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Catalyst for synthesizing dimethyl oxalate with gas phase CO coupling as well as preparation method and application of catalyst

A technology of dimethyl oxalate and catalyst, applied in the field of preparation and application of noble metal catalysts, to achieve high conversion rate and selectivity, improve conversion rate and selectivity, and strengthen the effect of strong interaction

Inactive Publication Date: 2018-07-06
NINGBO JINYUANDONG PETROCHEM ENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, there is no solution to greatly improve the conversion rate and selectivity of the catalyst by simply modifying or modifying the carrier during the preparation process

Method used

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  • Catalyst for synthesizing dimethyl oxalate with gas phase CO coupling as well as preparation method and application of catalyst
  • Catalyst for synthesizing dimethyl oxalate with gas phase CO coupling as well as preparation method and application of catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The preparation process of a kind of catalyst involved in the present embodiment comprises the following steps:

[0042] Select 50g main component as θ-Al 2 o 3 The carrier, the carrier is added to 200mmol / L scandium nitrate solution and impregnated for 24 hours. The impregnated support was separated and dried, and calcined at 1200°C for 15 hours to obtain modified α-Al 2 o 3 carrier. Modified α-Al 2 o 3 The carrier is added to a palladium chloride solution with a pH of 1 and a concentration of 100 mmol / L, soaked at room temperature for 24 hours, and the soaked carrier is separated and dried, washed with alkaline solution, washed with water, and then dried. H was used before the catalyst was used 2 reduction, H 2 Airspeed is 500h -1 , the reduction temperature is 200°C, and the reduction time is 24 hours. Catalyst sample No. 1 was obtained, wherein the loading amount of palladium was 0.5wt%.

Embodiment 2

[0044] The preparation process of a kind of catalyst involved in the present embodiment comprises the following steps:

[0045] Select 50g main component as θ-Al 2 o 3 The carrier, the carrier was added 100mmol / L scandium nitrate solution and impregnated for 24 hours. The impregnated support was separated and dried, and calcined at 1200°C for 15 hours to obtain modified α-Al 2 o 3 carrier. Modified α-Al 2 o 3 The carrier is added to a palladium chloride solution with a pH of 1 and a concentration of 50 mmol / L, soaked at room temperature for 24 hours, and the soaked carrier is separated and dried, washed with alkaline solution, washed with water, and then dried. H was used before the catalyst was used 2 reduction, H 2 Airspeed is 500h -1 , the reduction temperature is 200°C, and the reduction time is 24 hours. Catalyst sample No. 2 was obtained, wherein the loading amount of palladium was 0.25wt%.

Embodiment 3

[0047] The preparation process of a kind of catalyst involved in the present embodiment comprises the following steps:

[0048] Select 50g main component as θ-Al 2 o 3 The carrier, the carrier is added to 50mmol / L scandium nitrate solution and impregnated for 24 hours. The impregnated support was separated and dried, and calcined at 1200°C for 15 hours to obtain modified α-Al 2 o 3 carrier. Modified α-Al 2 o 3 The carrier is added to a palladium chloride solution with a pH of 1 and a concentration of 20mmol / L, soaked at room temperature for 24 hours, and the soaked carrier is separated and dried, washed with alkaline solution, washed with water, and then dried. H was used before the catalyst was used 2 reduction, H 2 Airspeed is 500h -1 , the reduction temperature is 200°C, and the reduction time is 24 hours. Catalyst sample No. 3 was obtained, wherein the loading amount of palladium was 0.1 wt%.

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Abstract

The invention discloses a catalyst for synthesizing dimethyl oxalate with gas phase CO coupling as well as a preparation method and application of the catalyst. The catalyst is a palladium supported Al2O3 catalyst modified by an additive, wherein the additive of alpha-Al2O3 as a carrier comprises one or more of scandium, yttrium, lanthanum, cerium, praseodymium and neodymium, the content of the additive is 0.1-5wt%, and the content of palladium is 0.1-1.0wt%. The invention also discloses the preparation method of the catalyst. The preparation method comprises the following steps of adopting anadditive salt solution to modify the carrier, performing drying and calcining, then dipping the carrier with a palladium precursor solution, then performing cleaning, drying and calcining, and performing reduction with H2 before use. The catalyst is simple in preparation process, has relatively high selectivity and space time yield and is particularly suitable for synthesizing the dimethyl oxalate with gas phase CO coupling in industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of noble metal catalysts, and in particular relates to a catalyst for CO gas-phase coupling synthesis of dimethyl oxalate, its preparation method, and its use process parameter conditions. Background technique [0002] Dimethyl oxalate is an important chemical and pharmaceutical raw material. Dimethyl oxalate can be hydrolyzed to produce oxalic acid, hydrogenated to produce ethylene glycol, and aminated to produce oxamide. At present, the hydrogenation reaction of dimethyl oxalate to synthesize ethylene glycol is the most attractive application of dimethyl oxalate. At the earliest, D.M.Fenton first discovered the new reaction of CO to synthesize oxalate, and then Japan Ube Industries Co., Ltd. introduced nitrite into the reaction system and used palladium catalyst to develop the reaction. [0003] Patent CN201110095791.7 proposes a catalyst composed of a main active component...

Claims

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Application Information

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IPC IPC(8): B01J23/63C07C67/36C07C69/36
CPCB01J23/63C07C67/36C07C69/36
Inventor 臧未一刘太泽
Owner NINGBO JINYUANDONG PETROCHEM ENG TECH