Method for preparing methyl furoate by directly oxidizing and esterifying furfural

A technology of oxidative esterification and methyl furoate, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problem of ineffective utilization and catalyst deactivation , active point coverage and other issues, to achieve significant industrial application value, simplify the reaction process, and easy to recycle

Pending Publication Date: 2019-05-31
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0005] However, the above nano-gold catalysts have the following problems when they are used for the synthesis of methyl furoate: 1. The gold composite particles are evenly loaded into the inside of the carrier. Since the diffusion of the reaction raw materials and reaction products is hindered by the internal pores of the carrier, they are loaded on the carrier. Internal composite particles cannot be effectively utilized when reacting
2. The nano-Au particles loaded on the outer surface of the carrier will cause the adsorption of reaction by-products and the accumulation of poisoning substances, which will cause the active points to be covered and inactivated.
3. The abrasion caused by the collision between the catalyst particles and the collision with the reactor wall, etc., causes the nanoparticles to fall off from the carrier, leading to the problem of catalyst deactivation

Method used

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  • Method for preparing methyl furoate by directly oxidizing and esterifying furfural

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preparation example Construction

[0023] Preparation of cobalt-based composite particle load carrier:

[0024] Mix 10g of 30% silica sol (pH=4.5), 1.96g of magnesium hydroxide, 7.5g of zirconium nitrate, 3g of concentrated nitric acid with a concentration of 80%, and 60mL of deionized water at 25°C. A homogeneous solid solution suspension was obtained, water was removed by rotary evaporation, and vacuum-dried at 80° C. to obtain a white powdery solid. Put the solid in a tube furnace, heat up and roast under nitrogen, heat up at 30-300°C for 3h (heating rate 1.5°C / min), keep at 300°C for 3h, heat up at 300-600°C for 3h (heating rate 1.7°C / min) , keep at 600°C for 3h. After natural cooling, a SiO2-MgO-ZrO2 metal composite oxide carrier is obtained.

Embodiment 1

[0026] Preparation of cobalt-based composite particle loading material A:

[0027] Add 1 g of SiO to the reactor sequentially 2 -MgO-ZrO 2 Carrier, 0.3g urea, 21.0mg chloroauric acid, 0.18g cobalt nitrate, and 70mL deionized water were mixed evenly, stirred and reacted at 80°C for 4h, and the mixture was cooled to room temperature, filtered under reduced pressure to obtain a solid, and the solid was vacuum-dried at 80°C 1h, the solid was calcined in a muffle furnace at 450°C for 3h. The cobalt-based composite particle load A was obtained after natural cooling.

[0028] The specific method for preparing methyl furoate by oxidative esterification of furfural is: 100mg of cobalt-based composite particle load A (0.1mol%), and the methanol solution (containing methanol 7.5mL) dissolved with 0.4805g (5mmol) furfural is added successively to the In a 25mL glass-lined autoclave, after three times of oxygen replacement, pressurize to 1.0MPa, stir at 500rpm, react at 130°C for 4h, co...

Embodiment 2

[0030] Preparation of cobalt-based composite particle load B:

[0031] Add 1 g of SiO to the reactor sequentially 2 -MgO-ZrO 2Carrier, 0.3g urea, 21.0mg chloroauric acid, 0.36g cobalt nitrate, and 70mL deionized water were mixed evenly, stirred and reacted at 80°C for 4h, and the mixture was cooled to room temperature, filtered under reduced pressure to obtain a solid, and the solid was vacuum-dried at 80°C 1h, the solid was calcined in a muffle furnace at 450°C for 3h. The cobalt-based composite particle load B was obtained after natural cooling.

[0032] The specific method of furfural oxidative esterification to prepare methyl furoate is: 100mg of cobalt-based composite particle load B (0.1mol%), dissolved in methanol solution (containing methanol 7.5mL) of 0.4805g (5mmol) furfural is added successively to the In a 25mL glass-lined autoclave, after three times of oxygen replacement, pressurize to 1.0MPa, stir at 500rpm, react at 130°C for 4h, cool to room temperature, de...

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Abstract

The invention relates to a method for preparing methyl furoate by directly oxidizing and esterifying furfural. The methyl furoate is prepared by using the furfural as the substrate and a cobalt-basedparticle supporter as the catalyst. The method specifically includes: dissolving the furfural into methanol, adding the cobalt-based particle supporter catalyst and auxiliaries, and performing stirring reaction at the temperature of 40-180 DEG C and in the oxygen atmosphere of 0.01-4MPa for 1-10 hours to prepare the methyl furoate through the one-step oxidization and esterification of the furfural. The method has the advantages that a two-step reaction including furfural oxidization and methanol esterification is shortened to the one-step oxidization and esterification, and the method is promising in application prospect; the cobalt-based particle supporter catalyst used by the method is mild in catalyzing conditions, good in effect, long in service life, easy to separate and recycle, capable of lowering production cost and evident in industrial application value.

Description

technical field [0001] The invention relates to a method for preparing methyl furoate, in particular to a method for preparing methyl furoate through direct oxidative esterification of furfural. Background technique [0002] Furfural, which can be obtained from C5 carbohydrates, is an important biomass platform compound and plays an important role in chemical production as a bridge connecting renewable biomass resources and non-renewable fossil fuels. Its molecule contains active functional groups such as a furan ring and an aldehyde group. Under certain conditions, reactions such as oxidative esterification, oxidative condensation, hydrogenation reduction, decarburization, and reductive amination can occur, thereby converting into high added value. chemicals. [0003] Methyl furoate is an important new synthetic fragrance with very important commercial value. At present, the methods for synthesizing methyl furoate mainly contain: hydrogen peroxide, concentrated sulfuric a...

Claims

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Application Information

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IPC IPC(8): C07D307/68B01J23/89
Inventor 高爽李国松吕迎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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