CN1935947A - Method for preparing biodiesel by ultrasonic and microwave combination - Google Patents
Method for preparing biodiesel by ultrasonic and microwave combination Download PDFInfo
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- CN1935947A CN1935947A CNA2006101047890A CN200610104789A CN1935947A CN 1935947 A CN1935947 A CN 1935947A CN A2006101047890 A CNA2006101047890 A CN A2006101047890A CN 200610104789 A CN200610104789 A CN 200610104789A CN 1935947 A CN1935947 A CN 1935947A
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
The invention relates to the method used ultrasonic wave and micro wave to prepare biological diesel oil. It includes the following steps: mixing the raw oil processed by depickling and dehydrating, methanol, and solid Lewis base catalyst; sending the mixture into ultrasonic wave emulsification reactor to process emulsification dispersion; then sending the mixture into micro wave reactor to process ester exchange; filtering the mixed liquor; processing centrifugal separation to divide the biological diesel oil from the glycerol; processing neutralizing, washing by water, drying, continuous vacuum distillation to gain high qualitative biological diesel oil. The invention is the method which uses animal and vegetable oils as raw material, adopts ultrasonic wave intensifying emulsifying dispersing technique and micro wave auxiliary energy providing to fast fit for commercialization product, reduce product cost and environment pollution.
Description
Technical field:
The present invention relates to a kind ofly utilize ultrasonic wave and microwave coupling to prepare method of bio-diesel oil, can increase substantially production efficiency, reduce production costs, particularly waste oil or their mixture with natural plant grease, animal tallow, recovery is the preparation method of bio-diesel oil that raw material production can substitute the petroleum diesel product.
Background technology
In recent years, along with reducing day by day and human quick increase to demand for energy of fossil energy, the alternative energy of development of new is all being accelerated in countries in the world.Bioenergy comprises fuel alcohol, biological hydrogen production and biofuel, has obtained people's attention with its good recyclability.Especially biofuel, its combustionproperty be not second to petroleum diesel, and can be directly used in diesel engine etc., is considered to the best substitute of petroleum diesel.Biofuel has the following advantages: nontoxic, biodegradable, cetane value is high, sulfide, CO (carbon monoxide converter) emission are few, and also the carbon of its discharging compares with petroleum diesel from atmosphere, can reduce emission amount of carbon dioxide.Therefore, biofuel is a kind of renewable environment-friendly fuel energy.
The suitability for industrialized production of biofuel and be applied in the history that more than ten years have abroad been arranged, production technology is comparative maturity, and industrial scale is also in continuous expansion.The technology input and the exploitation of biofuel have all successively been carried out in order to tackle energy dilemma in countries in the world, have formulated to help the policy that the biofuel industry develops in a healthy way, and the turnout of whole world biofuel is increased sharply.American energy policy method determines that the occupation rate of U.S.'s non-petroleum fuel in 2010 will bring up to 30%, the target that European Union promotes biofuel is: the biofuel share of market reached 5.75% in 2010, the year two thousand twenty reaches 20%, and this brings vast potential for future development can for undoubtedly the biofuel industry.At present, other country has also built up the biofuel factory of oneself in the world.
China's production of biodiesel still is in the exploitation starting stage, now only there are Fujian brilliance, the ancient China fir in Sichuan and Hainan just to build up production capacity respectively and surpass 10 with three companies, 000 ton/year small-sized biofuel factory, but since technology and cost aspect also fail to be promoted rapidly.Domestic patent application about biodiesel manufacture at present exists that long reaction time, reaction conversion ratio are not high, energy consumption is high, the high deficiency of production cost, can't be extensive use of in commercially producing.
