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Preparation method of sulfated carbonized corn cob catalyst and method for preparing furfural from xylose in presence of catalyst

A corncob and catalyst technology, which is applied in the field of catalyzing xylose to prepare furfural and sulfonating and carbonizing corncob catalysts, can solve problems such as lack of economical applicability, and achieve the advantages of low production cost, reduced production cost and avoidance of equipment corrosion. Effect

Inactive Publication Date: 2016-04-20
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The current solid acids mainly include emerging materials such as metal oxides, resins, and graphene. This type of solid acid has a remarkable catalytic effect, but none of them has economic applicability. This limits the large-scale use of solid acids in industry. The main bottleneck of production use

Method used

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  • Preparation method of sulfated carbonized corn cob catalyst and method for preparing furfural from xylose in presence of catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation of a kind of sulfonated carbonized corn cob catalyst of the present embodiment and the method for preparing furfural by catalyzing xylose, its process flow chart is as follows figure 1 shown. Concrete preparation steps are as follows:

[0027] (1) Preparation of carbonized corn cobs: Add 5 g of dry corn cobs (80 mesh) into a ceramic crucible, place them in a vacuum tube furnace and seal them well, pass nitrogen gas at a flow rate of 40 mL / min, and carbonize at 400 °C. The time is 4h;

[0028] (2) Preparation of sulfonated carbonized corncob catalyst: add 0.8 g of the carbonized corncob obtained in step (1) and 24 mL of concentrated sulfuric acid into a tetrafluoroethylene reaction tank, place it in an oven at 145° C. for 14 hours, and after the reaction , cooled, filtered, the solid was washed until the pH was 6.8, and dried in an oven for 10 hours;

[0029] (3) Preparation of xylose-containing hydrolyzate: corn cob and oxalic acid are ball milled, th...

Embodiment 2

[0036] The preparation of a kind of sulfonated carbonized corn cob catalyst of the present embodiment and the method for preparing furfural by catalyzing xylose, its process flow chart is as follows figure 1 shown. Concrete preparation steps are as follows:

[0037] (1) Preparation of carbonized corn cobs: Add 6 g of dry corn cobs (100 mesh) into a ceramic crucible, place them in a vacuum tube furnace and seal them well, pass nitrogen gas at a flow rate of 50 mL / min, and carbonize at 450 °C. The time is 5h;

[0038] (2) Preparation of sulfonated carbonized corncob catalyst: add 1.0 g of the carbonized corncob obtained in step (1) and 30 mL of concentrated sulfuric acid into a tetrafluoroethylene reaction tank, place it in an oven at 150° C. for 15 hours, and after the reaction , cooled, filtered, the solid was washed until the pH was 7.0, and dried in an oven for 12 hours;

[0039] (3) Preparation of xylose-containing hydrolyzate: corn cob and oxalic acid are ball-milled, t...

Embodiment 3

[0046] The preparation of a kind of sulfonated carbonized corn cob catalyst of the present embodiment and the method for preparing furfural by catalyzing xylose, its process flow chart is as follows figure 1 shown. Concrete preparation steps are as follows:

[0047] (1) Preparation of carbonized corn cobs: Add 7 g of dry corn cobs (120 mesh) into a ceramic crucible, place them in a vacuum tube furnace and seal them well, pass nitrogen, the nitrogen flux is 60 mL / min, and the carbonization temperature is 500 ° C. The time is 6h;

[0048](2) Preparation of sulfonated carbonized corn cob catalyst: add 1.2 g of the carbonized corn cob obtained in step (1) and 36 mL of concentrated sulfuric acid into a tetrafluoroethylene reaction tank, place it in an oven and react at 155 ° C for 16 h, after the reaction , cooled, filtered, the solid was washed until the pH was 7.2, and dried in an oven for 14 hours;

[0049] (3) Preparation of xylose-containing hydrolyzate: corn cob and oxalic...

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Abstract

The invention belongs to the technical field of preparation of biomass-based chemicals and discloses a preparation method of a sulfated carbonized corn cob catalyst and a method for preparing furfural from xylose in presence of the catalyst. The method comprises the steps of heating absolutely dry corn cob powder in a carbonization furnace to 400-500 DEG C in an atmosphere of nitrogen gas and carbonizing for 4-6h to obtain carbonized corn cob; adding the carbonized corn cob and concentrated sulfuric acid into a reactor and reacting at 145-155 DEG C for 14-16h; washing and drying the reaction product to obtain the sulfated carbonized corn cob catalyst; placing xylose-containing hydrolysis liquid, the sulfated carbonized corn cob catalyst and dichloromethane in the reactor and reacting at 160-180 DEG C for 1.5-2.5h, and performing separation and purification on the reaction product to obtain furfural. The sulfated carbonized corn cob catalyst has high catalytic efficiency, is low in cost, and can remarkably improve the yield of furfural and reduce the production cost of furfural when used for preparing furfural from xylose.

Description

technical field [0001] The invention belongs to the technical field of biomass chemical preparation, and in particular relates to the preparation of a sulfonated carbonized corn cob catalyst and a method for preparing furfural by catalyzing xylose. Background technique [0002] With the depletion of non-renewable primary energy—fossil energy—all countries in the world have begun to pay attention to the conservation of non-renewable energy and accelerate the research and development of renewable energy—biomass energy. Lignocellulosic biomass will play an important role in industrial development and environmental pollution because of its environmental friendliness, abundant reserves and low cost. [0003] Furfural, also known as furan formaldehyde, is one of the important furan derivatives. It is obtained from the dehydration of polypentose obtained by high temperature acid hydrolysis of agricultural and sideline products. It is widely used in petroleum industry, chemical prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J21/18C07D307/48
CPCB01J27/02B01J21/18C07D307/48
Inventor 任俊莉林琦璇孙润仓邓奥杰
Owner SOUTH CHINA UNIV OF TECH
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