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Catalyst for synthesizing diethyl oxalate by carbon monoxide gas-phase coupling of ethyl nitrite and preparation method and application thereof

A technology of ethyl nitrite and diethyl oxalate, applied in the direction of carbon monoxide or formate reaction preparation, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, etc., can solve the most difficult problems without industrialization. Excellent conditions, serious thermal migration, and high load, to achieve the effect of clever design, high dispersion, and improved dispersion

Active Publication Date: 2020-08-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to synthesize diethyl oxalate catalyst for existing carbon monoxide gas-phase coupling ethyl nitrite in industrial process, due to the catalyst palladium prepared by impregnation method High loading capacity, severe thermal migration, low dispersion on the carrier, high loss rate, etc., and the lack of optimal conditions for industrialization, provide a catalyst for the synthesis of diethyl oxalate by coupling ethyl nitrite with carbon monoxide The preparation method and its application

Method used

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  • Catalyst for synthesizing diethyl oxalate by carbon monoxide gas-phase coupling of ethyl nitrite and preparation method and application thereof
  • Catalyst for synthesizing diethyl oxalate by carbon monoxide gas-phase coupling of ethyl nitrite and preparation method and application thereof
  • Catalyst for synthesizing diethyl oxalate by carbon monoxide gas-phase coupling of ethyl nitrite and preparation method and application thereof

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Experimental program
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Effect test

Embodiment example 1-3

[0055] In order to compare with the preparation method of the catalyst described in the present invention, the traditional method previously reported was first selected to prepare the catalyst for the synthesis of diethyl oxalate by gas-phase coupling of carbon monoxide with ethyl nitrite, and the effects of different morphology supports were investigated, and the specific preparation Proceed as follows:

[0056] S1 carrier γ-Al 2 o 3 Pretreatment: 100g of commercially available large balls with an average diameter of 3.32mm and small balls with an average diameter of 2.36mm; commercial Raschig rings with an average size of outer diameter 3.8mm, inner diameter 1.0mm, and height 5.8mm Carrier γ-Al 2 o 3 Place it on a high-temperature muffle furnace and set the heating program to bake at 1200°C for 4 hours, and set aside;

[0057] Preparation of mixed solution of S2 palladium salt and iron salt: dissolve soluble palladium salt and iron salt in deionized water, place the solu...

Embodiment example 4-8

[0064] Carry out the preparation of carbon monoxide gas-phase coupling ethyl nitrite synthesis diethyl oxalate catalyst according to the preparation method of catalyst of the present invention, concrete preparation steps are as follows:

[0065] S1 carrier γ-Al 2 o 3 Pretreatment: 100g of the commercial Raschig cyclic carrier γ-Al 2 o 3 , the average size is: γ-Al with an outer diameter of 3.8mm, an inner diameter of 1.0mm, and a height of 5.8mm 2 o 3 Put it on a high-temperature muffle furnace and set the temperature rise program at 1200 ° C for 4 hours to obtain α-Al 2 o 3 carrier, spare;

[0066] Preparation of mixed solution of S2 palladium salt and iron salt: Dissolve soluble palladium salt and iron salt in deionized water, add different substances or co-stabilizers of different concentrations, and drop concentrated hydrochloric acid immediately during the stirring process, with a mass fraction of 37.5 %. Adjust the pH of the solution to 1, place the solution in a...

Embodiment example 9-10

[0072] In order to compare with the preparation method of the catalyst described in the present invention, prove that the catalytic activity of the present invention is high, select the traditional method of previous report again, carry out carbon monoxide vapor phase coupling ethyl nitrite synthetic diethyl oxalate by increasing the palladium loading capacity of double The preparation of ester catalyst, namely the palladium load of preparing catalyst respectively is 0.1wt% (invention method) and 1wt% (traditional method) as contrast, and concrete preparation steps are as follows:

[0073] S1 carrier γ-Al 2 o 3 Pretreatment: 100g of commercial Raschig cyclic carrier γ-Al 2 o 3 Place it on a high-temperature muffle furnace and set the heating program to bake at 1200°C for 4 hours, and set aside;

[0074] Preparation of S2 palladium salt and iron salt mixed solution: dissolve soluble palladium salt and iron salt in deionized water, and drop concentrated hydrochloric acid imme...

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Abstract

The invention relates to a catalyst for synthesizing diethyl oxalate by carbon monoxide gas-phase coupling of ethyl nitrite and a preparation method and application thereof. The catalyst comprises a carrier, an active component palladium and a metal auxiliary agent iron, wherein the carrier is commercial Raschig ring columnar [alpha]-Al2O3, the content of the active component palladium accounts for 0.1-1.0 wt% of the weight of the carrier, and the content of the metal auxiliary agent iron accounts for 0.1-1.0 wt% of the weight of the carrier. According to the preparation method, a commercial Raschig ring columnar carrier is adopted, and methyl cellulose and / or citric acid and / or microcrystalline cellulose are / is added as co-stabilizers, so that the active component palladium is relativelyuniformly distributed on the carrier in a nanoparticle state. The catalytic activity is basically improved by more than 2 times, the cost of the catalyst is reduced by more than 5 times, the catalystis suitable for filling of a high-airspeed fixed bed, and a way is opened up for large-scale production of diethyl oxalate.

Description

technical field [0001] The invention belongs to the technical field of diethyl oxalate catalysts, and in particular relates to the preparation and industrial application of a catalyst for synthesizing diethyl oxalate through gas-phase coupling of carbon monoxide to ethyl nitrite. Background technique [0002] Diethyl Oxalate (Diethyl Oxalate), the molecular formula is C 6 h 10 o 4 . It is an important chemical raw material, which is produced by CO gas-phase coupling catalysis. It is a topic of widespread concern in the previous international "chemical" new process research, and it is also a research topic for the sustainable development of non-petroleum routes that are key projects in my country's planning. one. The source of raw materials is extensive and cheap, which can be produced from coal or natural gas, and CO or CO in industrial waste gas can also be used 2 For raw materials. If we make full use of my country's rich coal and natural gas resources, it is a very e...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J37/08B01J37/02C07C67/36C07C69/36
CPCB01J37/0018B01J37/0203B01J23/8906C07C67/36B01J35/394B01J35/393C07C69/36
Inventor 王胜平邢伟超吕静马新宾赵玉军黄守莹王悦
Owner TIANJIN UNIV
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