Summary of the invention
The objective of the invention is to deficiency at the prior art scheme, a kind of method that adopts intensified by ultrasonic wave emulsification dispersion technology and microwave-assisted that energy is provided is provided, its being suitable for is rapidly and efficiently commercially produced, can significantly be reduced production costs, and what can alleviate environmental pollution simultaneously is the feedstock production method of bio-diesel oil with the animal-plant oil.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of ultrasonic wave and microwave coupling prepare method of bio-diesel oil, its special character is: the stock oil after depickling, processed enters the ultrasonic emulsification reactor with the mixture of methyl alcohol and solid Lewis alkaline catalysts to carry out emulsification and disperses, keeping the mol ratio of methyl alcohol and stock oil is 4: 1～20: 1, the catalyst quality percentage composition is 0.5%～5% of a grease weight, the emulsion reaction temperature is controlled at 25～50 ℃, emulsification times is 1～5min, and ultrasonic frequency is 30kHz～300kHz; After emulsion reaction finishes, mixture is sent into microwave reactor carry out transesterification reaction, control reaction temperature is 40～75 ℃, reflux 2～10min, after reaction finishes, mixed solution is filtered, liquid phase reclaims excessive methyl alcohol through distillation, adopt the method for centrifugation then, make crude product biofuel and glycerine separately; The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained high-quality biofuel.
Above-mentioned stock oil is the waste oil of crude vegetal, animal tallow, recovery, or above-mentioned several mixture.
Above-mentioned stock oil is through removing free fatty acids and processed, and acid number is less than 2mgKOHg
-1, water content is reduced to below 0.05%.
Above-mentioned solid Lewis alkaline catalysts is: lithium methoxide, sodium methylate, potassium methylate, the methyl alcohol rubidium, lithium ethoxide, sodium ethylate, potassium ethylate, the ethanol rubidium, magnesium methylate, aluminum methylate, magnesium ethylate, aluminum ethylate, lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, yellow soda ash, salt of wormwood, Lithium Oxide 98min, sodium oxide, potassium oxide, rubidium oxide, beryllium oxide, magnesium oxide, calcium oxide, strontium oxide, barium oxide, Scium trioxide, titanium oxide, titanium sesquioxide, four oxidation Tritanium/Trititaniums, the oxidation alum, three oxidations, two alum, four oxidations, three alum, Vanadium Pentoxide, chromic oxide, chromium sesquioxide, chromium trioxide, manganese oxide, Manganse Dioxide, ferric oxide, ferric oxide, Z 250, cobalt oxide, cobalt sesquioxide, nickel oxide, nickel sesquioxide, Red copper oxide, cupric oxide, zinc oxide, iridium oxide, zirconium sesquioxide, zirconium dioxide, Niobium Pentxoxide, molybdic oxide, three oxidations, two technetiums, three oxidations, two rubidiums, the titanium dioxide rubidium, four rubidium oxides, rhodium sesquioxide, palladous oxide, silver suboxide, titanium dioxide silver, Cadmium oxide, lanthanum sesquioxide, hafnium oxide, tantalum pentoxide, Tungsten oxide 99.999, rhenium oxide, osmium oxide, iridium oxide, platinum oxide, gold trioxide, the basic catalyst that red precipitate and lanthanide oxide and actinide elements oxide compound or other Lewis base constitute.
Above-mentioned transesterification reaction with the mixed solution filtered while hot, recycles after the activated processing of the solid-phase catalyst that obtains after finishing.
Above-mentioned liquid phase of separating after filtration behind the solid-phase catalyst is handled through distillation, reclaims excessive methyl alcohol, and it is recycled.
Liquid phase behind the above-mentioned recovery methyl alcohol, the method for employing centrifugation makes crude product biofuel and glycerine separately, and the crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained high-quality biofuel.
