Method for preparing furfural through catalytic conversion of xylose by acid photocatalyst under ultraviolet light

A photocatalyst and catalytic conversion technology, applied in organic chemistry and other fields, can solve the problem of high energy consumption of equipment, and achieve the effects of high selectivity, mild reaction conditions and high reactivity

Active Publication Date: 2014-12-31
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These reactions generally need to be carried out under high temperature and high pressure conditions, which require high equipment requirements and energy consumption.
There are no reports on the application of photocatalytic pathways to biomass conversion

Method used

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  • Method for preparing furfural through catalytic conversion of xylose by acid photocatalyst under ultraviolet light
  • Method for preparing furfural through catalytic conversion of xylose by acid photocatalyst under ultraviolet light
  • Method for preparing furfural through catalytic conversion of xylose by acid photocatalyst under ultraviolet light

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Preparation of photocatalyst by co-precipitation method: 6.445g ZrOCl 2 .8H 2 O, 0.013g La(NO 3 ) 3 .6H 2 O was dissolved in 100mL ultrapure water, and 3.7938g of TiCl was added dropwise while stirring 4 Solution, then adjust the pH to 8 with concentrated ammonia water, let stand at 25°C for 20h, dry at 100°C for 10h, and grind to obtain TiO 2 -ZrO 2 / La 0.1 ; figure 1 Be the infrared spectrogram of gained product, figure 11400cm -1 is a solid catalyst TiO 2 -ZrO 2 characteristic absorption peaks. figure 2 It is a transmission electron microscope picture of the obtained product, and it can be seen from the figure that the obtained product is a nano-scale round particle and has a strong aggregation effect.

[0033] (2) Preparation of acidic photocatalyst by impregnation method: Dilute 9.8g of concentrated sulfuric acid (0.1M) to 1000mL, pipette 200mL, then add 4.0g of photocatalyst prepared in step (1), stir at 25°C for 3h, and bake at 100°C Dry for 10 h...

Embodiment 2

[0043] (1) Preparation of photocatalyst by co-precipitation method: 6.445g ZrOCl 2 .8H 2 O, 0.13g La(NO 3 ) 3 .6H 2 O was dissolved in 100mL ultrapure water, and 7.5876g of TiCl was added dropwise while stirring 4 Solution, then adjust the pH to 10 with concentrated ammonia water, let stand at 30°C for 24h, dry at 110°C for 12h, and grind to obtain TiO 2 -ZrO 2 / La 1.0 ;

[0044] (2) Preparation of acidic photocatalyst by impregnation method: dilute 98g of concentrated sulfuric acid to 1000mL, pipette 200mL, then add 4.0g of photocatalyst prepared in step (1), stir at 30°C for 4h, dry at 110°C for 12h, and then Calcined at 600°C for 4 hours to obtain an acidic photocatalyst containing sulfate radicals;

[0045] (3) Hydrolysis reaction: put 0.2 xylose and 0.1 g of the acidic photocatalyst ore prepared in step (2) into a three-necked quartz flask, add 60 mL of distilled water, and react at 140 ° C for 8 h under the irradiation of ultraviolet light at 365 nm;

[0046] (4...

Embodiment 3

[0049] (1) Preparation of photocatalyst by co-precipitation method: 6.445g ZrOCl 2 .8H 2 O, 0.65g La(NO 3 ) 3 .6H 2 O was dissolved in 100mL ultrapure water, and 11.3814g of TiCl was added dropwise while stirring 4 solution, then adjust the pH to 11 with concentrated ammonia water, let stand at 40°C for 22h, dry at 120°C for 14h, and grind to obtain TiO 2 -ZrO 2 / La 5.0 ;

[0050] (2) Preparation of acidic photocatalyst by impregnation method: dilute 147g of concentrated sulfuric acid to 1000mL, pipette 200mL, then add 4.0g of photocatalyst prepared in step (1), stir at 40°C for 5h, dry at 120°C for 14h, and then Calcined at 700°C for 5 hours to obtain an acidic photocatalyst containing sulfate radicals;

[0051] (3) Hydrolysis reaction: put 0.2 xylose and 0.2 g of the acidic photocatalyst ore prepared in step (2) into a three-necked quartz flask, add 100 mL of distilled water, and react at 160 ° C for 12 h under the irradiation of ultraviolet light at 380 nm;

[0052...

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Abstract

The invention discloses a method for preparing furfural through catalytic conversion of xylose by acid photocatalyst under ultraviolet light. According to the method, ZrOCl2.8H2O and La(NO3)3.6H2O are added into distilled water and stirred to dissolve, TiVl4 solution is dropped so that pH is adjusted to a value between 8 and 11, photocatalyst is obtained through static placement and drying; sulfuric acid solution is prepared, the photocatalyst is added in the solution and the acid photocatalyst is obtained through stirring, drying and burning; the xylose and the acid photocatalyst are placed in a quartz three-neck flask, the distilled water is added and a reaction is conducted for 4h to 12h under irradiation of the ultraviolet light; and the furfural is obtained through natural cooling, suction filtration, filtrate distillation and concentration and organic solvent extraction and distillation. The acid photocatalyst has the advantages of being high in catalytic efficiency, strong in light responsiveness, renewable, capable of being recycled and the like. The preparation method has the advantages of being moderate in technology condition, low in energy consumption, high in efficiency, good in selection and the like. In the process of the reaction, no acid is added, device corrosion is avoided and environment is protected.

Description

technical field [0001] The invention belongs to the field of agricultural waste reuse, and relates to a method for preparing furfural by catalyzing xylose, in particular to a method for preparing furfural by catalytically converting xylose in the next step under the action of ultraviolet light with an acidic photocatalyst. Background technique [0002] Due to the excessive use of petrochemical resources by humans, it has caused a series of environmental problems while causing the depletion of global petrochemical resources. common goals of workers. Among many new energy sources, biomass is regarded as an ideal material to replace petrochemical resources due to its advantages such as wide sources, low price, and environmental friendliness. Agricultural waste biomass contains 25-35% hemicellulose, among which xylose, as the basic unit of xylan, the main component of hemicellulose, widely exists in agricultural waste. Therefore, how to effectively convert xylose into high-val...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/48B01J27/053
Inventor 任俊莉李慧玲王文菊孙润仓
Owner SOUTH CHINA UNIV OF TECH
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