CN103131541A - Method for preparing biodiesel from Xanthium strumarium - Google Patents
Method for preparing biodiesel from Xanthium strumarium Download PDFInfo
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- CN103131541A CN103131541A CN2013100762119A CN201310076211A CN103131541A CN 103131541 A CN103131541 A CN 103131541A CN 2013100762119 A CN2013100762119 A CN 2013100762119A CN 201310076211 A CN201310076211 A CN 201310076211A CN 103131541 A CN103131541 A CN 103131541A
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- siberian cocklebur
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- xanthium strumarium
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 Xanthium strumarium, which comprises the following steps: pulverizing Xanthium strumarium to 200 meshes or so, repeatedly soaking in petroleum ether until the extracting solution is light yellow, and carrying out vacuum distillation at 60-90 DEG C under the pressure of 0.07-0.08 MPa to obtain Xanthium strumarium oil; reacting methanol and the Xanthium strumarium oil in a mol ratio of (5-12):1 at 55-70 DEG C for 0.5-2 hours, wherein the amount of a catalyst potassium hydroxide is 0.5-1 wt% of the oil; and after the reaction finishes, adding petroleum ether according to the oil/petroleum ether mol ratio of (1-3):1, standing for stratification for 10 minutes, removing the understratum, washing the solution with water to a neutral state, and carrying out vacuum distillation at 60-90 DEG C under the pressure of 0.07-0.08 MPa to obtain the Xanthium strumarium oil biodiesel. The product obtained by the method disclosed by the invention conforms to the National Biodiesel DB100 Standard, and has the advantages of low pollution, wide raw material sources, low cost, simple technique and high economic benefit.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to a kind of method that Siberian cocklebur prepares biofuel.
Background technology
Development along with society, demand to the energy also increases thereupon, particularly petrifaction diesel faces increasingly exhausted situation and the also day by day deterioration of consequent problem of environmental pollution, these severe problems are huge challenges to human survival and development, and the biofuel of developing a kind of sustainable, environmental protection replaces petrifaction diesel to become the focus of mankind nowadays research.
Biofuel (Biodiesel) refers to that the reproducibility diesel oil fuel general reference of the replaced petrifaction diesel made by ester exchange process take the waterplant grease such as oil crops, Wild oil plant and engineering microalgae and animal grease, food garbage wet goods as stock oil is by solid, liquid or the geseous fuel energy of biomass composition or extraction.Can substitute gasoline and the diesel oil produced by oil, be renewable, the environment-friendly type energy.The biofuel overwhelming majority derives from vegetables oil, at present can't to popularize be mainly because technology maturation and high expensive not enough to biofuel, almost account for biofuel total cost 80% left and right, can't be at war with petrifaction diesel, so suitable raw material sources just become one of key that solves current this problem.At present the main raw material sources of biofuel are take the grain oil crops as main, along with showing especially of food problem, countries in the world begin the non-grain and oil material keen interest of having made deposits yields, although non-grain and oil material crop species is various, prepared biofuel can with petrifaction diesel have fairly good fuel performance but seldom.
Siberian cocklebur (Xanthium sibiricum), feverfew, another name: the road number of people, pig ear, a silly mother-in-law, thorn, it is a kind of non-this oilseed plant of army provisions, this plant has that plantation is simple, vitality is indomitable, the source is wide, growth cycle is short, strong stress resistance, reproductivity are strong, cheap, and seed production is high, the seed oil length is high, and its seed oil content is more than 40%, the acid number of seed oil is low, is 1.38 mgKOH/g.Xing Weihe etc. analyze and research to seed oil content and the lipid acid composition of Siberian cocklebur, detect four kinds of lipid acid, unsaturated fatty acid content in seed (91.55%) is far above saturated fatty acid content (8.45%), and unsaturated fatty acids is all the C18 unsaturated fatty acids, this is for utilizing the degeneration-resistant energy-source plant of marginal land germplasm, developing green reproducible biomass energy provides plant germplasm resource, to solve the restriction Biomass Energy Development bottleneck---the insufficient raw material problem is significant.Danger Wen Liang etc. 2008 is to 42 kinds of oilseed plant energy utilization Potential Evaluation of China, think that Siberian cocklebur is one of desirable feedstock of Developing Biodiesel (danger Wen Liang, Jin Mengyang. the energy utilization Potential Evaluation of 42 parts of non-traditional oil tree resources. Chinese oil .2008,33 (5), 73-76.).Zu YuanGang mention in " biofuel " book Siberian cocklebur be a kind of have development potentiality, can be at the non-grain biofuel energy-source plant that is unsuitable for planting on the marginality soil of proportion of crop planting.(Zu YuanGang, Fu Yujie, biofuel. Beijing Science Press, 2006.).
At present, there is not yet report take Siberian cocklebur as raw material for the preparation of the method for Siberian cocklebur biofuel.
Summary of the invention
The object of the invention is to provide a kind of national biofuel DB100 standard that meets, and pollutes method little, that Siberian cocklebur that raw material sources are wide, cost is low, technique is simple, economic benefit is high prepares biofuel.