The present invention is with respect to prior art, and its production technique novelty through fully emulsified dispersive mixture, can prepare high-quality biofuel product, and speed of response is fast, energy consumption is low, transformation efficiency is high, production cost is low, is suitable for commercially producing.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
The present invention prepares method of bio-diesel oil, comprises the steps:
Stock oil makes acid number less than 2mgKOHg through depickling and processed
-1, water content is reduced to below 0.05%; Depickling, stock oil after the dehydration etc. enters the ultrasonic emulsification reactor with the mixture of methyl alcohol and solid base catalyst to carry out emulsification and disperses, keeping the mol ratio of methyl alcohol and stock oil is 4: 1～20: 1, the catalyst quality percentage composition is for being 0.5%～5% of grease weight, the emulsion reaction temperature is controlled at 25～50 ℃, ultrasonic frequency is 30kHz～300kHz, emulsification times is 1～5min, after emulsion reaction finishes, make mixture enter microwave reactor and carry out transesterification reaction, control reaction temperature is 40～75 ℃, reflux 2～10min with the mixed solution filtered while hot, recycles after the activated processing of the solid catalyst that obtains after reaction finishes.Liquid reclaims excessive methyl alcohol through distillation.Adopt the method for centrifugation then, make crude product biofuel and glycerine separately.The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained highly purified biofuel.
Below in conjunction with specific embodiments, the present invention is described further:
Embodiment 1
Add the soya-bean oil 1mol, the methyl alcohol 6mol that handle through depickling, dehydration etc. in 1.5 liters of flasks, catalyst oxidation calcium 2% is put into ultrasound reactor emulsification 2min under 35 ℃, 50kHz.After emulsion reaction finishes, mixture changed over to carry out transesterification reaction in the microwave reactor, control reaction temperature is 45 ℃, and reflux 3min with the mixed solution filtered while hot, recycles after the activated processing of the solid catalyst that obtains after reaction finishes.Liquid reclaims excessive methyl alcohol through distillation.
Adopt the method for centrifugation then, make crude product biofuel and glycerine separately.The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained highly purified biofuel.Detect through chromatogram, the fatty acid methyl ester of biofuel is 98.3%.
Embodiment 2
Add the rapeseed oil 1mol, the methyl alcohol 8mol that handle through depickling, dehydration etc. in 1.5 liters of flasks, catalyst oxidation barium 3% is put into ultrasound reactor emulsification 3min under 40 ℃, 100kHz.After emulsion reaction finishes, mixture changed over to carry out transesterification reaction in the microwave reactor, control reaction temperature is 65 ℃, and reflux 7min with the mixed solution filtered while hot, recycles after the activated processing of the solid catalyst that obtains after reaction finishes.Liquid reclaims excessive methyl alcohol through distillation.
Adopt the method for centrifugation then, make crude product biofuel and glycerine separately.The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained highly purified biofuel.Detect through chromatogram, the fatty acid methyl ester of biofuel is 97.3%.
Embodiment 3
Add the recovery waste oil 1mol, the methyl alcohol 12mol that handle through depickling, dehydration etc. in 1.5 liters of flasks, catalyst oxidation zinc 2.5% is put into ultrasound reactor emulsification 2min under 45 ℃, 150kHz.After emulsion reaction finishes, mixture changed over to carry out transesterification reaction in the microwave reactor, control reaction temperature is 65 ℃, and reflux 8min with the mixed solution filtered while hot, recycles after the activated processing of the solid catalyst that obtains after reaction finishes.Liquid reclaims excessive methyl alcohol through distillation.
Adopt the method for centrifugation then, make crude product biofuel and glycerine separately.The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained highly purified biofuel.Detect through chromatogram, the fatty acid methyl ester of biofuel is 95.3%.
Embodiment 4
Add the shea butter 1mol, the methyl alcohol 16mol that handle through depickling, dehydration etc. in 1.5 liters of flasks, catalyst oxidation zirconium 5% is put into ultrasound reactor emulsification 5min under 50 ℃, 250kHz.After emulsion reaction finishes, mixture changed over to carry out transesterification reaction in the microwave reactor, control reaction temperature is 75 ℃, and reflux 8min with the mixed solution filtered while hot, recycles after the activated processing of the solid catalyst that obtains after reaction finishes.Liquid reclaims excessive methyl alcohol through distillation.
