CN101798524B - Method for poly-generation of extracting and separating biological oil with two solvents - Google Patents
Method for poly-generation of extracting and separating biological oil with two solvents Download PDFInfo
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- CN101798524B CN101798524B CN2010101138434A CN201010113843A CN101798524B CN 101798524 B CN101798524 B CN 101798524B CN 2010101138434 A CN2010101138434 A CN 2010101138434A CN 201010113843 A CN201010113843 A CN 201010113843A CN 101798524 B CN101798524 B CN 101798524B
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Abstract
The invention discloses a method for poly-generation of extracting and separating biological oil with two solvents, which comprises the following steps of: firstly, using ether as a solvent to extract the biological oil at the normal temperature and the normal pressure so as to obtain an ether soluble substance (ES); secondly, adding dichloromethane into the remaining ether insoluble substance (EIS) at the normal temperature and the normal pressure to obtain a dichloromethane soluble substance (DCMS) and a dichloromethane insoluble substance (DCMIS); and thirdly, perform low-temperature drying on the two products to obtain a lignin component, wherein the two solvents, namely the ether and the dichloromethane can be reclaimed for cyclic utilization by adopting a rotary evaporation method. The method can effectively separate out the lignin component (the lignin component can be used for preparing chemical products with high added values after reprocessing) in the biological oil, the ether soluble substance can be used as a derivative of the biological oil, and the physical and chemical properties of the ether soluble substance are greatly improved. The method solves the aging problems of the whole biological oil in the storing process. The method has simple technological operations, and can realize poly-generation application of the biological oil easily.
Description
Technical field
The present invention relates to a kind of fractional separation Poly-generation method of bio oil, particularly a kind of double solvent extraction method of bio oil.
Background technology
The energy and environment problem gets more and more people's extensive concerning.Flourish along with economy; It is more and more outstanding with environmental pollution that power supply is not enough; Fossil oil not only is difficult to satisfy the needs of human society industrial development at present; And, caused a series of problems such as " acid rain ", " Greenhouse effect " because exploitation has excessively brought serious topsoil, brought very serious consequence to existent environment of people.Therefore, countries in the world all begin to be devoted to develop the renewable energy source of cleaning, separate the environment crisis to replace traditional fossil energy to ease up.Biomass energy in use produces environmental pollution hardly as a kind of important renewable energy, and realizes CO
2" near zero release ".The environment friendly of biomass energy makes it to become the important component part of following Sustainable development energy resource system.The multi-functional characteristic of biomass has promoted countries in the world to accelerate the paces of biomass energy technological development and biomass resource application under backgrounds such as energy dilemma, environmental pollution, disruption of ecological balance.The U.S. has formulated " biomass technological line figure " in 2002, European Union 2006 issue " biomass energy action plan " etc.Classify the biomass energy technology as renewable energy source focus technology development field in China's National Program for Medium-to Long-term Scientific and Technological Development in 2004.It is like a raging fire that the research of biomass energy is carried out, and do not base oneself upon current resources situation and research and development strength, the trend of blindly following but also expose.The development biomass energy is badly in need of wanting scientific guiding, realizes incrementally, and fast development is beneficial to give full play to the multifunctionality of biomass energy.Expect mid-21st Century, various biomass renewable energy sources will account for more than 40% of global total energy consumption.The advantage of bio oil is that not only it is the energy derive of no greenhouse gas emission, and it can reduce the dependence of present human society to fossil oil, the realization Sustainable development.But chemical constitution complicated in the bio oil causes its character relatively poor, and high-moisture, rich oxygen content, HV, high acidity, storage are prone to aging layering or the like.All these shortcomings cause bio oil nonflammable, can't use on a large scale.Up to the present, very ripe both at home and abroad for the understanding of biomass pyrolytic technology, developed different types of pyrolysis reactor, obtained to make the correlation parameter of maximize production, but the shortcoming of above-mentioned bio oil more requires the maximization of bio oil quality.Existing both at home and abroad many scholars are in the research of carrying out aspect the bio oil quality-improving; And the fractional separation Poly-generation technology of bio oil is as the part of bio oil upgrading; Not only help farthest using bio oil, promote its quality, and can access the Chemicals of high value.
Summary of the invention
Technical problem: in storage process, be prone to take place the aged phenomenon in order to solve bio oil; As the part of bio oil quality-improving and the Chemicals that can obtain high added value, the invention provides a kind of method of double solvent extraction fractional separation bio oil Poly-generation simultaneously.
Technical scheme: the present invention at first uses the ether of 50-70 part as solvent, joins with even velocity in the bio oil of 30-50 part, stirs the mixture static layering about 20 minutes.Collect upper solution-ether soluble substance and lower floor's solution-ether insolubles.The methylene dichloride of then getting 60-70 part joins with even velocity in the ether insolubles of 30-40 part as solvent, stirs the mixture standing demix about 20 minutes.Collect upper solution-methylene dichloride solvend and lower floor's solution-methylene dichloride insolubles.
