CN104327888A - Method for preparing biodiesel from shiny-leaved yellowhorn kernels under microwave catalysis - Google Patents
Method for preparing biodiesel from shiny-leaved yellowhorn kernels under microwave catalysis Download PDFInfo
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- CN104327888A CN104327888A CN201410685845.9A CN201410685845A CN104327888A CN 104327888 A CN104327888 A CN 104327888A CN 201410685845 A CN201410685845 A CN 201410685845A CN 104327888 A CN104327888 A CN 104327888A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention discloses a method for preparing biodiesel from shiny-leaved yellowhorn kernels under microwave catalysis and aims to provide a method which has the advantages that the reaction speed is high, the reaction time is greatly shortened, high efficiency and energy conservation can be achieved, the oil extraction rate is high, the oil quality is high, the reacted products are automatically separated from catalysts, the separation process is easy and convenient, the corrosion is low and the emission amount of alkali wastewater is small. According to the technical key points, the method comprises the following steps: 1) in a microwave reactor, by taking shiny-leaved yellowhorn kernels as raw materials, by taking ionic liquid and alkali as phase transfer catalysts and by taking a short chain alcohol as a solvent, reacting at the temperature of 40-80 DEG C for 3-25 minutes to finish extraction of oil of the shiny-leaved yellowhorn kernels and synthesis of biodiesel through a one-pot process; and 2) standing and layering after the reaction is ended, and separating out the products, wherein the product on the upper layer is the biodiesel. The method belongs to the technical fields of agricultural product processing technology and green renewable energy sources.
Description
Technical field
The invention provides a kind of clean, to prepare with ionic liquid-catalyzed Wood of Shinyleaf Yellowhorn kind benevolence single stage method biofuel method, belong to agro-processing technology and technical field of green regenerative energy sources.
Background technology
Along with the development of world industry and the sustainable growth of population in the world, energy demand gets more and more, and energy dilemma is one of main problem of facing of modern social development.But along with the fast development of economic globalization, countries in the world also increase day by day for the demand of Energy resources, and oil reserve also constantly reduces, can predict in the near future prospective oil by approach exhaustion.Biofuel, as the potential substitute of crude oil, be a kind of can be the green energy resource of Material synthesis by the waterplant greases such as various oil crops, Wild oil plant and engineered microbes algae and animal grease and discarded food and drink wet goods.Biofuel is compared with crude oil, and advantage is its recyclability and the feature of environmental protection.
The method obtaining biofuel mainly comprises directly makes usage, hybrid system, microemulsion method, high temperature pyrolytic cracking and ester-interchange method.Through assessing the many-side such as transformation efficiency, practical application, production cost of biofuel technology of preparing, what be mainly used in biofuel large-scale production at present is ester-interchange method.Ester-interchange method refers to triglyceride level in raw materials such as utilizing animal-plant oil and short chain alcohol, generates the process of corresponding fatty acid ester under certain condition by there is transesterification.Its reaction product can obtain biodiesel oil product again after subsequent disposal such as being separated, washing, be dry.Carbochain due to short chain alcohol is short and have the features such as polarity is strong, cost is low, therefore usually selects short chain alcohol to be used in the middle of the preparation of biofuel as the substrate of transesterification reaction at present.In general, having all can catalyzed transesterification compared with the catalyzer of strong acid alkalescence.Ionic liquid is as a kind of novel environmentally friendly liquid acid alkaline catalysts, have the high-density reaction active site of liquid soda acid and the non-volatility of solid acid-base, simultaneously its structure and acid-basicity adjustable, easily and product from, reusable, thermostability is high, is green solvent truly and catalyzer.
