Method for preparing sorbitol from cellulose

A technology of cellulose and sorbitol, which is applied in the field of cellulose conversion to prepare sorbitol, which can solve the problems of intensified hydrogenolysis reaction, long time, and reduced sorbitol yield, so as to increase the hydrolysis rate, increase the yield, and facilitate hydrolysis Effect

Active Publication Date: 2016-11-23
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are the following main problems in the preparation of sorbitol by hydrolysis and hydrogenation of cellulose: (1) at a relatively low reaction temperature (such as 150°C), the hydrolysis rate of cellulose is slow, which becomes the rate-controlling step of the reaction, resulting in a slow reaction rate, Long time; (2) At a higher reaction temperature (eg >230°C), the hydrolysis rate of cellulose and the overall reaction rate are significantly increased, but the degree of hydrogenolysis reaction is intensified, resulting in a decrease in the yield of sorbitol
(3) Add copper salt to the reaction system, the reaction process will generate acid, and increase the difficulty of subsequent separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1 CO 2 Promotes the hydrolysis of cellulose

[0017] In a 30mL autoclave lined with polytetrafluoroethylene, add 10mL H 2 O, 0.2g cellulose, do not add catalyst, tighten the reactor, use N under room temperature 2 Purging for 5min, adding 2MPa CO 2 , preheated at 245°C for 15 minutes, hydrolyzed for 1 hour, cooled down, centrifuged the unreacted cellulose, dried, and calculated the conversion rate of cellulose was 70.2%.

Embodiment 2

[0021] Example 2 Preparation of Sorbitol by Hydrogenation of Cellulose

[0022] In a 30mL autoclave lined with polytetrafluoroethylene, add 10mL H 2 The catalyst PtNi / MESHZSM-5 of O, 0.3g cellulose, 0.1g reduction, the mass content of Pt and Ni are respectively 1% and 17%, tighten the reactor, use high-purity N at room temperature 2 Purge for 5 minutes to remove the air in the reactor. The reactor was preheated in a constant temperature water bath at 245°C for 15 minutes, and filled with 4MPa H 2 and 2MPa CO 2 , start stirring, and react for 2h. The reaction kettle is cooled down, and the liquid product is analyzed by liquid chromatography, and the analysis conditions are: differential refractive index detector (Shimadzu RID-10A), chromatographic column Shodex USP pak MN-431 (I.D.40mm * 250mm), and the temperature of the column oven is 50°C, the mobile phase is ultrapure water, and the flow rate is 0.2mL / min. Calculate cellulose conversion, product selectivity and yield. ...

Embodiment 3

[0028] Example 3 Preparation of Sorbitol by Hydrogenation of Cellulose

[0029] The reaction time is 4h, and the catalyst and other conditions are the same as in Example 2. The conversion rate of cellulose was 100%, the yield rate of sorbitol was 48.6%, and the yield rate of mannitol was 3.8%.

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Abstract

The invention relates to a method for preparing sorbitol through cellulose hydrolysis and hydrogenation. The method comprises that under carbon dioxide pressure of 0.1-3MPa, in the presence of a hydrogen mesoporous ZSM-5 zeolite-loaded Pt-Ni catalyst, under conditions of a temperature of 230-250 DEG C and H2 pressure of 0.5-6 MPa, sorbitol is prepared through cellulose hydrolysis and hydrogenation, wherein a sorbitol yield is 53.2% and a ratio of sorbitol to sorbitol isomer mannitol is greater than 12, and after the reaction, carbon dioxide spontaneously separates from the liquid product. The method is free of a liquid inorganic acid so that acid pollution and equipment corrosion are avoided. The method solves the problem that a sorbitol yield is low at a high reaction temperature of 230-250 DEG C, realizes rapid cellulose conversion and improves a sorbitol yield.

Description

technical field [0001] The invention relates to a method for preparing sorbitol by hydrolysis and hydrogenation of cellulose. It specifically relates to a method for preparing sorbitol by hydrolysis and hydrogenation of cellulose with Pt-Ni supported on mesoporous ZSM-5 zeolite as a catalyst in the presence of compressed carbon dioxide. Background technique [0002] Cellulose is the most abundant biomass resource in nature. The conversion and utilization of cellulose can reduce the dependence of human beings on fossil resources. The "one-pot" hydrolysis and hydrogenation of cellulose in high-temperature water to produce important chemical platform molecules such as sorbitol, mannitol, ethylene glycol, and propylene glycol is one of the green and feasible processes for utilizing cellulose. [0003] Cellulose hydrolysis and hydrogenation products are complex, and the basic reaction process is as follows: cellulose is hydrolyzed to generate glucose, while glucose is hydrogenat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/26C07C29/00C07C29/136
CPCC07C29/00C07C29/136C07C31/26
Inventor 孟祥春王观亚
Owner CHANGCHUN UNIV OF TECH
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