CN108441248A - A method of being prepared as raw material using discarded Poplar Powder has antioxidative bio oil - Google Patents
A method of being prepared as raw material using discarded Poplar Powder has antioxidative bio oil Download PDFInfo
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- CN108441248A CN108441248A CN201810297868.0A CN201810297868A CN108441248A CN 108441248 A CN108441248 A CN 108441248A CN 201810297868 A CN201810297868 A CN 201810297868A CN 108441248 A CN108441248 A CN 108441248A
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- bio oil
- liquefaction
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- raw material
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
Abstract
The method with antioxidative bio oil being prepared as raw material to discard Poplar Powder the present invention relates to a kind of, belongs to biomass utilization technologies field.Bio oil is prepared by liquefaction as raw material in the waste poplar that this method is generated using industrial processes.Liquefaction device therefor is batch reactor, and liquefaction solvent is water, and 220~280 DEG C of reaction temperature keeps the temperature 30min, and liquefaction products obtain bio oil through filtering, extracting, extraction and rotary evaporation.The inventive method, which realizes, discards efficiently using for Poplar Powder in industrial processes, operating method is simple, while liquefaction condition uses water as solvent, is conducive to environmental protection.Producing obtained biological oil product, there is stronger inoxidizability, free radical elimination factor to be up to 90.85%, have a good application prospect.
Description
Technical field
The invention belongs to biomass utilization technologies fields, are related to a kind of preparation method having antioxidative bio oil.
Technical background
Biomass content is abundant and renewable, is the important regenerative resource for replacing fossil fuel.Turn of biomass at present
Change technology mainly has biochemical transformation and thermochemical study, and wherein thermochemical study includes mainly pyrolysis, liquefaction and gasification, production
Object includes gas, liquid and solid, and wherein product liquid is commonly referred to as bio oil.Bio oil chemical composition is complex, mainly
Contain the compounds such as ketone, aldehyde, phenol, alkene, aliphatic acid and esters.
Fast pyrogenation prepares bio oil because the advantages that its rate of heat addition is fast, the gas phase residence time is short is generally adopted by laboratory
With.But equipment energy consumption used by fast pyrogenation is big, raw material needs drying and dehydrating, the bio oil high oxygen content of gained (30%~
60%), extensive use is not yet received in this method at present.Hydrothermal liquefaction process is using water as solvent, and water has higher electricity under high temperature
From constant, soda acid self-catalysis may be implemented.Hydrothermal liquefaction prepares bio oil and usually utilizes thermal energy of the water under sub-/overcritical, will
The molecular link of larger molecular organics, hydrocarbon in biomass interrupts, while also will be between organic molecule and heavy metal ion
Chelate bonds interrupt so that heavy metal release enter aqueous solution generate coarse biometric oil.Usual hydrothermal liquefaction prepares biology in interval
It is carried out in reaction kettle, obtained solid-liquid mixture need to be filtered, and solid is further extracted to obtain residue with organic solvent
With bio oil (heavy oil), and liquid obtains bio oil (light oil) by the modes such as extraction and separation, rotary evaporation.At present waste,
The biomass such as algae and forest prepare bio oil and are reported.Chinese patent CN105733693A is with a kind of algae and wooden
Biomass is raw material, and alcohol-water cosolvent is that reaction medium carries out co grinding method and prepares bio oil, realizes algae and Wooden Biomass
Recycling；Chinese patent CN103265967A is reported during hydrothermal liquefaction prepares bio oil, by hydrogen supply dissolvent
Introduce traditional CO/H2O/ base metal catalysts create " a hydrogen supply dissolvent/H2The new line of O " is particularly suitable for moisture content
High biomass.Largely discarded wood powder is produced in poplar process, is to realize Poplar Resource synthesis to its processing and utilization
The important channel utilized.The present invention, which proposes a kind of prepared as raw material using discarded Poplar Powder, has antioxidative bio oil
Method.
Invention content
The purpose of the present invention is to propose to a kind of the side with antioxidative bio oil being prepared as raw material to discard Poplar Powder
Method.Specifically, the present invention is using discarded Poplar Powder as raw material, and using water as solvent, being prepared using batch reactor has antioxygen
The bio oil for the property changed.
