adjust the dropping speed to ensure that the pH value of the solution in the reaction vessel is around 9; after the dropping is completed, age for 6 hours; filter, wash, dry, and roast at 500°C for 2 hours to obtain Cu / Mo / α-Al 2 o 3 Precursor; weigh the calculated amount of palladium chloride to make a solution, impregnate Cu / Mo / α-Al 2 o 3 Precursor, let it stand for 6 hours; filter, put it into the reaction container after drying ...

Embodiment 2

[0040] Weigh 10 grams of α-Al 2 o 3 Support, according to 1.0wt%Cu+0.01wt%Fe+0.3wt%Pd / α-Al 2 o 3 Content preparation catalyst, its steps are as follows: take calculated amount of copper nitrate and ferric nitrate dissolved in water to make a solution, the specific surface area is 10.0 m 2 / g of α-Al 2 o 3 The carrier is soaked in the prepared impregnation solution for 5 hours, filtered, dried at room temperature, put into a reaction vessel, and an appropriate amount of water is added, and a KOH aqueous solution with a concentration of 1mol / L is added dropwise in a 50°C water bath and stirred. , adjust the rate of addition to ensure that the pH of the solution in the reaction vessel is around 9; after the addition is completed, age for 2 hours; filter, wash, dry, and roast at 300 ° C for 5 hours to obtain Cu / Fe / α-Al 2 o 3 Precursor; weigh the calculated amount of palladium nitrate to make a solution, impregnate Cu / Fe / α-Al 2 o 3 The precursor was left to stand for 4 hour...

Embodiment 3

[0043] Weigh 10 grams of α-Al 2 o 3 Support, according to 0.3wt%Cu +0.9wt%Zn +0.4wt%Pd / α-Al 2 o 3 Content preparation catalyst, its steps are as follows: take calculated amount of copper nitrate and zinc nitrate dissolved in water to make a solution, the specific surface area is 30.0 m 2 / g of α-Al 2 o 3 The carrier was soaked in the prepared impregnation solution for 6 hours, filtered, dried at room temperature, put into the reaction vessel, added an appropriate amount of water, and added dropwise Na 2 CO 3 Aqueous solution, adjust the dropping speed to ensure that the pH value of the solution in the reaction vessel is around 10; after the dropping is completed, age for 6 hours; filter, wash, dry, and roast at 400°C for 4 hours to obtain Cu / Zn / α-Al 2 o 3 Precursor; Weigh the calculated amount of palladium acetate to make a solution, impregnate Cu / Zn / α-Al 2 o 3 The precursor was left to stand for 2 hours; filtered, dried at room temperature, put into a reaction vessel...

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Abstract

Belonging to the technical field of oxalate ester preparation, the invention aims to provide a catalyst which has high activity and high selectivity and is used in a reaction between carbon monoxide and nitrous acid ester for gas-phase synthesis of oxalate ester as well as its preparation method. The catalyst takes alpha-Al2O3 as a carrier, adopts palladium as a main active component, and employs copper as a first auxiliary agent and M as a second auxiliary agent, wherein, M can be ferrum, nickel, zinc, cobalt, titanium, cerium, molybdenum or tungsten. In terms of the carrier mass, the catalyst is composed of: 0.01-0.5 wt% of palladium, 0.01-1.0 wt% of copper, and 0.01-1.0 wt% of M. Prepared by a deposition-precipitation method, the catalyst of the invention can be used for carbonylation of CO and nitrous acid ester so as to synthesize oxalate ester. And the catalyst is used at a reaction temperature of 80-140DEG C, a reaction pressure of normal pressure to 1.0Mpa, and a reaction space velocity of 500-9000h<-1>. The catalyst provided in the invention has high reaction activity and selectivity, good repeatability of reaction performance, low cost, and simple preparation method, thus being easy for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of oxalate preparation, and relates to a catalyst for carbonylation of carbon monoxide and nitrite to synthesize oxalate and a preparation method thereof. Background technique [0002] Oxalate is an important organic chemical raw material, which can be used to prepare oxalic acid, ethylene glycol, carbonate, oxalamide, oxalyl chloride, etc. In 1965, D.M. Fenton and others in the United States discovered that α-Al 2 o 3 As a carrier, metal palladium is used as a catalyst, and carbon monoxide is carried out in an alcohol medium to perform a coupling reaction to synthesize an oxalic acid diester, which opens up an important way for the C1 chemical synthesis of oxalate. Its reaction principle is as follows: [0003] [0004] Wherein: R is an alkane group. [0005] The nitrite required for this reaction can be reacted with nitrous acid and alcohol or by NO, O 2 It can be produced by reacting with alcohol,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89C07C69/36C07C67/36
Inventor 蒋元力赵立红闫捷李伍成魏灵朝刘艳侠苗杰梁旭李丰丁建础贾金才张秀全
Owner 河南能源集团研究总院有限公司
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