Catalyst for preparing oxalate through CO gas phase synthesis and preparation method and application thereof

A gas-phase synthesis and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, carbon monoxide or formate reaction preparation, etc., can solve the problems of low activity and selectivity, poor stability, etc., and achieve high activity and selectivity performance-enhancing, easy-to-control effects

Active Publication Date: 2017-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] One of the technical problems to be solved by the present invention is that there are technical problems of low activity and selectivity and poor stability in the prior art, and a new CO gas-phase synthesis oxalate catalyst is provided. It has high activity and selectivity in the reaction of acid ester, and the temperature distribution of the bed is reasonable, it can withstand the influence of impurities such as hydrogen and water vapor, it has the advantages of long life and easy control of the reaction.

Method used

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  • Catalyst for preparing oxalate through CO gas phase synthesis and preparation method and application thereof
  • Catalyst for preparing oxalate through CO gas phase synthesis and preparation method and application thereof
  • Catalyst for preparing oxalate through CO gas phase synthesis and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0030] The formed pseudo-boehmite is treated with steam at 750°C for 6-8 hours, and then roasted at 1250°C for 3 hours to obtain α-Al 2 o 3 Alumina carrier. Weigh 100g of alumina support, based on metal element (the same below), according to 1.0wt%Pd+0.25wt%Zn+0.15wt%La / Al 2 o 3 content to prepare the catalyst, the specific steps are as follows: select lanthanum nitrate, prepare an impregnating solution according to the loading capacity, in order to control the modification of the surface of the support by rare earth metals, add succinic acid to the impregnating solution to make the solution pH=2, and then increase the specific surface area to 6.84 m 2 / g Al 2 o 3 Soak the carrier in the impregnating solution for 1 hour, then dry the solid at 110°C for 4 hours, and roast it at 400°C for 2 hours, then use palladium chloride and nitric acid as the carrier modified by rare earth according to the loading capacity of Pd and Zn. Pd-Zn-La / Al is prepared by preparing zinc into t...

Embodiment 2

[0032] Calcining pseudo-boehmite powder at 1250°C for 4 hours to obtain 2 o 3 powder, then mixed with pseudo-boehmite powder at a mass ratio of 1:1, treated with steam at 750°C for 2 hours, and then calcined at 900°C for 4 hours to obtain α-Al 2 o 3 and θ-Al 2 o 3 Mixed crystal alumina carrier. Weigh 100g of alumina carrier, based on metal element (the same below), according to 2.0wt%Pd+0.5wt%Zn+0.7wt%La / Al 2 o 3 content to prepare the catalyst, the specific steps are as follows: select lanthanum acetate, prepare an impregnating solution according to the loading capacity, in order to control the modification of the surface of the carrier by rare earth metals, add succinic acid to the impregnating solution to make the solution pH=2, and then increase the specific surface area to 8.74 m 2 / g Al 2 o 3 Soak the carrier in the impregnating solution for 1 hour, then dry the solid at 110°C for 4 hours, and roast it at 400°C for 2 hours, then use palladium chloride and nitric...

Embodiment 3

[0034] Calcining pseudo-boehmite powder at 1250°C for 4 hours to obtain 2 o 3 powder, mixed with pseudo-boehmite powder at a mass ratio of 7:1, treated with steam at 750°C for 3 hours, and then calcined at 850°C for 5 hours to obtain α-Al 2 o 3 and θ-Al 2 o 3 Mixed crystal alumina carrier. Weigh 100g of alumina carrier, based on metal element (the same below), according to 0.75wt%Pd+1.0wt%Zn+0.85wt%La+0.55wt%Ce / Al 2 o 3 content to prepare the catalyst, the specific steps are as follows: select lanthanum nitrate and cerium sulfate, and prepare an impregnation solution according to the loading capacity, in order to control the modification of the surface of the carrier by rare earth metals, add terephthalic acid to the impregnation solution to make the solution pH=1, and then The specific surface area is 8.79m 2 / g Al 2 o 3 Soak the carrier in the impregnating solution for 3 hours, then dry the solid at 80°C for 4 hours, and bake it at 450°C for 3 hours, then use pallad...

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Abstract

The invention relates to a catalyst for preparing oxalate through CO gas phase synthesis and a preparation method and application of the catalyst. The catalyst is mainly used for solving the problems that activity and selectivity are low and stability is poor in the prior art. According to the adopted technical scheme, the catalyst comprises, by weight, an active component, an additive, a modifying agent and a carrier, wherein palladium is adopted as the active component with the using amount elementally accounting for 0.1-4.0% of the weight of the carrier, a rare earth element is adopted as the modifying agent with the using amount elementally accounting for 0.1-3.0% of the weight of the carrier, aluminum oxide is used the carrier which is modified by the rare earth element, the specific area of the aluminum oxide carrier is 3-40 m<2> / g, and the pore volume with the pore diameter being 15-40 nanometers accounts for 75%-95% of the total pore volume. Accordingly, the problems are well solved, and the catalyst can be used in industrial production for preparing oxalate through CO gas phase synthesis.

Description

technical field [0001] The invention relates to a catalyst, preparation method and application of CO vapor phase synthesis of oxalate. Background technique [0002] Oxalate is an important chemical raw material, which can be used to prepare oxalic acid, ethylene glycol, carbonate, intermediates of drugs and dyes, plastic accelerators and solvents, etc. The traditional synthesis method of dimethyl oxalate is to use the esterification reaction of oxalic acid and methanol. One of the main raw materials, oxalic acid, is produced by the sodium formate method. Sodium formate is synthesized by combining carbon monoxide and sodium hydroxide at 160°C and a pressure of 18-20kg. , then concentrated and dehydrogenated at 400°C to form sodium oxalate, then reacted with lead sulfate to produce lead oxalate, further acidified with sulfuric acid to obtain crude oxalic acid, and finally coagulated and precipitated with barium carbonate and 1% polyacrylamide to obtain refined oxalic acid, but...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63C07C67/36C07C69/36
Inventor 朱俊华李斯琴唐康健程远琳王黎敏
Owner CHINA PETROLEUM & CHEM CORP
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