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

A technology of ethyl nitrite and diethyl oxalate, applied in the direction of catalyst activation/preparation, carbon monoxide or formate reaction preparation, chemical instruments and methods, etc. Problems such as high loss rate, to achieve the effect of ingenious design, high mechanical strength, and inhibition of agglomeration

Active Publication Date: 2020-08-07
TIANJIN UNIV
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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 content is high, the thermal migration of palladium in the catalyst is serious on the carrier, and the dispersion degree on the carrier is low, the loss rate is high, and the optimal conditions for industrialization are not yet available. By adding methyl cellulose and / or lemon On the basis of optimizing the catalyst with an acid co-stabilizer, a preparation method of a carbon monoxide gas-phase coupling ethyl nitrite synthesis diethyl oxalate catalyst is provided

Method used

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

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Embodiment 1-3

[0050] 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:

[0051] S1 carrier γ-Al 2 o 3 Pretreatment: 100g is made of commercial large spherical shape with an average diameter of 3.32mm; γ-Al 2 o 3 The carrier is placed on a high-temperature muffle furnace and set to a heating program, and roasted at 1200°C for 4 hours, and set aside;

[0052] Preparation of mixed solution of S2 palladium salt and iron salt: dissolve soluble palladium salt and iron salt in deionized water, place the solution in a constant temperature ultrasonic water bath at 30°C for 1 hour, until the solids are completely dissolved, and prepare palladium, Iron...

Embodiment 4

[0060] 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:

[0061] S1 carrier γ-Al 2 o 3 Pretreatment: 100g of commercial hollow column 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 it aside;

[0062] Preparation of mixed solution of S2 palladium salt and iron salt: Dissolve soluble palladium salt and iron salt in deionized water, add vegetable tannin, and drop concentrated hydrochloric acid at a concentration of 12mol / L to adjust the pH of the solution while stirring To 2.5, the solution is placed in a constant temperature ultrasonic water bath at 50°C for 2 hours, until the solution is completely dissolved, and then prepared into a palladium and iron impregnated aqueous solution, wherein the concentrations of pa...

Embodiment 5

[0068] 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:

[0069] S1 carrier γ-Al 2 o 3 Pretreatment: 100g of γ-Al 2 o 3 (The average size is: outer diameter 3.8mm, inner diameter 1.0mm, height 5.8mm) placed on a high-temperature muffle furnace, set the heating program, roasted at 1200 ° C for 4 hours, and set aside;

[0070] Preparation of mixed solution of S2 palladium salt and iron salt: Dissolve soluble palladium salt and iron salt in deionized water, add vegetable tannin, and drop concentrated hydrochloric acid at a concentration of 12mol / L to adjust the pH of the solution while stirring To 2.5, put the solution in a constant temperature ultrasonic water bath at 30°C for 3 hours, until the solution is completely dissolved, and prepare a palladium and iron impregnated aqueous solution, wherein...

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Abstract

The invention relates to a catalyst for synthesizing diethyl oxalate by CO gas-phase coupling of ethyl nitrite and a preparation method thereof. The catalyst comprises a carrier, an active component palladium and a metal auxiliary agent iron, wherein the carrier is commercial hollow columnar [alpha]-Al2O3, the content of the active component palladium accounts for 0.1-1.0 wt% of the weight of thecarrier, 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 hollow columnar carrier is adopted,and vegetable tannin and/or anhydrous dextrose and/or polyvinylpyrrolidone are/is added, so that palladium metal nanoparticles in the catalyst are smaller, the dispersity is higher, and the palladiumloading capacity is lower. The catalytic activity of the catalyst is basically improved by more than two times, the cost of the catalyst is reduced by more than four times, the prepared catalyst carrier is suitable for filling of a fixed bed with high space velocity by taking industrialization as a reference, and more precious experience is provided for industrialization of diethyl oxalate production.

Description

technical field [0001] The invention belongs to the application of one-carbon chemical industry technology in organic chemical industry, be specifically related to a kind of preparation method of the catalyst of preparing diethyl oxalate with CO. 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 our country's rich coal and natural gas resources, it is a very economical and reasonable route to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J21/04B01J37/08B01J37/02C07C67/36C07C69/36
CPCB01J35/006B01J37/0203B01J37/0018B01J35/0066B01J21/04B01J23/8906C07C67/36C07C69/36
Inventor 吕静邢伟超王胜平马新宾赵玉军黄守莹王悦
Owner TIANJIN UNIV
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