Wood of Shinyleaf Yellowhorn is the distinctive excellent woody oil tree species of China, its seed oil length is at 52-66%, and have bear fruit early, output is high, oil yield is high, oil product is good feature, be classified as one of eight large seeds manufacturing biofuel by relevant department of China, there is larger biodiesel raw material potentiality to be exploited.And Wood of Shinyleaf Yellowhorn has cold-resistant, drought-resistant ability and extremely strong adaptive faculty preferably, and wastely can to grow on a large scale on the ground on non-agricultural land, extensively distributing in China " three Norths " area at present, is the economic tree of the northern area of China sand prevention and soil conservation.In order to realize in energy development process the target of clean, environmental protection and energy-saving and emission-reduction, CNPC and the State Administration of Forestry have worked out " CNPC of the State Administration of Forestry one woods oil integrative project Eleventh Five-Year Plan construction plan " jointly, to realize the target jointly promoting the construction of base of biodiesel raw material woods and the integrated industry development of woods oil.In construction plan, Wood of Shinyleaf Yellowhorn planning of trees and shrubs plants 1,800,000 mu, accounts for 30% of biofuel seeds, is mainly distributed in the Inner Mongol, Liaoning, Shaanxi, Gansu, Hei Longjiangwu province.
At present, the research of biofuel is comparatively extensive, comprise the raw material comparative analysis of different sources, preparation method, kinetics, different catalyzer and combustionproperty etc., but be this field of Material synthesis biofuel at Wood of Shinyleaf Yellowhorn, mainly study based on Wood of Shinyleaf Yellowhorn seed kernel oil raw material, the rarely seen report of research being raw material with Wood of Shinyleaf Yellowhorn kind benevolence.Chen Yanqin etc. utilize [C
4mIm] HSO
4ionic liquid is catalyzer, its catalysis Wood of Shinyleaf Yellowhorn seed kernel oil supercritical methanol preparing biodiesel by ester interchange is studied, at 300 DEG C, molar ratio of methanol to oil 42: 1, reaction times 25min, reaction pressure 11MPa, catalyst levels is under the Optimizing Technical of 0.5wt%, and in product, methyl esters yield can reach 92.33%; Li Ji etc. synthesize [BSO
3hMIM] HSO
4-Fe
2(SO
4)
3acidic ion liquid is catalyzer, and the optimal processing parameter of microwave-assisted Wood of Shinyleaf Yellowhorn seed oil conversion biodiesel is: temperature of reaction: 60 DEG C, molar ratio of methanol to oil: 8, catalyst levels: 3%, biofuel transformation efficiency can reach 97.5%; Field bravery waits (CN103571635A) to disclose a kind of method utilizing Wood of Shinyleaf Yellowhorn seed kernel oil to prepare biofuel, with acidic ion liquid [C
4mIm] HSO
4for catalyzer, Wood of Shinyleaf Yellowhorn seed kernel oil is raw material, and methanol mixed is placed in 100mL autoclave, adds [the C of 0.3-0.5wt%
4mIm] HSO
4, reaction pressure 10-15MPa, stirs and is rapidly heated to 280-320 DEG C, constant temperature 20-30min; The open one Wood of Shinyleaf Yellowhorn seed kernel oil of high-new one-tenth etc. (CN101629089) prepares biodiesel process, Wood of Shinyleaf Yellowhorn seed kernel oil is made corresponding biofuel after acidification, catalyst preparing, esterification, filtration, refining, glycerin purification, and general esterification yield can reach more than 95%; It take shinyleaf yellowhorn oil as the method for raw material production biofuel that Wang Jinyan (CN102154066A) discloses a kind of, solid super-strong acid is catalyzer, standard raw materials oil, methyl alcohol and solid super acid catalyst are thoroughly mixed to form mixture in the reactor, standard raw materials oil: methyl alcohol: catalyzer=100: 25-30: 3-5, mixture reacts in reactor, detects methyl ester content and reaches more than 96%; Zhou Quancheng etc. (CN101696373A) disclose a kind of method of preparing biodiesel from Xanthoceras sorbifolia through in-situ transesterification, are 1: 15 ~ 40 insert Wood of Shinyleaf Yellowhorn Renhe low-carbon alcohol in ultrasound reactor and react 6-10 hour productive rate up to 56% by solid-liquid ratio (g/mL); Ding Lijun is with Wood of Shinyleaf Yellowhorn kind benevolence for raw material, and the technique that synthesis one step of the extraction and biofuel that have studied Wood of Shinyleaf Yellowhorn seed kernel oil completes, abstraction reaction temperature is 80 DEG C, and sherwood oil liquid ratio is 5:1, and methanol usage 12%, NaOH consumption is 0.4%.Biofuel average yield is 64.65% under this condition.As can be seen here, to have applied in the research prepared in biofuel and the good ionic-liquid catalyst of effect is BrSnsted acid type ion liquid.
