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Method for synthesizing methyl formate by gas-phase carbonylation of methyl alcohol

A gas-phase methanol and methyl formate technology, applied in the preparation of carbon monoxide or formate, chemical instruments and methods, organic chemistry, etc., can solve the problems of difficult separation of catalysts and products, catalyst corrosion, high reaction pressure, etc., and achieve impurity content Low requirements, mild reaction conditions and high selectivity

Active Publication Date: 2014-04-02
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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Problems solved by technology

[0005] Aiming at the defects existing in the method for synthesizing methyl formate by methanol carbonylation in the existing liquid phase, the invention provides a method for synthesizing methyl formate by gas phase methanol carbonylation, which solves the technical problems existing in the present industrial synthesis technology: 1. Extremely high requirements for purity; 2. The catalyst corrodes the equipment severely; 3. It is difficult to separate the catalyst from the product; 4. The reaction pressure is high; 5. The operation is difficult

Method used

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  • Method for synthesizing methyl formate by gas-phase carbonylation of methyl alcohol
  • Method for synthesizing methyl formate by gas-phase carbonylation of methyl alcohol

Examples

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Embodiment 1

[0026] Weigh 1g of alumina and impregnate it into 15mL of 50mmol / L CuCl 2 2H 2 O ethanol solution, let it stand for 18 hours, dry at 100°C for 15 hours, roast at 400°C for 5 hours, then re-immerse in 1.25mL of 37.6mmol / L potassium chloropalladate aqueous solution, add 4mL of water, and stir for 3 hours. Ultrasonic dispersion for 3 hours, drying at 120°C for 15 hours, roasting at 400°C for 5 hours, adding 0.1g ascorbic acid, 0.2g citric acid, 0.5g polyvinylpyrrolidone, reducing at 90°C for 1 hour, and drying at 60°C for 15 hours in a vacuum. Pd-Cu / Al for the Synthesis of Methyl Formate by Gas-Phase Methanol Carbonylation 2 o 3 Catalyst 1.

Embodiment 2

[0028] Weigh 1g of magnesia 17mL50mmol / L Ni(NO 3 ) 2 ·6H 2 In O ethanol solution, let stand for 18 hours, dry at 100°C for 15 hours, bake at 400°C for 5 hours, and then re-impregnate into 0.63mL37.6mmol / L potassium chloropalladate and 0.34mL37.6mmol / L chloroplatinic acid Add 4mL of water to the aqueous solution, stir for 3 hours, ultrasonically disperse for 3 hours, dry at 120°C for 15 hours, bake at 400°C for 5 hours, add 1mL of formaldehyde, 0.24g of sodium citrate, 0.6g of polyethylene oxide-polyepoxide Propane-polyethylene oxide triblock copolymer was reduced at 100°C for 2 hours and dried at 60°C in vacuum for 15 hours to obtain PtPd-Ni / MgO catalyst 2 for the gas-phase methanol carbonylation to methyl formate reaction.

Embodiment 3

[0030] Weigh 1g of alumina and impregnate it into 1.25mL37.6mmol / L potassium chloropalladate aqueous solution, then add 4mL of water, stir for 3 hours, ultrasonically disperse for 3 hours, dry at 120°C for 15 hours, bake at 400°C for 5 hours, add 0.1 g ascorbic acid, 0.2g citric acid, 0.5g polyvinylpyrrolidone, reduce at 90°C for 1 hour, and dry at 60°C in vacuum for 15 hours, then you can get Pd / Al which is used in gas-phase methanol carbonylation to methyl formate. 2 o 3 Catalyst 3.

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Abstract

The invention discloses a method for synthesizing methyl formate by gas-phase carbonylation of methyl alcohol. A fixed bed reaction technology is used, and raw materials including methyl alcohol, carbon monoxide, hydrogen and oxygen generate gas-phase carbonylation reaction under the action of supported nano platinum family metal heterogeneous catalyst so as to generate methyl formate. The reaction raw materials include 10%-50% of methyl alcohol, 10%-50% of carbon monoxide, 10%-30% of hydrogen and 5%-20% of oxygen by volume ratio, and react under the conditions that air speed is 500-5000h<-1>, reaction temperature is 323K-423K and reaction pressure is 0.01Mpa-2Mpa.

Description

technical field [0001] The invention belongs to the technical field of methyl formate synthesis, and relates to a method for synthesizing methyl formate by gas-phase methanol carbonylation. Background technique [0002] Methyl formate is a very important intermediate in carbon-chemistry and has a wide range of uses. From methyl formate, formic acid, formamide, N,N-dimethylformamide, dimethyl carbonate, ethylene glycol, acetic acid, methyl acetate, acetic anhydride, methyl methacrylate, high-purity Products such as CO and diphosgene can also be used as insecticides, fungicides, fumigants and tobacco treatment agents. At present, the annual production capacity of methyl formate in my country is about 50,000 tons, and the demand is about 100,000 tons. The consumption structure is as follows: synthetic leather accounts for 30%, pesticides account for 26%, medicine accounts for 25%, acrylonitrile accounts for 10%, and others 9%. With the development of polyacrylonitrile fiber, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/06C07C67/36B01J23/89B01J23/44
CPCC07C67/36C07C69/06
Inventor 徐忠宁郭国聪彭思艳王志巧陈青松王明盛姚元根
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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