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A green and efficient method for preparing furfural from biomass catalyzed by solid acid

A solid acid catalyst and biomass raw material technology, applied in organic chemistry, chemical recycling, etc., can solve problems such as high energy consumption, easy passivation of catalysts, equipment corrosion, etc., to avoid environmental pollution, reduce condensation reactions, and equipment corrosion small effect

Active Publication Date: 2021-02-12
BEIJING FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although Quaker Oats optimized the process system for continuous production in 1966 and increased the temperature to 184°C, the entire reaction process still took 1 hour
Today's furfural production process is still based on this, so many disadvantages remain so far, such as long reaction time, high energy consumption, low furfural yield, which is only less than 50%; sulfuric acid is used as a catalyst, which severely corrodes equipment and has not been used. Discharge of the treated acid will cause serious pollution to the environment, etc.
[0004] However, there are still deficiencies in the current research, for example, the commercial solid acid catalyst has poor catalytic effect and the yield of furfural is low; the preparation process of the synthesized solid acid catalyst is complicated and difficult to industrialize
In addition, solid acid catalysts with heterogeneous catalysis have common problems, such as the catalyst is easy to passivate and requires a regeneration process; the efficiency of heterogeneous catalysis is low, resulting in a large amount of catalyst used, or low yield of furfural; it is not easy to separate from the solid substrate, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 0.2g xylose, prepare 10mL solvent system with water and γ-valerolactone at a volume ratio of 1:9, add it to a reactor equipped with a polyphenol inner tank with a capacity of 100mL, add 10mol% sulfamic acid, and seal it. The reaction kettle was placed in a heating magnetic stirrer to raise the temperature to 190° C., the rotation speed was 350 rpm, and the temperature was kept for 15 minutes. Rinse the reaction kettle with cold water after the end of the reaction and make it drop to room temperature and open the lid. After the reaction solution is filtered through a disposable syringe filter with a pore size of 0.2 μm, it is detected and calculated by a high-performance liquid chromatography. The conversion rate of xylose is 99.91%. The yield of furfural was 70.19%.

Embodiment 2

[0026] Weigh 0.2g xylose, prepare 10mL solvent system with water and tetrahydrofuran at a volume ratio of 1:4, add it to a reaction kettle equipped with a polyphenol inner tank with a capacity of 100mL, add 10mol% sulfamic acid, and seal it. The reaction kettle was placed in a heating magnetic stirrer to raise the temperature to 180° C., the rotation speed was 350 rpm, and the temperature was kept for 90 minutes. Rinse the reaction kettle with cold water after the end of the reaction to make it drop to room temperature and open the lid. After the reaction solution is filtered through a disposable syringe filter with a pore size of 0.2 μm, it is detected and calculated by a high-performance liquid chromatograph. The conversion rate of xylose is 96.80%. The yield of furfural was 57.86%.

Embodiment 3

[0028] Weigh 0.2g xylose, prepare 10mL solvent system with water and γ-valerolactone at a volume ratio of 1:4, add it to a reactor equipped with a polyphenol inner tank with a capacity of 100mL, add 40mol% sulfamic acid, and seal it. The reaction kettle was placed in a heating magnetic stirrer to raise the temperature to 180° C., the rotation speed was 350 rpm, and the temperature was kept for 90 minutes. Rinse the reaction kettle with cold water after the end of the reaction to make it drop to room temperature and open the lid. After the reaction solution is filtered through a disposable syringe filter with a pore size of 0.2 μm, it is detected and calculated by a high-performance liquid chromatography. The conversion rate of xylose is 98.88%. The yield of furfural was 61.28%.

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PUM

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Abstract

The invention discloses a method for efficiently catalyzing various biomass raw materials to prepare furfural in a bifunctional solid organic acid in a two-phase system. The method comprises: 1) pulverizing the biomass raw materials, extracting with a mixed solvent, and drying; 2) adding the solid acid catalyst into the biphasic system of the organic solvent and water; 3) adding the biomass raw material into the reaction system of step 2), stirring and heating to the desired temperature and then keeping it warm; 4) after the reaction, Rapid cooling of the reactor to room temperature; and 5) the reaction liquid is filtered, detected and calculated by a high performance liquid chromatography. According to the preparation method of the present invention, the selected solid organic acid catalyst is catalyzed under homogeneous conditions, has little corrosion to equipment, is convenient for transportation, can be recycled, and avoids environmental pollution; compared with heterogeneous solid acid catalysts, it is cheap and easy Therefore, it has high catalytic efficiency, is easy to separate from solid biomass raw materials, and does not require catalyst regeneration treatment.

Description

technical field [0001] The invention belongs to the field of chemical synthesis. Specifically, it relates to a method for efficiently catalyzing a variety of biomass raw materials to prepare furfural with a bifunctional solid organic acid in a two-phase system. Background technique [0002] Furfural, also known as 2-furyl formaldehyde, is an important platform chemical, which can be used to prepare high value-added chemicals such as furfuryl alcohol, tetrahydrofuran, succinic acid, levulinic acid, and γ-valerolactone. It can also be used as a solvent , fuel additives, widely used in petrochemical and other industries. The earliest furfural industrial production process was proposed by the American Quaker Oats Company in 1921. It prepared furfural by catalytic hydrolysis and dehydration of oat husks at 153°C with 2wt% dilute sulfuric acid. The product was separated and purified by high-temperature steam. up to 5 hours. Although Quaker Oats optimized the process system for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/50
CPCC07D307/50Y02P20/584
Inventor 许凤张奇琳游婷婷张逊
Owner BEIJING FORESTRY UNIVERSITY