Ionic liquid is as a kind of novel green solvent and catalyzer, have that liquid state range is wide, soluble end is wide, vapour pressure is zero, good stability, acid-basicity is adjustable, product is easily separated and a series of particular advantages such as reusable edible, applied research in organic synthesis is subject to people's attention day by day, has become one of focus of Green Chemistry research.And microwave is as the novel synthesis ancillary technique of one, in organic synthesis, play important role all the time.Microwave can not only make speed of reaction improve several times even thousands of times, and also have simple to operate, by product is few, and productive rate is high, easy purifying and advantages of environment protection, can say that the appearance of microwave brings a qualitative leap to organic synthesis.The advantage of set ionic liquid of the present invention and microwave technology, in microwave reactor, be phase-transfer catalyst with alkali ionic liquid, sodium hydroxide makes alkali, and one pot of change completes Wood of Shinyleaf Yellowhorn seed kernel oil and extracts and the synthesis of biofuel in a solvent.Easy and simple to handle, highly shortened the reaction times, good reaction selectivity, productive rate is also higher, is a kind of environmentally friendly technique.
Summary of the invention
For above-mentioned deficiency, the object of the present invention is to provide the method for a kind of environmental friendliness, reaction times short, the simple catalysis for preparing biodiesel oil of technique
For solving the problems of the technologies described above, technical scheme provided by the invention is such: this use microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence prepares the method for biofuel, comprises the following steps successively:
1) in microwave reactor, with Wood of Shinyleaf Yellowhorn kind benevolence for raw material, with ionic liquid and alkali for phase-transfer catalyst, short chain alcohol is solvent, and at 40 ~ 80 DEG C, reaction 3min ~ 25min mono-pot of change completes Wood of Shinyleaf Yellowhorn seed kernel oil and extracts and the synthesis of biofuel;
2), after reaction terminates, stratification, separates product, and upper strata is biofuel.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, described Wood of Shinyleaf Yellowhorn benevolence be shell decortication Wood of Shinyleaf Yellowhorn benevolence, whole benevolence or pulverize after.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, described ionic liquid is alkali ionic liquid.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, described alkali ionic liquid is alkyl imidazole compounds, and its molecular formula is:
The wherein alkyl of X-to be OH-, R be C2-C4.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, described alkali is NaOH or KOH.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, described short chain alcohol is one or more of methyl alcohol or ethanol or Virahol or propyl carbinol.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, every gram of described Wood of Shinyleaf Yellowhorn benevolence adds 3 ~ 28 milliliters of solvents.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, described alkali ionic liquid and the mol ratio of alkali are 20 ~ 1:20.
Further, the above-mentioned method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, the mass ratio of described catalyst quality and Wood of Shinyleaf Yellowhorn benevolence is 1 ~ 16:100.
Compared with prior art, technical scheme provided by the invention has following technological merit:
1) compared with conventional heating mode, speed of response is fast, greatly reduces the reaction times, energy-efficient;
2) ionic liquid used is a kind of easily preparation, eco-friendly catalyzer, and reacted catalyzer, can reuse after simply dewatering, catalytic activity is constant, is applicable to industrial scale and produces;
3) technique is simple, and the reaction times is short, and catalytic efficiency is high, and catalyst levels is few, and product yield is high, and reaction product only needs extracting and demixing, and underpressure distillation can obtain high-quality product, and productive rate can reach 70% ~ 96%;
4) compared with traditional catalyzer, there is lower corrodibility, reduce discharge alkaline wastewater.