The method using discarded wood powder as raw material liquefaction preparation with antioxidative bio oil proposed by the present invention, including with
Lower step：
(1) it is the Poplar Powder and water in mass ratio 1 of 20~80 mesh by granularity:10 mixing, are put into batch reactor,
It is purged with the air in cleaning reaction kettle with nitrogen, it is 220~280 DEG C that reaction temperature is arranged after sealing, in stirring condition
Lower soaking time 30min stops heating, is passed through cold water in system, reaction system is cooled to room temperature later, obtains solid-liquid mixing
Object；
(2) above-mentioned reaction mixture is separated by solid-liquid separation with funnel, the solid of gained is carried with acetone in Soxhlet after filtering
It takes in device and is stripped, extract until extracting solution color becomes colorless, the liquid of gained is rotated with Rotary Evaporators after extracting
Evaporative removal solvent, extract are placed in drying 12h in 60 DEG C of baking ovens and obtain weight bio oil；It is separated by solid-liquid separation the aqueous solution second of gained
Ethyl acetate phase and water phase is obtained by extraction in acetoacetic ester, and ethyl acetate phase rotary evaporation is removed solvent, is subsequently placed in 60 DEG C of bakings
12h is dried in case, obtains light bio oil.
It is proposed by the present invention to prepare the method with antioxidative bio oil, its advantage is that：
(1) liquefaction solvent that the present invention uses is water, and compared with acid, alkali, organic solvent, cost is relatively low, acetone used
Recyclable with ethyl acetate, preparation process does not pollute environment structure.
(2) present invention realizes the reasonable utilization of tree growth law waste resource, and the random disposition of reduction is discarded wood powder and caused
Problem of environmental pollution.
(3) present invention carries out the preparation of bio oil using hydrothermal liquefaction method, and liquefaction process and easy to operate has potential
Application prospect.
Specific implementation mode
A kind of liquefied for raw material using discarded wood powder proposed by the present invention prepares the method with antioxidative bio oil,
Include the following steps：
(1) it is the Poplar Powder and water in mass ratio 1 of 20~80 mesh by granularity:10 mixing, are put into batch reactor,
It is purged with the air in cleaning reaction kettle with nitrogen, it is 220~280 DEG C that reaction temperature is arranged after sealing, in stirring condition
Lower soaking time 30min stops heating, is passed through cold water in system, reaction system is cooled to room temperature later, obtains solid-liquid mixing
Object；
Above-mentioned reaction mixture is separated by solid-liquid separation with funnel, the solid acetone of gained is in Soxhlet extractor after filtering
In be stripped, extract until extracting solution color becomes colorless, after extracting gained liquid Rotary Evaporators rotary evaporation
Solvent is removed, extract is placed in drying 12h in 60 DEG C of baking ovens and obtains weight bio oil；It is separated by solid-liquid separation the aqueous solution acetic acid second of gained
Ethyl acetate phase and water phase is obtained by extraction in ester, and ethyl acetate phase rotary evaporation is removed solvent, is subsequently placed in 60 DEG C of baking ovens
12h is dried, light bio oil is obtained.The bio oil of above-mentioned gained is used into literature procedure (Lu Xiaoxiang, Chen Jie, Tang Jinzhong, four
The Study of Antioxidation of kind camellia, food research and development, 2006 (8):Inoxidizability 22-25) is measured, bio oil is calculated
Free radical scavenging activity.
The embodiment of the method for the present invention is described below：
Embodiment 1：
(1) it is the Poplar Powder and water in mass ratio 1 of 20~80 mesh by granularity:10 mixing, are put into batch reactor,
It is purged with the air in cleaning reaction kettle with nitrogen, it is 220 DEG C that reaction temperature is arranged after sealing, is kept the temperature under agitation
Time 30min stops heating, is passed through cold water in system, reaction system is cooled to room temperature, solidliquid mixture is obtained later；
(2) above-mentioned reaction mixture is separated by solid-liquid separation with funnel, the solid of gained is carried with acetone in Soxhlet after filtering
It takes in device and is stripped, extract until extracting solution color becomes colorless, the liquid of gained is rotated with Rotary Evaporators after extracting
Evaporative removal solvent, extract are placed in drying 12h in 60 DEG C of baking ovens and obtain weight bio oil；It is separated by solid-liquid separation the aqueous solution second of gained
Ethyl acetate phase and water phase is obtained by extraction in acetoacetic ester, and ethyl acetate phase rotary evaporation is removed solvent, is subsequently placed in 60 DEG C of bakings
12h is dried in case, obtains light bio oil.Weight bio oil yield 7.28%, free radical scavenging activity 86.77%；Light bio oil yield
2.10%, free radical scavenging activity 86.78%.
