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Catalyst, preparation method and application of co gas phase synthesis of oxalate

A gas-phase synthesis and catalyst technology, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, carbon monoxide or formate reaction preparation, etc., can solve the problems of poor stability, low activity and selectivity, and achieve improved performance and high efficiency. The effect of reasonable activity and selectivity and bed temperature distribution

Active Publication Date: 2019-12-10
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, preparation method and application of co gas phase synthesis of oxalate
  • Catalyst, preparation method and application of co gas phase synthesis of oxalate
  • Catalyst, preparation method and application of co gas phase synthesis of oxalate

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Embodiment 1

[0027] 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 3Alumina carrier. Weigh 100g of alumina support, based on metal element (the same below), according to 1.0wt%Pd+0.45wt%Zr / Al 2 o 3 content to prepare the catalyst, the specific steps are as follows: select zirconium nitrate and palladium chloride, prepare an impregnation solution according to the loading capacity, add succinic acid to the impregnation solution to make the solution pH=2, and then make the specific surface area 6.84m 2 / g Al 2 o 3 The carrier is soaked in the impregnating solution for 1 hour, and then the solid is dried at 110°C for 4 hours and calcined at 400°C for 2 hours to make Pd-Zr / Al 2 o 3 Catalyst C1. The catalyst composition and properties are shown in Table 1.

Embodiment 2

[0029] 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 support, based on metal element (the same below), according to 2.0wt%Pd+0.5wt%Ti+0.7wt%Bi / Al 2 o 3 content to prepare the catalyst, the specific steps are as follows: select palladium chloride, titanium sulfate, bismuth nitrate, prepare an impregnation solution according to the loading capacity, add succinic acid to the impregnation solution to make the solution pH=2, and then make the specific surface area 8.74m 2 / g Al 2 o 3 The carrier is soaked in the impregnating solution for 1 hour, and then the solid is dried at 110°C for 4 hours and calcined at 400°C for 2 hours to make Pd-Ti-Bi / Al 2 o 3 Catalyst C2. The catalyst composition and properties are sh...

Embodiment 3

[0031] 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%Ba+0.85wt%La+0.55wt%Ce / Al 2 o 3 content to prepare the catalyst, the specific steps are as follows: select palladium nitrate, barium nitrate, lanthanum nitrate and cerium nitrate, prepare an impregnation solution according to the loading capacity, add terephthalic acid to the impregnation solution to make the solution pH=1, and then make the specific surface area 8.79 m 2 / g Al 2 o 3 The carrier is soaked in the impregnating solution for 3 hours, and then the solid is dried at 80°C for 4 hours and calcined at 450°C for 3 hours to make Pd-Ba-La-Ce / Al 2 o 3 Catalyst C3. The catalyst...

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Abstract

The invention relates to a CO gaseous-phase synthetic oxalic ester catalyst, a preparation method and application. The CO gaseous-phase synthetic oxalic ester catalyst mainly solves the technical problems of low activity and selectivity and low stability existing in the prior art. The catalyst is prepared from the following components in percentages by weight: a) using palladium as an active component, wherein the dosage of the active component is 0.1% to 4.0% of the weight of a carrier; b) using at least one element of IV B family or the sixth period in the periodic table of elements as an accessory ingredient, wherein the dosage of the accessory ingredient is 0.05% to 4.0% of the weight of the carrier; and c) using aluminum oxide as the carrier, wherein the specific surface area of the aluminum oxide carrier is 3 to 30 square meters per gram, and the average pore diameter of the aluminum oxide carrier is 15 to 40 nm. The catalyst can be used in industrial production of CO gaseous-phase synthetic oxalic ester.

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 Patents(China)
IPC IPC(8): B01J23/44B01J23/644B01J23/63B01J23/66B01J23/652B01J35/10C07C69/36C07C67/36
Inventor 朱俊华唐康健程远琳王黎敏
Owner CHINA PETROLEUM & CHEM CORP
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