Generally speaking, technical scheme provided by the invention, adopt alkali ionic liquid [Cmmim] OH and alkali compound as catalyzer, simultaneously using Microwave synthesize instrument as assisted reaction device, be applied to biofuel transesterification reaction, there is not been reported for document.Therefore the present invention has technique simply, and speed of response is fast, and the reaction times is short, and energy consumption is low, efficiency of pcr product advantages of higher, belongs to environmentally friendly technique.
Embodiment
Below in conjunction with embodiment, claim of the present invention is described in further detail; but do not form any limitation of the invention; the amendment of anyone limited number of time made within the scope of the claims in the present invention, still within claims of the present invention.
Embodiment 1
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, methanol solution 20ml, ionic liquid [C
2mim] OH 0.5000g (0.0039mol), NaOH 0.0156 (0.00039mol) adds in there-necked flask, be positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 60 C condition, reaction times 8min, after reaction terminates, stratification, separates biofuel phase, and biofuel yield is 85%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Embodiment 2
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, methanol solution 30ml, ionic liquid [C
2mim] OH 0.3500g (0.0027mol), NaOH 0.0080g (0.00019mol) adds in there-necked flask, be positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 65 DEG C of conditions, reaction times 12min, after reaction terminates, stratification, separates biofuel phase, and biofuel yield is 80%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Embodiment 3
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, methanol solution 25ml, ionic liquid [C
2mim] OH 0.2500g (0.0020mol), NaOH 0.0112g (0.00028mol) adds in there-necked flask, be positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 60 C condition, reaction times 25min, after reaction terminates, stratification, separates biofuel phase, and biofuel yield is 96%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Embodiment 4
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, propanol solution 40ml, ionic liquid [C
2mim] OH 0.7000g (0.0054mol), KOH 0.03g (0.00054mol) adds in there-necked flask, is positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 55 DEG C of conditions, reaction times 5min.After reaction terminates, stratification, separates biofuel phase, and biofuel yield is 65%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Embodiment 5
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, aqueous isopropanol 40ml, ionic liquid [C
2mim] OH 0.7000g (0.0054mol), KOH 0.0300g (0.00054mol) adds in there-necked flask, is positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 70 C condition, reaction times 3min.After reaction terminates, stratification, separates biofuel phase, and biofuel yield is 74%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Embodiment 6
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, butanol solution 15ml, ionic liquid [C
2mim] OH 0.6000g (0.0047mol), KOH 0.0329g (0.00059mol) adds in there-necked flask, is positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 80 DEG C of conditions, reaction times 10min.After reaction terminates, stratification, separates biofuel phase, and biofuel yield is 79%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Embodiment 7
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, ethanolic soln 50ml, ionic liquid [C
3mim] OH 0.4000g (0.0026mol), KOH 0.0096g (0.00017mol) adds in there-necked flask, is positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 67 DEG C of conditions, reaction times 8min.After reaction terminates, stratification, separates biofuel phase, and biofuel yield is 84%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Embodiment 8
Take the Wood of Shinyleaf Yellowhorn kind benevolence 5g after drying and crushing respectively, ethanolic soln 65ml, ionic liquid [C
4mim] OH 0.2000g (0.0010mol), NaOH 0.0109g (0.00027mol) adds in there-necked flask, is positioned in the microwave reactor of condensation reflux unit and infrared probe, at radiation power 400W, under temperature 73 DEG C of conditions, reaction times 17min.After reaction terminates, stratification, separates biofuel phase, and biofuel yield is 75%.By lower floor's mixture by rotary evaporation removing residue methyl alcohol, then by cold method and recyclable ionic-liquid catalyst.
