Catalyst used for synthesis of dimethyl oxalate and preparation method thereof

A technology for synthesizing dimethyl oxalate and dimethyl oxalate, applied in the directions of carbon monoxide or formate reaction preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of increasing the dechlorination process, the complicated catalyst preparation process, problems such as poor catalyst activity, to achieve the effect of reducing the dechlorination process, shortening the preparation cycle, and small particle size

Active Publication Date: 2016-07-27
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN1066070 reports a kind of Pd-Zr/Al 2 o 3 The preparation method of catalyst, although the catalyst prepared by this method has higher reactivity, selectivity and long life-span, but the loading of active component palladium is more than 1%, which undoubtedly increases the production cost of the catalyst
Patent 201410435876.9 reported a Pd/α-Al prepared by anion regulation method 2 o 3 The catalyst, the loading of the active component palladium is 0.05-1%. Although the catalyst prepared by this method has higher activity, the ion regulation step is added in the early stage of the catalyst...

Method used

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  • Catalyst used for synthesis of dimethyl oxalate and preparation method thereof
  • Catalyst used for synthesis of dimethyl oxalate and preparation method thereof
  • Catalyst used for synthesis of dimethyl oxalate and preparation method thereof

Examples

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Effect test

Embodiment 1

[0021] According to the loading capacity of 0.3wt% Pd, measure 15mL of 0.04mol / L palladium acetate dichloromethane solution, add 10gα-Al 2 o 3 (specific surface area 3m 2 / g, particle size 2.5mm) soaked in this active ingredient solution for 12 hours, then transferred to a 60°C oven to evaporate the liquid to dryness. Finally, the sample impregnated with active components was calcined at 500° C. for 4 hours to obtain the desired catalyst.

[0022] Measure 10mL of catalyst plus 10mL of magnetic ring and place it in a stainless steel reaction tube with an inner diameter of 20mm, and reduce it under a hydrogen atmosphere or a carbon monoxide atmosphere at 180°C for 4 hours, and then introduce 100mL / min methyl nitrite when the temperature drops to room temperature. 150mL / min carbon monoxide and 150mL / min nitrogen, start to heat up to react, the reaction pressure is 0.05MPa, the reaction temperature is 135°C, and the average space-time yield of dimethyl oxalate is 950g / L·h. We f...

Embodiment 2

[0024] According to the loading capacity of 0.5wt% Pd, measure 15mL of 0.06mol / L palladium acetate in acetone solution, mix 10g α-Al 2 o 3 (specific surface area 3m 2 / g, particle size 2.5mm) soaked in this active ingredient solution for 12 hours, then transferred to a 60°C oven to evaporate the liquid to dryness. Finally, the sample impregnated with active components was calcined at 600° C. for 4 hours to obtain the desired catalyst.

[0025] Measure 10mL of the catalyst of Example 2 plus 10mL of the magnetic ring, evaluate the catalyst according to the evaluation conditions of Example 1, and the space-time yield of dimethyl oxalate is 1050g / L·h.

Embodiment 3

[0027] According to the loading capacity of 0.1wt% Pd, measure 15mL of 0.02mol / L palladium acetate in chloroform solution, mix 10g α-Al 2 o 3 (specific surface area 3m 2 / g, particle size 2.5mm) soaked in this active ingredient solution for 16 hours, then transferred to a 60°C oven to evaporate the liquid to dryness. Finally, the sample impregnated with active components was calcined at 400° C. for 4 hours to obtain the desired catalyst.

[0028] Measure 10mL of the catalyst of Example 3 plus 10mL of the magnetic ring, evaluate the catalyst according to the evaluation conditions of Example 1, and the space-time yield of dimethyl oxalate is 852g / L·h.

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Abstract

The invention provides a catalyst used for synthesis of dimethyl oxalate and a preparation method thereof. The catalyst comprises an active component of palladium and a carrier of spherical alpha-Al2O3, wherein the loading amount of palladium accounts for 0.1 to 0.5% of the mass of the carrier; palladium particles have an average particle size of 2.5 to 3 nm and a dispersity of 34 to 37%; and the spherical alpha-Al2O3 has a particle size of 1 to 3 mm and a specific surface area of 0.5 to 10 m2/g. The catalyst is prepared through the following steps: dissolving palladium acetate in an organic solvent so as to prepare an impregnating solution, then impregnating the spherical alpha-Al2O3 in the impregnating solution for 12 to 24 hours, and carrying out drying and calcining. According to the invention, by using the organic solvent as the impregnating solution, the palladium particles on the carrier have high dispersity and small particle size. Thus, the catalyst has high reaction activity and long service life in reaction of synthesizing dimethyl oxalate from carbon monoxide and methyl nitrite.

Description

technical field [0001] The invention belongs to the field of preparation of a catalyst for synthesizing dimethyl oxalate in a coal-to-ethylene glycol process, and in particular relates to a catalyst for synthesizing dimethyl oxalate through gas-phase catalytic coupling of carbon monoxide and a preparation method thereof. Background technique [0002] Dimethyl oxalate is an important organic chemical raw material, which can be used to manufacture oxalic acid, oxamide, ethylene glycol, etc. In 1980, Japan's UBE Corporation and the United States' United Carbon Corporation successively disclosed carbon monoxide, methyl nitrite or ethyl nitrite as raw materials, and loaded Pd / α-Al 2 o 3 As a catalyst, to catalyze the method of carbon monoxide coupling to synthesize dimethyl oxalate or diethyl oxalate. Subsequently, Ube Industries has carried out a lot of research work on the development of high-efficiency catalysts and optimization of process flow, and built an industrial demon...

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C67/36C07C69/36
Inventor 姚元根张鑫潘鹏斌黄园园覃业燕陈建姗
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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