Adopt the method for centrifugation then, make crude product biofuel and glycerine separately.The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained highly purified biofuel.Detect through chromatogram, the fatty acid methyl ester of biofuel is 96.3%.
Embodiment 5
Add the plam oil 1mol, the methyl alcohol 6mol that handle through depickling, dehydration etc. in 1.5 liters of flasks, catalyst oxidation strontium 4% is put into ultrasound reactor emulsification 5min under 40 ℃, 150kHz.After emulsion reaction finishes, mixture changed over to carry out transesterification reaction in the microwave reactor, control reaction temperature is 75 ℃, and reflux 6min with the mixed solution filtered while hot, recycles after the activated processing of the solid catalyst that obtains after reaction finishes.Liquid reclaims excessive methyl alcohol through distillation.
Adopt the method for centrifugation then, make crude product biofuel and glycerine separately.The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained highly purified biofuel.Detect through chromatogram, the fatty acid methyl ester of biofuel is 97.3%.
Claims (7)
1, a kind of ultrasonic wave and microwave coupling prepare method of bio-diesel oil, it is characterized in that: the stock oil after depickling, processed enters the ultrasonic emulsification reactor with the mixture of methyl alcohol and solid Lewis alkaline catalysts to carry out emulsification and disperses, keeping the mol ratio of methyl alcohol and stock oil is 4: 1～20: 1, the catalyst quality percentage composition is 0.5%～5% of a grease weight, the emulsion reaction temperature is controlled at 25～50 ℃, emulsification times is 1～5min, and ultrasonic frequency is 30kHz～300kHz; After emulsion reaction finishes, mixture is sent into microwave reactor carry out transesterification reaction, control reaction temperature is 40～75 ℃, reflux 2～10min, after reaction finishes, mixed solution is filtered, liquid phase reclaims excessive methyl alcohol through distillation, adopt the method for centrifugation then, make crude product biofuel and glycerine separately; The crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, is obtained high-quality biofuel.
2, ultrasonic wave according to claim 1 and microwave coupling prepare method of bio-diesel oil, it is characterized in that: described stock oil is the waste oil of crude vegetal, animal tallow, recovery, or above-mentioned several mixture.
3, ultrasonic wave according to claim 1 and microwave coupling prepare method of bio-diesel oil, it is characterized in that: described stock oil is through removing free fatty acids and processed, and acid number is less than 2mgKOHg
-1, water content is reduced to below 0.05%.
4, ultrasonic wave according to claim 1 and microwave coupling prepare method of bio-diesel oil, it is characterized in that: described solid Lewis alkaline catalysts is: lithium methoxide, sodium methylate, potassium methylate, the methyl alcohol rubidium, lithium ethoxide, sodium ethylate, potassium ethylate, the ethanol rubidium, magnesium methylate, aluminum methylate, magnesium ethylate, aluminum ethylate, lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, yellow soda ash, salt of wormwood, Lithium Oxide 98min, sodium oxide, potassium oxide, rubidium oxide, beryllium oxide, magnesium oxide, calcium oxide, strontium oxide, barium oxide, Scium trioxide, titanium oxide, titanium sesquioxide, four oxidation Tritanium/Trititaniums, the oxidation alum, three oxidations, two alum, four oxidations, three alum, Vanadium Pentoxide, chromic oxide, chromium sesquioxide, chromium trioxide, manganese oxide, Manganse Dioxide, ferric oxide, ferric oxide, Z 250, cobalt oxide, cobalt sesquioxide, nickel oxide, nickel sesquioxide, Red copper oxide, cupric oxide, zinc oxide, iridium oxide, zirconium sesquioxide, zirconium dioxide, Niobium Pentxoxide, molybdic oxide, three oxidations, two technetiums, three oxidations, two rubidiums, the titanium dioxide rubidium, four rubidium oxides, rhodium sesquioxide, palladous oxide, silver suboxide, titanium dioxide silver, Cadmium oxide, lanthanum sesquioxide, hafnium oxide, tantalum pentoxide, Tungsten oxide 99.999, rhenium oxide, osmium oxide, iridium oxide, platinum oxide, gold trioxide, the basic catalyst that red precipitate and lanthanide oxide and actinide elements oxide compound or other Lewis base constitute.
