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A microwave-assisted sncl4 catalyzed method for preparing furfural from corn cobs

A microwave-assisted, corncob technology, applied in the direction of organic chemistry and the like, can solve the problems of complex structure and reduce furfural yield, etc., and achieve the effects of high catalytic efficiency, improved furfural yield, and environmental protection of the process.

Active Publication Date: 2017-12-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the various components and complex structures of lignocellulosic raw materials, various side reactions are bound to occur during the hydrolysis process, thereby reducing the yield of furfural

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A microwave-assisted SnCl 4 The method for preparing furfural by catalyzing corncobs may further comprise the steps:

[0025] Add 1.0g degreased raw corncob, 0.1g SnCl 4 and 25 mL of ultrapure water. Place the polytetrafluoroethylene inner tank in an ultrasonic cleaner and perform ultrasonication at 35KHz for 5 minutes, so that the raw material particles are evenly dispersed in water, infiltrated and the air in the raw material gaps is excluded. Put the PTFE inner tank into the PEEK outer tank and tighten it, put it into the microwave reactor, insert the sensor, and screw on the pressure measuring nut. Nitrogen was passed for 7 minutes to replace the oxygen in the tank. Set the reaction temperature to 170°C, the heating time to 14 minutes, the reaction time to 0 minutes, the power to 400W, adjust the rotation speed, and start the reaction.

[0026] Take corn cob raw material of the same quality as above, SnCl 4 The catalyst and the same amount of water with the sam...

Embodiment 2

[0032] A microwave-assisted SnCl 4 The method for preparing furfural by catalyzing corncobs may further comprise the steps:

[0033] Add 1.0g degreased raw corn cob, 0.2g SnCl 4 and 15 mL of ultrapure water. Place the polytetrafluoroethylene inner tank in an ultrasonic cleaner and perform ultrasonication at 40KHz for 8 minutes to uniformly disperse and infiltrate the raw material particles in water and remove the air in the gaps of the raw material. Put the PTFE inner tank into the PEEK outer tank and tighten it, put it into the microwave reactor, insert the sensor, and screw on the pressure measuring nut. Nitrogen was passed for 10 minutes to replace the oxygen in the tank. Set the reaction temperature to 180°C, the heating time to 18 minutes, the reaction time to 2.5 minutes, the power to 500W, adjust the rotation speed, and start the reaction.

[0034] Take another 1.0g defatted corncob raw material, 0.2g SnCl 4 Catalyst and 15mL ultrapure water, after 40KH Z The ultr...

Embodiment 3

[0038] A microwave-assisted SnCl 4 The method for preparing furfural by catalyzing corncobs may further comprise the steps:

[0039] Mix 1 g of defatted corncob, 20 mL of ultrapure water and 0.1 g of SnCl 4 Add it into a polytetrafluoroethylene inner tank, and use an ultrasonic cleaner with a power of 30KHz to sonicate for 10 minutes. After it was loaded into the microwave reactor, nitrogen gas was introduced for 8 minutes to remove the oxygen in the container. The microwave reaction conditions are as follows: reaction temperature 190°C, heating time 21 min, reaction time 0 min, microwave power 600W.

[0040] Under the same conditions of corncob quality, catalyst dosage and solid-to-liquid ratio as above, after ultrasonic treatment with the same power and time, the mixed solution was transferred to a high-pressure reactor, and the catalytic reaction was carried out at the same temperature and time.

[0041] After the reaction is over, place the reaction tank / kettle in an ic...

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Abstract

The invention belongs to the technical field of preparation of biomass chemicals and discloses a method for preparing furfural from corncobs through microwave assisted SnCl4 catalysis. The preparation method comprises steps as follows: degreased corncobs, a catalyst SnCl4 and water are added to a reactor and evenly mixed ultrasonically, then nitrogen is introduced at the microwave power of 400-600 W for oxygen removal, the mixture is heated by microwaves to the temperature of 160-190 DEG C for a reaction for 0-50 min, reaction products are separated and purified, and a product, namely, the furfural, is obtained. According to the method, the SnCl4 is used as the catalyst, the production of the furfural is highly selective, the catalytic efficiency is high, the environment-friendly effect is realized, corrosion is small, and the technological process is more environment-friendly; the reaction rate and the energy utilization rate are increased through microwave assisted heating, so that the reaction time is shortened, and the yield of the furfural is increased.

Description

technical field [0001] The invention belongs to the technical field of biomass chemical preparation, in particular to a microwave-assisted SnCl 4 A method for preparing furfural by catalyzing corn cobs. Background technique [0002] With the depletion of fossil energy and the increasing impact of petroleum fuel emissions on the earth's climate, exploring non-fossil energy has become an urgent task for all mankind. Biomass energy, as a new type of energy with wide distribution, large total amount, renewable and environment-friendly, has the greatest compatibility with modern industrial technology and modern life, and has the greatest potential to replace fossil energy. [0003] Furfural, also known as furan formaldehyde, is a common chemical raw material and chemical solvent derived from biomass. It is widely used in many fields such as petroleum, chemical industry, medicine, pesticide, food, synthetic rubber, and synthetic resin. The commercial application of furfural was ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/48C07D307/50
CPCC07D307/48C07D307/50
Inventor 任俊莉严羽欢孙润仓林琦璇邓奥杰
Owner SOUTH CHINA UNIV OF TECH
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