Method for preparing bio-oil by performing two-step grading hydrothermal liquification on lignocellulose under CO2 atmosphere

A lignocellulose and hydrothermal liquefaction technology, which is used in the preparation of liquid hydrocarbon mixtures, the petroleum industry, and the treatment of hydrocarbon oil, etc., can solve the problems of low biomass conversion rate, high equipment performance requirements, complex product components, etc. The effect of short reaction time, high bio-oil yield and high product conversion rate

Active Publication Date: 2018-03-30
SHENYANG AEROSPACE UNIVERSITY
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

Supercritical CO 2 Pretreatment is easier for subsequent hydrolysis, but this method is similar to steam explosion, and rapid pressure relief requires high equipment
[0005] Based on the current research results of hydrothermal liquefaction of lignocellulosic biomass, the preparation of bio-oil by ordinary hydrothermal liquefaction has high temperature and high pressure, resulting in high energy consumption and high requirements for equipment performance, as well as low biomass conversion rate and bio-oil yield and product. In order to realize the industrialization of lignocellulosic biomass energy, develop new, efficient and practical pretreatment methods, and reduce the complexity of bio-oil chemical components to achieve directional enrichment of specific intermediate products, so that the components are relatively Liquid phase products as chemical production platform compounds will be the main research direction in the field of supercritical fluid liquefaction to produce bio-oil
Currently about CO 2 Two-step fractional liquefaction of lignocellulose under atmosphere to produce bio-oil has not been reported

Method used

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  • Method for preparing bio-oil by performing two-step grading hydrothermal liquification on lignocellulose under CO2 atmosphere
  • Method for preparing bio-oil by performing two-step grading hydrothermal liquification on lignocellulose under CO2 atmosphere
  • Method for preparing bio-oil by performing two-step grading hydrothermal liquification on lignocellulose under CO2 atmosphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] After crushing and sieving, the rice straw is selected to be 30-50 mesh. Add 15g of rice straw powder into an intermittent high-temperature and high-pressure reactor with a magnetic stirrer (Yantai Songling Chemical Industry Co., Ltd.), add 150mL of deionized water, stir evenly with a glass rod, seal the reactor, and use high-purity carbon dioxide to Purge and replace the air in the kettle. Heat to the required reaction temperature of 200°C through the heating rate of the external heating mantle, and keep for a certain reaction time of 10 minutes. The magnetic stirrer rotates at 100r / min. The above is the pretreatment step.

[0061] Then stay at 270°C, 295°C, 320°C, and 345°C for 15 minutes and 30 minutes in the high temperature stage respectively. A subsequent liquefaction stage produces bio-oil. After the reaction was over, the heating mantle was removed and the reactor was cooled by a fan. When the temperature in the kettle drops to about room temperature, open th...

Embodiment 2

[0069] The solvent water is replaced with ethanol, and the specific operation is the same as that of Example 1. In the separation step, the mixture is suction-filtered with acetone, and the bio-oil can be obtained after constant-temperature rotary evaporation in a water bath at 82-85°C. As shown in Table 6, the product conversion rate can reach about 41.83-80.16%, and the bio-oil yield is 26.40-47.78%. As shown in Table 7, when the reaction temperature is 320°C and the residence time is 15 minutes, the bio-oil yield is the highest at 47.78%, and the bio-oil GC-MS detects 69 compounds, most of which are ester compounds, with a calorific value of 28.62 MJ / kg.

[0070] Table 6 Distribution of liquefaction products in two-step liquefaction with ethanol as solvent

[0071]

[0072] Table 7 GC-MS analysis of two-step liquefied bio-oil with ethanol as solvent (reaction condition: 320℃, 15min)

[0073]

[0074]

[0075]

Embodiment 3

[0077] The specific operation of replacing water with a mixed solution of water and ethanol with a volume ratio of 1:1 is consistent with Example 1. As shown in Table 8, the product conversion rate can reach about 78.55-88.37%, and the bio-oil yield is 30.97-50.66%. As shown in Table 9, when the reaction temperature is 270°C and the residence time is 30 minutes, the bio-oil yield is the highest at 50.66%, and the bio-oil GC-MS detects 83 compounds with a calorific value of 24.6MJ / kg. However, when the reaction temperature is 320°C and the residence time is 30min, the highest bio-oil yield is 31.96%, and the calorific value is 30.22MJ / kg.

[0078] Table 8 Distribution of liquefaction products in two-step liquefaction with water and ethanol (volume 1:1) as solvent

[0079]

[0080]

[0081] Table 9 GC-MS analysis of two-step liquefied bio-oil with water and ethanol (volume 1:1) as solvent (reaction condition: 270°C, 30min)

[0082]

[0083]

[0084]

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Abstract

The invention belongs to the technical field of green renewable energy of bio-oil prepared by biomass, and in particular relates to a method for preparing bio-oil by performing two-step grading hydrothermal liquification on lignocellulose under CO2 atmosphere. The invention provides a method for preparing bio-oil and chemical products with high additional value by performing high-temperature and high-pressure liquification on lignocelluloses biomass in an intermittent reaction kettle. According to the method, gas generated based on liquification reaction is CO2 mainly, the defect that supercritical CO2 fluid cannot be directly extracted to prepare the bio-oil is overcome, the CO2 and the solvent form an acidic thermal solvent by a mode of externally supplying the CO2 to achieve the pretreatment coupling effect, the integrated liquification process is divided into a plurality of stages based on different heat stability of three components, such as cellulose, hemicellulose and lignin, ofthe lignocelluloses, the conversion rate and the yield of the bio-oil are further increased, the generation quantity of residues and gases are reduced, and directional regulation and control of the biomass liquification process are realized.

Description

technical field [0001] The invention belongs to the technical field of green renewable energy for preparing bio-oil from biomass, and specifically relates to a CO 2 A method for preparing bio-oil by two-step hydrothermal liquefaction of lignocellulose under atmosphere. Background technique [0002] Biomass is one of the most promising renewable energy sources amid rising energy demand and depletion of fossil fuels. The annual output of crop straw in my country is about 700 million tons, and the resources are rich and have broad development potential. Due to the wide distribution and low utilization rate of straw, most of them have not been rationally utilized, causing air and water pollution. In recent years, the green chemical technology represented by supercritical fluid technology has developed rapidly, and has achieved fruitful results and progress in the research and application of the energy field. On the one hand, supercritical fluid bio-oil can enhance the mass tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G1/00
CPCC10G1/00C10G2300/1011
Inventor 杨天华王建李润东李秉硕开兴平
Owner SHENYANG AEROSPACE UNIVERSITY
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