Ether soluble substance is as the verivate of bio oil, owing to isolated macromolecular xylogen part, so its physical and chemical performance is compared with bio oil and increased significantly.The fuel that can be used as stable in properties uses.
Next the methylene dichloride solvend is carried out filtration under diminished pressure and lyophilize, the lyophilize temperature is :-50 ℃.Lyophilize pressure is: 0.024mBar.Obtain low-molecular-weight pyrolysis lignin powder.
The methylene dichloride insolubles is adopted same filtration under diminished pressure and lyophilize, and the lyophilize temperature is :-50 ℃.Lyophilize pressure is: 0.024mBar.Obtain high-molecular weight pyrolysis lignin powder.
The present invention utilizes macromolecular lignin component in the bio oil not to be soluble in the character of ether, utilizes ether as extraction agent, and extracting influences the most serious lignin component of bio oil ageing property, obtains the verivate-ether soluble substance of bio oil.The inventive method can solve bio oil well and be prone to the aged shortcoming, and after carrying out deep processing for the lignin component of separating, can be used as good Chemicals.
The present invention also has the following advantages:
1, the bio oil extracting and separating is obtained ether soluble substance, macromole xylogen and small molecules xylogen, utilization ratio is high.
2, extraction agent ether, methylene dichloride all can be through the mode recycle and reuse of rotary evaporation.Utilization ratio is high, has reduced the isolating cost price of bio oil.
3, this technological operation is simple, realizes the Poly-generation of bio oil easily.
Description of drawings
Fig. 1 is a process flow sheet of the present invention,
Fig. 2 is GC-MS (gas chromatography mass spectrometry) spectrogram of bio oil,
Fig. 3 is GC-MS (gas chromatography mass spectrometry) spectrogram of bio oil verivate-ether soluble substance.
Embodiment
Below in conjunction with embodiment the present invention is done further description.In order to prove repeatability of the present invention, three groups of embodiment have been carried out.
The bio oil that the present invention uses is provided by the famous VTT company of Finland, and raw material is a cork.The bio oil water ratio is 28.05wt.%.The sample water ratio adopts Ka Erfei to amend the law to measure according to ASTM D 1744 standards in the test.
Embodiment 1:
Get the 20g ether, at ambient temperature, join in the 10g bio oil, stirred the mixture static layering about 20 minutes with even velocity.Isolate upper solution, be transferred to Rotary Evaporators, evaporate ether, obtain ether soluble substance 4.1g, so the productive rate of ether soluble substance is 41wt.% in the bio oil.Weighing lower floor solution, weight are 5.4g, and promptly the productive rate of ether insolubles is 54%.At this moment, the utilization ratio of bio oil is 95wt.%.
Get the 15g methylene dichloride, at ambient temperature, join in the 5.4g ether insolubles, stirred the mixture static layering about 20 minutes with even velocity.Isolate upper solution, move to Rotary Evaporators, evaporate methylene dichloride, obtain the methylene dichloride solvend, the methylene dichloride solvend is carried out filtration under diminished pressure, then sample was placed in-50 ℃, the freeze drier of 0.024mBar 48 hours.Obtain low uniformly molecule xylogen powder at last.Be weighed as 1.8g.Therefore low molecule xylogen powder productive rate is 18wt.% in the bio oil.
After the methylene dichloride insolubles adopted filtration under diminished pressure, sample was placed equally in-50 ℃, the freeze drier of 0.024mBar 48 hours.Obtain uniform polymer wood quality powder at last.Be weighed as 2.6g.Therefore low molecule xylogen powder productive rate is 26wt.% in the bio oil.
To sum up, the utilization ratio of bio oil in whole sepn process is 85wt% among the embodiment 1.
Embodiment 2:
Get the 20g ether, at ambient temperature, join in the 10g bio oil, stirred the mixture static layering about 20 minutes with even velocity.Isolate upper solution, be transferred to Rotary Evaporators, evaporate ether, obtain ether soluble substance 3.8g, so the productive rate of ether soluble substance is 38wt.% in the bio oil.Weighing lower floor solution, weight are 5.2g, and promptly the productive rate of ether insolubles is 52%.At this moment, the utilization ratio of bio oil is 90wt.%.
Get the 15g methylene dichloride, at ambient temperature, join in the 5.5g ether insolubles, stirred the mixture static layering about 20 minutes with even velocity.Isolate upper solution, move to Rotary Evaporators, evaporate methylene dichloride, obtain the methylene dichloride solvend, the methylene dichloride solvend is carried out filtration under diminished pressure, then sample was placed in-50 ℃, the freeze drier of 0.024mBar 48 hours.Obtain low uniformly molecule xylogen powder at last.Be weighed as 1.9g.Therefore low molecule xylogen powder productive rate is 19wt.% in the bio oil.