Embodiment 2：
(1) it is the Poplar Powder and water in mass ratio 1 of 20~80 mesh by granularity:10 mixing, are put into batch reactor,
It being purged with nitrogen to remove air, it is 240 DEG C that reaction temperature is arranged after sealing, under agitation soaking time 30min,
Stop heating later, being passed through cold water in system is cooled to room temperature, and solidliquid mixture is obtained；
(2) above-mentioned reaction mixture is separated by solid-liquid separation with funnel, the solid of gained is carried with acetone in Soxhlet after filtering
It takes in device and is stripped, extract until extracting solution color becomes colorless, the liquid of gained is carried out with Rotary Evaporators after extracting
Rotary evaporation removes solvent, and extract is placed in drying 12h in 60 DEG C of baking ovens and obtains weight bio oil；It is separated by solid-liquid separation the aqueous solution of gained
It is extracted with ethyl acetate to obtain ethyl acetate phase and water phase, and ethyl acetate phase rotary evaporation is removed into solvent, be subsequently placed in 60
12h is dried in DEG C baking oven, obtains light bio oil.Weight bio oil yield 10.38%, free radical scavenging activity 75.87%；Light bio oil
Yield 2.99%, free radical scavenging activity 90.29%.
Embodiment 3：
(1) it is the Poplar Powder and water in mass ratio 1 of 20~80 mesh by granularity:10 mixing, are put into batch reactor,
It is purged with the air in cleaning reaction kettle with nitrogen, it is 260 DEG C that reaction temperature is arranged after sealing, is kept the temperature under agitation
Time 30min stops heating, is passed through cold water in system, reaction system is cooled to room temperature, solidliquid mixture is obtained later；
(2) above-mentioned reaction mixture is separated by solid-liquid separation with funnel, the solid of gained is carried with acetone in Soxhlet after filtering
It takes in device and is stripped, extract until extracting solution color becomes colorless, the liquid of gained is rotated with Rotary Evaporators after extracting
Evaporative removal solvent, extract are placed in drying 12h in 60 DEG C of baking ovens and obtain weight bio oil；It is separated by solid-liquid separation the aqueous solution second of gained
Ethyl acetate phase and water phase is obtained by extraction in acetoacetic ester, and ethyl acetate phase rotary evaporation is removed solvent, is subsequently placed in 60 DEG C of bakings
12h is dried in case, obtains light bio oil.Weight bio oil yield 12.00%, free radical scavenging activity 72.21%；Light bio oil yield
2.49%, free radical scavenging activity 90.28%.
Embodiment 4：
(1) it is the Poplar Powder and water in mass ratio 1 of 20~80 mesh by granularity:10 mixing, are put into batch reactor,
It is purged with the air in cleaning reaction kettle with nitrogen, it is 280 DEG C that reaction temperature is arranged after sealing, is kept the temperature under agitation
Time 30min stops heating, is passed through cold water in system, reaction system is cooled to room temperature, solidliquid mixture is obtained later；
(2) above-mentioned reaction mixture is separated by solid-liquid separation with funnel, the solid of gained is carried with acetone in Soxhlet after filtering
It takes in device and is stripped, extract until extracting solution color becomes colorless, the liquid of gained is rotated with Rotary Evaporators after extracting
Evaporative removal solvent, extract are placed in drying 12h in 60 DEG C of baking ovens and obtain weight bio oil；It is separated by solid-liquid separation the aqueous solution second of gained
Ethyl acetate phase and water phase is obtained by extraction in acetoacetic ester, and ethyl acetate phase rotary evaporation is removed solvent, is subsequently placed in 60 DEG C of bakings
12h is dried in case, obtains light bio oil.Weight bio oil yield 12.10%, free radical scavenging activity 75.29%；Light bio oil yield
3.15%, free radical scavenging activity 90.85%.