A kind of Siberian cocklebur of the present invention prepares the method for biofuel, comprises the following steps:
(1) be 5-12:1 with methyl alcohol and Siberian cocklebur oil by molar ratio of methanol to oil, catalyzer potassium hydroxide consumption is the 0.5-1% of oil plant quality, is 55-70 ℃ in temperature, reaction 0.5-2h;
(2) after reaction finishes, add the sherwood oil standing demix, except sub-cloud, water is washed till neutrality with solution, and 60-90 ℃, under 0.07-0.08MPa, underpressure distillation namely gets the Siberian cocklebur oil biodiesel.
Above-mentioned a kind of Siberian cocklebur prepares the method for biofuel, and wherein: Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 60-90 ℃, 0.07-0.08MPa carries out underpressure distillation and obtains Siberian cocklebur oil.
Above-mentioned a kind of Siberian cocklebur prepares the method for biofuel, and wherein: standing demix adds sherwood oil, standing 10min according to oil with sherwood oil mol ratio 1-3:1.
The present invention compared with prior art has obvious beneficial effect, as can be known from the above technical solutions: take Siberian cocklebur oil and methyl alcohol as raw material under catalyzer potassium hydroxide existence condition, pass through catalyzed reaction and make biofuel.Through it is carried out the fuel performance analysis, its performance meets national standard.In fuel performance, density, flash-point, sulphur content, sulfated ash, water-content, mechanical impurity, copper corrosion, acid number, iodine number, 90% recovered temperature, free glycerol content and total glycerol content all meet national biofuel DB100 standard; Cetane value is 48.8, although a little less than EN14214-08 and GB/T20828-07 defined more than or equal to 49 standard, met ASTM D6751-10 defined more than or equal to 47 standard; Wherein it is worth noting sulfated ash in its fuel performance and sulphur content be far smaller than GB2433-2001 and SH/T0689-2000 defined less than or equal to 0.02 with less than or equal to 0.005.So just make this biofuel be emitted on airborne sulfurous gas and greatly reduce, thereby reduced pollution to environment.Because the acid number of Siberian cocklebur oil is low, so do not need pre-esterification with Siberian cocklebur oil preparation biofuel the time, can directly carry out esterification, thus production cost and the production cycle of having reduced biofuel, reduce the discharging of the three wastes, established certain basis for breaking through the Biodiesel bottleneck.Simultaneously with non-grain and oil material crop---Siberian cocklebur is the new non-grain and oil tannin plant of the Developing of Biodiesel for the preparation of the raw material of biofuel.Land utilization ratio can be improved, rocky desertification problem can be solved to a certain extent.
Embodiment
Embodiment 1
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 80 ℃, 0.08MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 5g, methyl alcohol 1.87g in the round-bottomed flask of 50mL, catalyzer is that KOH0.04g stirs 1h in 65 ℃, reaction adds the 30mL sherwood oil after finishing, standing 10min, system layering discards lower floor, and the washing upper solution is to neutral, at 80 ℃, 0.08MPa carries out the underpressure distillation filtration and namely gets biofuel.
Measure making biofuel, its fatty acid methyl ester is 98.3%, and other the results are shown in following table:
| Siberian cocklebur biofuel test item | Test basis | Detected result |
| Moisture content, % (massfraction) | SH/ T 0246- 1992(2004) | 0.049 |
| Sulfate ash content, % (massfraction) | GB/ T 2433- 2001 | 0.004 |
| 20 ℃ of (kg/cm of density 3) | GB/ T 1884-2000 | 874.7 |
| Kinematic viscosity (40 ℃) mm 2/s | GB/T 265-1988 | 3.723 |
| Sulphur content, % (massfraction) | SH/ T 0689- 2000 | 0.0003 |
| Cetane value | GB/T 386- 2010 | 48.8 |
| Copper corrosion (50 ℃, 3 h), level | GB/ T 5096- 1985(1991) | 1a |
| Acid number (mg KOH/g) | GB/T 264- 1983(1991) | 0.07 |
| Free state glycerol content % (massfraction) | ASTM D 6584- 10ae1 | 0.0008 |
| Total glycerol content % (massfraction) | ASTM D 6584- 10ae1 | 0.135 |
| Oxidation stability (110 ℃, h) | EN 14112- 2003 | 1.2 |
| Cold filter clogging temperature (CFPP, ℃) | SH/ T 0248- 2006 | -3 |
| Mechanical impurity, % (massfraction) | GB/T 511- 2010 | Do not detect |
| 90% recovered temperature, ℃ | ?GB/ T 6536- 2010 | 337.5 |
Embodiment 2:
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 90 ℃, 0.07MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 5g, ethanol 2.68 g in the round-bottomed flask of 50mL, catalyzer is that KOH0.04g stirs 1h in 65 ℃, reaction adds 30 mL sherwood oils after finishing, standing 10min, system layering discards lower floor, and the washing upper solution is to neutral, at 90 ℃, 0.07MPa carries out the underpressure distillation filtration and namely gets biofuel.Measure making product, its fatty-acid ethyl ester is 97.7%.