Claims (9)
1. prepare a method for biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, it is characterized in that, comprise the following steps successively:
1) in microwave reactor, with Wood of Shinyleaf Yellowhorn kind benevolence for raw material, with ionic liquid and alkali for phase-transfer catalyst, short chain alcohol is solvent, and at 40 ~ 80 DEG C, reaction 3min ~ 25min mono-pot of change completes Wood of Shinyleaf Yellowhorn seed kernel oil and extracts and the synthesis of biofuel;
2), after reaction terminates, stratification, separates product, and upper strata is biofuel.
2. the as claimed in claim 1 method preparing biofuel with microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, is characterized in that, described Wood of Shinyleaf Yellowhorn benevolence is the Wood of Shinyleaf Yellowhorn benevolence of decortication of shelling, after whole benevolence or pulverizing.
3. the method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence as claimed in claim 1, it is characterized in that, described ionic liquid is alkali ionic liquid.
4. the method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence as claimed in claim 3, it is characterized in that, described alkali ionic liquid is alkyl imidazole compounds, and its molecular formula is:
The wherein alkyl of X-to be OH-, R be C2-C4.
5. the method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence as claimed in claim 1, it is characterized in that, described alkali is NaOH or KOH.
6. the as claimed in claim 1 method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence, is characterized in that, described short chain alcohol is one or more of methyl alcohol or ethanol or Virahol or propyl carbinol.
7. microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence according to claim 1 prepares the method for biofuel, it is characterized in that, every gram of described Wood of Shinyleaf Yellowhorn benevolence adds 3 ~ 28 milliliters of solvents.
8. the method preparing biofuel by microwave catalysis Wood of Shinyleaf Yellowhorn kind benevolence as claimed in claim 1, it is characterized in that, described alkali ionic liquid and the mol ratio of alkali are 20 ~ 1:20.
9. the method for claim 1, is characterized in that, the mass ratio of described catalyst quality and Wood of Shinyleaf Yellowhorn benevolence is 1 ~ 16:100.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114686312A (en) * | 2022-04-24 | 2022-07-01 | 内蒙古农业大学 | Method for rapidly preparing biodiesel under low-temperature condition |
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| CN101323791A (en) * | 2008-07-24 | 2008-12-17 | 广东工业大学 | Method for preparing biodesel by microwave catalysis |
| CN101629089A (en) * | 2008-07-14 | 2010-01-20 | 陕西西部绿色能源有限公司 | Method for preparing biodiesel by using seed kernel oil of shinyleaf yellowhorn |
| CN101696373A (en) * | 2009-10-23 | 2010-04-21 | 山东理工大学 | Method for preparing biodiesel from Xanthoceras sorbifolia through in-situ transesterification |
| CN102586005A (en) * | 2012-02-21 | 2012-07-18 | 大连理工大学 | Method for preparing biodiesel by extraction-ester exchange-separation coupling technique |
| CN102703135A (en) * | 2012-05-03 | 2012-10-03 | 北京国力源高分子科技研发中心 | Method for producing biodiesel |
| CN103571635A (en) * | 2012-07-31 | 2014-02-12 | 青岛嘉能节能环保技术有限公司 | Method for preparing biodiesel by shiny-leaved yellowhorn kermel oil |
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2014
- 2014-11-25 CN CN201410685845.9A patent/CN104327888A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101629089A (en) * | 2008-07-14 | 2010-01-20 | 陕西西部绿色能源有限公司 | Method for preparing biodiesel by using seed kernel oil of shinyleaf yellowhorn |
| CN101323791A (en) * | 2008-07-24 | 2008-12-17 | 广东工业大学 | Method for preparing biodesel by microwave catalysis |
| CN101696373A (en) * | 2009-10-23 | 2010-04-21 | 山东理工大学 | Method for preparing biodiesel from Xanthoceras sorbifolia through in-situ transesterification |
| CN102586005A (en) * | 2012-02-21 | 2012-07-18 | 大连理工大学 | Method for preparing biodiesel by extraction-ester exchange-separation coupling technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114686312A (en) * | 2022-04-24 | 2022-07-01 | 内蒙古农业大学 | Method for rapidly preparing biodiesel under low-temperature condition |
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Application publication date: 20150204 |