After the methylene dichloride insolubles adopted filtration under diminished pressure, sample was placed equally in-50 ℃, the freeze drier of 0.024mBar 48 hours.Obtain uniform polymer wood quality powder at last.Be weighed as 2.9g.Therefore low molecule xylogen powder productive rate is 29wt.% in the bio oil.
To sum up, the utilization ratio of bio oil in whole sepn process is 86wt% among the embodiment 2.
Embodiment 3:
Get the 20g ether, at ambient temperature, join in the 10g bio oil, stirred the mixture static layering about 20 minutes with even velocity.Isolate upper solution, be transferred to Rotary Evaporators, evaporate ether, obtain ether soluble substance 3.7g, so the productive rate of ether soluble substance is 37wt.% in the bio oil.Weighing lower floor solution, weight are 5.5g, and promptly the productive rate of ether insolubles is 55%.At this moment, the utilization ratio of bio oil is 92wt.%.
Get the 15g methylene dichloride, at ambient temperature, join in the 5.5g ether insolubles, stirred the mixture static layering about 20 minutes with even velocity.Isolate upper solution, move to Rotary Evaporators, evaporate methylene dichloride, obtain the methylene dichloride solvend, the methylene dichloride solvend is carried out filtration under diminished pressure, then sample was placed in-50 ℃, the freeze drier of 0.024mBar 48 hours.Obtain low uniformly molecule xylogen powder at last.Be weighed as 1.6g.Therefore low molecule xylogen powder productive rate is 16wt.% in the bio oil.
After the methylene dichloride insolubles adopted filtration under diminished pressure, sample was placed equally in-50 ℃, the freeze drier of 0.024mBar 48 hours.Obtain uniform polymer wood quality powder at last.Be weighed as 2.8g.Therefore low molecule xylogen powder productive rate is 28wt.% in the bio oil.
To sum up, the utilization ratio of bio oil in whole sepn process is 81wt% among the embodiment 3.
Claims (2)
1. the method for a poly-generation of extracting and separating biological oil with two solvents is characterized in that this method may further comprise the steps:
1), the ether of getting 50-70 part is as solvent, joins with even velocity in the bio oil of 30-50 part, stirs the mixture static layering 20 minutes; Collect upper solution-ether soluble substance and lower floor's solution-ether insolubles; Then ether soluble substance is rotated evaporation, the distilling off solvent ether;
2), the methylene dichloride of getting 60-70 part is as solvent, joins with even velocity in the ether insolubles of 30-40 part, stirs the mixture standing demix 20 minutes; Collect upper solution-methylene dichloride solvend and lower floor's solution-methylene dichloride insolubles; Then upper solution is rotated evaporation, distills out methylene dichloride, obtain the methylene dichloride solvend, afterwards the methylene dichloride solvend that obtains is carried out filtration under diminished pressure, then carry out lyophilize and obtain low-molecular-weight relatively pyrolysis lignin powder;
To step 2) in the methylene dichloride insolubles that obtains carry out filtration under diminished pressure, then carry out lyophilize and obtain relative high-molecular weight pyrolysis lignin powder.
2. the method for poly-generation of extracting and separating biological oil with two solvents according to claim 1, it is characterized in that: said ether, methylene dichloride are as the extraction agent recycle.
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| CN102851072A (en) * | 2012-07-30 | 2013-01-02 | 东南大学 | Method for refining waste paperboard pyrolytic oil |
| CN103524283B (en) * | 2013-10-12 | 2015-07-08 | 浙江大学 | Method for extracting monophenol compounds and pyrolysis lignin from biological oil |
| CN103740461B (en) * | 2014-01-11 | 2018-03-06 | 河南工业大学 | A kind of method of refining for bio oil multi-stage separation |
| CN106244251A (en) * | 2016-08-04 | 2016-12-21 | 陈永林 | A kind of method utilizing abandoned biomass to prepare biofuel oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1045119A (en) * | 1989-02-27 | 1990-09-05 | 科尔-麦克基公司 | Solvent extraction method |
| CN101338221A (en) * | 2008-08-20 | 2009-01-07 | 河北科技大学 | Fuel oil desulfurization process by ionic liquid extraction-photocatalytic oxidation method |
| CN101497594A (en) * | 2009-03-03 | 2009-08-05 | 东北林业大学 | Method for extracting, separating and purifying genistein from pigeon pea rhizome |
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| US20040078870A1 (en) * | 2002-10-29 | 2004-04-29 | Jones Herbert R. | Cap-attachable peripheral-viewing mirrors assembly |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1045119A (en) * | 1989-02-27 | 1990-09-05 | 科尔-麦克基公司 | Solvent extraction method |
| CN101338221A (en) * | 2008-08-20 | 2009-01-07 | 河北科技大学 | Fuel oil desulfurization process by ionic liquid extraction-photocatalytic oxidation method |
| CN101497594A (en) * | 2009-03-03 | 2009-08-05 | 东北林业大学 | Method for extracting, separating and purifying genistein from pigeon pea rhizome |
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