Embodiment 3:
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 80 ℃, 0.075MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 200g, methyl alcohol 74.8g in the round-bottomed flask of 500mL, catalyzer is that KOH1.6g stirs 1h in 65 ℃, reaction adds the 100mL sherwood oil after finishing, standing 10min, system layering discards lower floor, and the washing upper solution is to neutral, at 80 ℃, 0.075MPa carries out the underpressure distillation filtration and namely gets biofuel.Measure making product, its fatty acid methyl ester is 96.9%.
Embodiment 4:
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 60 ℃, 0.08MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 200g, ethanol 107.2g in the round-bottomed flask of 500 mL, catalyzer is that KOH 1.6 g stir 1h in 65 ℃, reaction adds the 100mL sherwood oil after finishing, standing 10min, system layering discards lower floor, and the washing upper solution is to neutral, at 60 ℃, 0.08MPa carries out the underpressure distillation filtration and namely gets biofuel.Measure making product, its fatty-acid ethyl ester is 97.1%.
Embodiment 5:
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 80 ℃, 0.07MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 5g, methyl alcohol 0.935g in the round-bottomed flask of 50mL, catalyzer is that KOH0.025g stirs 2h in 70 ℃, reaction adds 20 mL sherwood oils after finishing, standing 10min, system layering discards lower floor, and the washing upper solution is to neutral, at 80 ℃, 0.07MPa carries out the underpressure distillation filtration and namely gets biofuel.Measure making product, its fatty acid methyl ester is 95.8%.
Embodiment 6:
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 80 ℃, 0.073MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 5g, methyl alcohol 1.496g in the round-bottomed flask of 50 mL, catalyzer is that KOH0.05g stirs 0.5h in 70 ℃, reaction adds the 40mL sherwood oil after finishing, standing 10min, system layering, discard lower floor, the washing upper solution is to neutral, and underpressure distillation is filtered and namely got biofuel.Measure making product, its fatty acid methyl ester is 97.6%.
Embodiment 7:
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 80 ℃, 0.078MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 5g, methyl alcohol 2.244g in the round-bottomed flask of 50 mL, to be KOH0.05g stir 2h in 55 ℃ with catalyzer, and reaction adds the 40mL sherwood oil after finishing, standing 10min, system layering discards lower floor, the washing upper solution is to neutral, and underpressure distillation is filtered and namely got biofuel.Measure making product, its fatty acid methyl ester is 97.1%.
Embodiment 8:
A kind of Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) Siberian cocklebur is crushed to about 200 orders, repeatedly soaks until extracting solution is faint yellow by sherwood oil, at 80 ℃, 0.08MPa carries out underpressure distillation and obtains Siberian cocklebur oil;
(2) drop into Siberian cocklebur oil 5g, ethanol 3.216g in the round-bottomed flask of 50 mL, catalyzer is that KOH 0.05g stirs 0.5h in 70 ℃, reaction adds 30 mL sherwood oils after finishing, standing 10min, system layering, discard lower floor, the washing upper solution is to neutral, and underpressure distillation is filtered and namely got biofuel.Measure making product, its fatty-acid ethyl ester is 98.0%.
The above, it is only preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment does according to technical spirit of the present invention.
Claims (3)
1. a Siberian cocklebur prepares the method for biofuel, comprises the following steps:
(1) be 5-12:1 with methyl alcohol and Siberian cocklebur oil by molar ratio of methanol to oil, catalyzer potassium hydroxide consumption is the 0.5-1% of oil plant quality, is 55-70 ℃ in temperature, reaction 0.5-2 h;
(2) after reaction finishes, add the sherwood oil standing demix, except sub-cloud, water is washed till neutrality with solution, and 60-90 ℃, under 0.07-0.08MPa, underpressure distillation namely gets the Siberian cocklebur oil biodiesel.
2. a kind of Siberian cocklebur as claimed in claim 1 prepares the method for biofuel, wherein: Siberian cocklebur is crushed to about 200 orders, repeatedly soak until extracting solution is faint yellow by sherwood oil, at 60-90 ℃, 0.07-0.08MPa carries out underpressure distillation and obtains Siberian cocklebur oil.
3. a kind of Siberian cocklebur as claimed in claim 1 or 2 prepares the method for biofuel, and wherein: standing demix adds sherwood oil, standing 10min according to oil with sherwood oil mol ratio 1-3:1.
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Cited By (2)
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| CN103436303A (en) * | 2013-07-23 | 2013-12-11 | 济南开发区星火科学技术研究院 | B5 biodiesel |
| CN104830379A (en) * | 2015-04-14 | 2015-08-12 | 贵州大学 | Firmiana platanifolia seed biodiesel and preparation method thereof |
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| CN103436303A (en) * | 2013-07-23 | 2013-12-11 | 济南开发区星火科学技术研究院 | B5 biodiesel |
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| CN104830379A (en) * | 2015-04-14 | 2015-08-12 | 贵州大学 | Firmiana platanifolia seed biodiesel and preparation method thereof |
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Application publication date: 20130605 |