Method for preparing agricultural and forestry waste hydrothermal liquefied furfural in CO2 atmosphere

A technology for agricultural and forestry waste and hydrothermal liquefaction, which is applied in the field of hydrothermal liquefaction of furfural of agricultural and forestry waste, can solve the problems of many side reactions, high cost and high energy consumption, and achieves improved selectivity, yield, stability and quality Improve and alleviate the effect of corrosion problems

Active Publication Date: 2019-04-16
HUAZHONG UNIV OF SCI & TECH
View PDF3 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. N is commonly used in the prior art 2 As an inert gas for the reaction, the yield of furfural usually needs to be further improved;
[0005] 2. The patent with the application number "201610692355.0" discloses a method for preparing furfural from camellia oleifera husks, and mentions the use of carbon dioxide as a weakly acidic gas catalyst, but the patent also uses catalyst additives to act together
There are many side reactions in the existing catalytic system, and these side reactions will reduce the selectivity of pentose to furfural, resulting in a large loss of furfural;
[0006] 3. In the prior art, the production of furfural per ton needs to consume 25 to 35 tons of water vapor, the reaction time is relatively long, and the use of steam as a heat source and extractant consumes a lot of energy and high cost; and the pyrolysis process has high energy consumption, The problem of high catalyst cost needs to be improved
[0007] 4. Using dilute acid as a catalyst is easy to corrode equipment, which requires expensive metal equipment maintenance costs and serious environmental pollution
And its separation and recycling are very difficult, and the dilute acid hydrolysis method will also lead to a large amount of acidic furfural wastewater, which is extremely difficult to treat
[0008] In short, the furfural industry is a typical industry with high energy consumption and heavy pollution. It has been reported that the furfural preparation method has a great effect on increasing the yield, reducing energy consumption, reducing wastewater discharge and slowing down equipment corrosion, but it still cannot completely solve the pollution problem. or cannot be applied due to high cost

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing agricultural and forestry waste hydrothermal liquefied furfural in CO2 atmosphere
  • Method for preparing agricultural and forestry waste hydrothermal liquefied furfural in CO2 atmosphere
  • Method for preparing agricultural and forestry waste hydrothermal liquefied furfural in CO2 atmosphere

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0031] figure 1 It is a process flow diagram involved in the preparation method of hydrothermal liquefaction of furfural from agricultural and forestry waste under a CO2 atmosphere, such as figure 1 As shown, a method for preparing furfural from agricultural and forestry waste hydrothermally liquefied under a CO2 atmosphere comprises the following steps:

[0032] S1: Collect agricultural and forestry waste, crush and sieve to a particle size of 60-120 mesh, add it to a hydrothermal reactor, and mix it with deionized water to form a mixed solution with a mass-volume ratio of 1:5 to 1:15;

[0033] S2: Purge the kettle body with CO2, exhaust the air in the reactor, then close the outlet valve, fill in 0Mpa~2MpaCO2, then seal the reactor, heat it up to 150℃~250℃ under stirring, and keep it at 10~50 minute;

[0034] S3: After cooling the hydrothermal reactor to room temperature, release the pressure to collect the gas, collect the reacted solid-liquid mixture in the reactor, and ...

Embodiment 1

[0040] a CO 2 The method for preparing furfural by hydrothermal liquefaction of agricultural and forestry waste under atmosphere specifically comprises the following steps:

[0041] S1: Weigh 10g of rice husk and place it in a 500ml high-temperature and high-pressure hydrothermal reaction kettle, and add 100ml of deionized water;

[0042] S2: Seal the reactor, drain the air in the reactor, and fill it with CO with an initial pressure of 2Mpa 2 , turn on the heating switch, set the stirring speed to 200r / min, raise the temperature to 200°C at a rate of 8°C / min, keep it for 30min, then turn off the heating switch immediately;

[0043] S3: After the reactor is cooled to room temperature, collect the generated gas, open the reactor to take out the reaction mixture, and use CH 2 Cl 2 Clean the inner wall of the reactor and the stirrer;

[0044] S4: Using CH 2 Cl 2 The reaction mixture was extracted, CH 2 Cl 2 The extraction ratio to the reaction mixture is 1:2, the extracti...

Embodiment 2

[0047] S1: Weigh 10g of corn stalks, put it in a 500ml high temperature and high pressure hydrothermal reaction kettle, and add 150ml of deionized water;

[0048] S2: Seal the reactor, drain the air in the reactor, and fill it with CO2 with an initial pressure of 1.5Mpa, turn on the heating switch, set the stirring speed to 200r / min, and raise the temperature to 200°C at a rate of about 8°C / min , after keeping for 30min, turn off the heating switch immediately;

[0049] S3: After the reaction kettle is cooled to room temperature, the generated gas is collected, the reaction kettle is opened to take out the reaction mixture, and the inner wall of the reaction kettle and the stirrer are cleaned with ether;

[0050] S4: Extract the mixture with diethyl ether, the ratio of diethyl ether to the reaction mixture is 1:2, the extraction time is 12h, filter the diethyl ether phase with a vacuum filtration device, and then recover the diethyl ether by vacuum distillation, and obtain bio...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
particle size (mesh)aaaaaaaaaa
Login to view more

Abstract

The invention discloses a method for preparing agricultural and forestry waste hydrothermal liquefied furfural in a CO2 atmosphere, which comprises the following steps of: S1, collecting agriculturaland forestry waste, crushing and screening the agricultural and forestry waste, adding the agricultural and forestry waste into a hydrothermal reaction kettle, and mixing the agricultural and forestrywaste with deionized water to form a mixed solution with a mass-volume ratio of 1:15 to 1:5; S2, blowing the kettle body by using CO2, after exhausting the air in the reaction kettle, closing an airoutlet valve, filling 0-2Mpa CO2, sealing the reaction kettle, raising the temperature to 150-250 DEG C under stirring, and keeping the temperature for 10-50 minutes; S3, after the hydrothermal reaction kettle is cooled to room temperature, releasing pressure to collect gas, collecting solid-liquid mixture in the reaction kettle after reaction, and carrying out vacuum filtration separation to obtain a solid part and a liquid part; S4, extracting the liquid part by using an organic solvent, separating and filtering an organic phase, removing the organic solvent, and obtaining biological oil rich in furfural through rotary evaporation. CO2 is used as inert atmosphere, and proper parameters are selected to jointly improve the selectivity and yield of furfural.

Description

technical field [0001] The invention belongs to the technical field of biomass energy, and more specifically relates to a CO 2 Preparation method of hydrothermal liquefaction of furfural from agricultural and forestry waste under atmosphere. Background technique [0002] Furfural, also known as 2-furyl formaldehyde, is a series of natural precursors of furan-based chemicals and solvents. It has high application value and is widely used in organic synthesis, analytical reagents, raw material preparation of pharmaceuticals and industrial products, etc. At present, furfural preparation methods mainly include hydrolysis liquefaction, catalysis and pyrolysis of biomass and so on. Biomass is rich in hemicellulose, which in turn degrades into furfural. In the hydrolysis method, hemicellulose is hydrolyzed under the action of acid and water to generate xylose, and xylose undergoes isomerization and continuous dehydration reaction to generate furfural. Biomass pyrolysis refers to ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C10G1/00C10G1/08B01J19/14
CPCB01J19/14C10G1/002C10G1/086C10G2300/1014
Inventor 王贤华曲磊陈应泉杨海平杨晴曾阔陈伟张世红陈汉平
Owner HUAZHONG UNIV OF SCI & TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products