Claims (1)
1. a kind of preparing the method with antioxidative bio oil to discard Poplar Powder as raw material, it is characterised in that this method packet
Include following steps：
(1) it is the Poplar Powder and water in mass ratio 1 of 20~80 mesh by granularity:10 mixing, are put into batch reactor, use nitrogen
Gas carries out purging and removes air, and it is 220~280 DEG C that reaction temperature is arranged after sealing, under agitation soaking time 30min,
Stop heating later, being passed through cold water in system is cooled to room temperature, and solidliquid mixture is obtained；
(2) above-mentioned reaction mixture is separated by solid-liquid separation with funnel, the solid acetone of gained is in Soxhlet extractor after filtering
In be stripped, extract until extracting solution color becomes colorless, after extracting gained liquid Rotary Evaporators rotary evaporation
Solvent is removed, extract is placed in drying 12h in 60 DEG C of baking ovens and obtains weight bio oil；It is separated by solid-liquid separation the aqueous solution acetic acid second of gained
Ethyl acetate phase and water phase is obtained by extraction in ester, and ethyl acetate phase rotary evaporation is removed solvent, is subsequently placed in 60 DEG C of baking ovens
12h is dried, light bio oil is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810297868.0A CN108441248A (en) | 2018-04-03 | 2018-04-03 | A method of being prepared as raw material using discarded Poplar Powder has antioxidative bio oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810297868.0A CN108441248A (en) | 2018-04-03 | 2018-04-03 | A method of being prepared as raw material using discarded Poplar Powder has antioxidative bio oil |
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| CN108441248A true CN108441248A (en) | 2018-08-24 |
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| CN201810297868.0A Pending CN108441248A (en) | 2018-04-03 | 2018-04-03 | A method of being prepared as raw material using discarded Poplar Powder has antioxidative bio oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852468A (en) * | 2020-12-23 | 2021-05-28 | 北京林业大学 | Method for preparing biological oil rich in phenolic compounds by liquefying eucalyptus black liquor |
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| CN101294076A (en) * | 2008-06-17 | 2008-10-29 | 南昌大学 | Method for preparing biological diesel oil antioxidant additive with biomass microwave auxiliary directional thermal decomposition |
| CN103060023A (en) * | 2011-10-24 | 2013-04-24 | 上海复寰生物质能源有限公司 | Method for preparing bio-oil by rice straw |
| CN103102253A (en) * | 2012-12-26 | 2013-05-15 | 宋卫华 | Method for comprehensively utilizing straw liquid by liquefaction and separation |
| CN103159595A (en) * | 2013-03-06 | 2013-06-19 | 复旦大学 | Method for preparing phenolic compound by liquefaction of salix mongolica |
| CN104774636A (en) * | 2015-03-31 | 2015-07-15 | 天津大学 | Preparation method of biological oil |
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2018
- 2018-04-03 CN CN201810297868.0A patent/CN108441248A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294076A (en) * | 2008-06-17 | 2008-10-29 | 南昌大学 | Method for preparing biological diesel oil antioxidant additive with biomass microwave auxiliary directional thermal decomposition |
| CN103060023A (en) * | 2011-10-24 | 2013-04-24 | 上海复寰生物质能源有限公司 | Method for preparing bio-oil by rice straw |
| CN103102253A (en) * | 2012-12-26 | 2013-05-15 | 宋卫华 | Method for comprehensively utilizing straw liquid by liquefaction and separation |
| CN103159595A (en) * | 2013-03-06 | 2013-06-19 | 复旦大学 | Method for preparing phenolic compound by liquefaction of salix mongolica |
| CN104774636A (en) * | 2015-03-31 | 2015-07-15 | 天津大学 | Preparation method of biological oil |
Non-Patent Citations (1)
| Title |
|---|
| 邹勇等: "木屑快速热解生物油中酚类提取物的抗氧化及抑真菌活性研究", 《西北林学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852468A (en) * | 2020-12-23 | 2021-05-28 | 北京林业大学 | Method for preparing biological oil rich in phenolic compounds by liquefying eucalyptus black liquor |
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Application publication date: 20180824 |