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Method for preparing glucose-based 5-hydroxymethylfurfural from dimethyl sulphoxide and trichlorate

A technology of hydroxymethylfurfural and trichloride, which is applied in the field of biomass sugar resource utilization, can solve the problems of cumbersome solvent DMSO extraction process, lack of environmental friendliness, and high energy consumption, so as to avoid the difficulty of recycling and benefit the industry The effect of optimizing and optimizing process technology

Inactive Publication Date: 2015-12-16
JIANGSU UNIV
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  • Claims
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Problems solved by technology

People such as Jiang Chengzhen have studied in using dimethyl sulfoxide as reaction solvent, chromium chloride is catalyst, catalyzes fructose and is converted into 5-HMF (Jiang Chengzhen, Hu Tingfeng, Jiao Fen, Wang Fangfang, a kind of preparation method of 5-hydroxymethylfurfural , 201210434718.2), however, this catalytic system also has obvious defects, the yield of 5-HMF is measured by a spectrophotometer, the error is large, the solvent DMSO extraction process is cumbersome, and the energy consumption is high
[0004] In conclusion, although methods for the conversion of glucose and other biomass glycogens to 5-HMF have been reported, so far there is still a lack of systems that are environmentally friendly, utilize catalysts efficiently, and can recycle solvents.

Method used

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  • Method for preparing glucose-based 5-hydroxymethylfurfural from dimethyl sulphoxide and trichlorate
  • Method for preparing glucose-based 5-hydroxymethylfurfural from dimethyl sulphoxide and trichlorate
  • Method for preparing glucose-based 5-hydroxymethylfurfural from dimethyl sulphoxide and trichlorate

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Experimental program
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Effect test

Embodiment 1

[0046] Glucose (100mg) and dimethyl sulfoxide (1mL) were added to a 5mL ampoule, ultrasonically assisted dissolution: three-frequency simultaneous ultrasonic treatment under the condition of ultrasonic frequency and power of 25kHz and 600W, 28kHz and 600W, 40kHz and 600W, respectively 15 minutes each, temperature 25-30°C, put the ultrasonic solution in a water bath at 50°C for preheating for 15 minutes, add FeCl 3 ·6H 2 O (10 mg), carry out nitrogen flushing and saturation treatment for 5 minutes, and seal with alcohol blowtorch. Under the oil bath heating conditions of 100°C, 110°C, 120°C, and 130°C, heat for 8 hours respectively, take samples every 15 minutes for the first hour, and take samples every 1 hour for the next 7 hours. Each sample was parallelized 3 times. At 130℃, the highest yield of 5-HMF was 12.54±0.27% when reacted for 420min. Distill the reacted sample at atmospheric pressure at a temperature of 105-125°C to separate 5-hydroxymethylfurfural; the remaining...

Embodiment 2

[0048] Glucose (100mg) and dimethyl sulfoxide (1mL) were added to a 5mL ampoule, ultrasonically assisted dissolution: three-frequency simultaneous ultrasonic treatment under the condition of ultrasonic frequency and power of 25kHz and 600W, 28kHz and 600W, 40kHz and 600W, respectively 15 minutes each, temperature 25-30°C, put the ultrasonic solution in a water bath at 50°C for preheating for 15 minutes, add AlCl 3 (10 mg), carry out nitrogen flushing and saturation treatment for 5 minutes, and seal with alcohol blowtorch. Under the oil bath heating conditions of 100°C, 110°C, 120°C, and 130°C, heat for 8 hours respectively, take samples every 15 minutes for the first hour, and take samples every 1 hour for the next 7 hours. Each sample was parallelized 3 times. At 120℃, the highest yield of 5-HMF was 52.86±1.10% when reacted for 240min. Distill the reacted sample at atmospheric pressure at a temperature of 105-125°C to separate 5-hydroxymethylfurfural; the remaining sample i...

Embodiment 3

[0050] Glucose (100mg) and dimethyl sulfoxide (1mL) were added to a 5mL ampoule, ultrasonically assisted dissolution: three-frequency simultaneous ultrasonic treatment under the condition of ultrasonic frequency and power of 25kHz and 600W, 28kHz and 600W, 40kHz and 600W, respectively 15 minutes each, temperature 25-30°C, put the ultrasonic solution in a water bath at 50°C for preheating for 15 minutes, add CrCl 3 ·6H 2 O (10 mg), carry out nitrogen flushing and saturation treatment for 5 minutes, and seal with alcohol blowtorch. Under the oil bath heating conditions of 100°C, 110°C, 120°C, and 130°C, heat for 8 hours respectively, take samples every 15 minutes for the first hour, and take samples every 1 hour for the next 7 hours. Each sample was parallelized 3 times. With the increase of reaction temperature and the prolongation of reaction time, the yield of 5-HMF increased continuously but did not reach the maximum value. At 130℃, the yield of 5-HMF reached 54.43±1.13% a...

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Abstract

The invention provides a method for preparing glucose-based 5-hydroxymethylfurfural from dimethyl sulphoxide and trichlorate, which belongs to the technical field of resource utilization of biomass saccharides. The method employs an ion-free solvent dimethyl sulphoxide and a trichlorate catalyst and adopts the operation procedures consisting of multi-frequency ultrasonic wave-aided dissolving, pre-reaction preheating, nitrogen saturation, sealing of an ampoule bottle, separation of 5-hydroxymethylfurfural through normal-pressure distillation, recovery of the solvent dimethyl sulphoxide through reduced-pressure distillation and realization of recycling to continuously supplement raw materials for glucose and realize repeated usage of the solvent and the catalyst, so high-efficiency conversion of glucose-based 5-hydroxymethylfurfural, recovery of the solvent and high-efficiency utilization of the catalyst are realized. The method is designed on account of the key speed limit step in resource utilization of biomass saccharides, i.e., conversion of glucose into 5-hydroxymethylfurfural, and has the advantages of simple process, repeatable cycling, mild conditions and the like; and a novel approach is opened up for preparation of a 5-hydroxymethylfurfural platform chemical during resource utilization of biomass saccharides.

Description

technical field [0001] The invention belongs to the technical field of biomass sugar resource utilization, and specifically relates to a method for preparing glucosyl 5-hydroxymethylfurfural by using dimethyl sulfoxide as a solvent and trichloride as a catalyst. Background technique [0002] With the decrease of fossil resources, due to the dual pressure of energy crisis and environmental protection, biomass resources, as a renewable resource, can be converted into fine chemicals compared with solar energy, wind energy and other resources. Among the synthetic chemicals, 5-hydroxymethylfurfural (5-hydroxymethylfurfural, 5-HMF) obtained through carbohydrate degradation is an important platform compound. 5-HMF is an important chemical raw material. Its molecule contains an aldehyde group and a hydroxymethyl group. It can be used for synthesis through hydrogenation, oxidative hydrogenation, esterification, halogenation, polymerization, hydrolysis and other chemical reactions. M...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 周存山赵静马海乐刘伟民余筱洁任晓峰刘淑兰
Owner JIANGSU UNIV
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