5, ultrasonic wave according to claim 1 and microwave coupling prepare method of bio-diesel oil, it is characterized in that: described transesterification reaction with the mixed solution filtered while hot, recycles after the activated processing of the solid-phase catalyst that obtains after finishing.
6, ultrasonic wave according to claim 1 and microwave coupling prepare method of bio-diesel oil, it is characterized in that: described liquid phase of separating after filtration behind the solid-phase catalyst is handled through distillation, reclaims excessive methyl alcohol, and it is recycled.
7, ultrasonic wave according to claim 1 and microwave coupling prepare method of bio-diesel oil, it is characterized in that: the liquid phase behind the described recovery methyl alcohol, adopt the method for centrifugation, make crude product biofuel and glycerine separately, to the crude product biofuel through neutralization, washing, drying, in 220～250 ℃ of continuous underpressure distillation, obtain high-quality biofuel.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010130006A1 (en) * | 2009-05-15 | 2010-11-18 | Ausbiodiesel Pty Ltd | Method and apparatus for the making of a fuel |
| CN101058097B (en) * | 2007-05-31 | 2011-04-06 | 张虎明 | Resource using method for food and drink garbage |
| CN101307246B (en) * | 2008-06-26 | 2011-05-04 | 济南大学 | Process for co-preparing biodiesel by ultrasonic and microwave |
| CN101381613B (en) * | 2008-09-26 | 2011-11-02 | 中国科学院西双版纳热带植物园 | Method for continuously producing biodiesel using jatropha curcas oil as raw material and apparatus thereof |
| US8052848B2 (en) * | 2007-06-26 | 2011-11-08 | The Penn State Research Foundation | Ultrasonic and microwave methods for enhancing the rate of a chemical reaction and apparatus for such methods |
| CN102676308A (en) * | 2012-06-04 | 2012-09-19 | 昆明理工大学 | Method for preparing biodiesel fuel with kitchen waste |
| TWI383043B (en) * | 2008-09-12 | 2013-01-21 | ||
| CN103122278A (en) * | 2013-03-07 | 2013-05-29 | 中国石油大学(华东) | Preparation method of biodiesel |
| WO2015122428A1 (en) * | 2014-02-14 | 2015-08-20 | マイクロ波化学株式会社 | Method for producing organic compound, and method for producing ester |
| CN106520383A (en) * | 2016-11-22 | 2017-03-22 | 上海应用技术大学 | Ultrasonic-assisted process optimization method for preparing biodiesel |
| WO2018115296A1 (en) | 2016-12-22 | 2018-06-28 | Antofenol | Preparation of a dry biomass extract rich in polyphenols |
| CN108795511A (en) * | 2018-06-28 | 2018-11-13 | 鹿寨知航科技信息服务有限公司 | A kind of composite biodiesel and its efficient lactate synthesis method |
| CN108841422A (en) * | 2018-06-28 | 2018-11-20 | 鹿寨知航科技信息服务有限公司 | A kind of hybrid diesel fuel and preparation method thereof |
| CN108865447A (en) * | 2018-06-29 | 2018-11-23 | 鹿寨知航科技信息服务有限公司 | The method of catalysis of metalloporphyrin gutter oil biodiesel synthesis |
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2006
- 2006-10-23 CN CNA2006101047890A patent/CN1935947A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058097B (en) * | 2007-05-31 | 2011-04-06 | 张虎明 | Resource using method for food and drink garbage |
| US8052848B2 (en) * | 2007-06-26 | 2011-11-08 | The Penn State Research Foundation | Ultrasonic and microwave methods for enhancing the rate of a chemical reaction and apparatus for such methods |
| CN101307246B (en) * | 2008-06-26 | 2011-05-04 | 济南大学 | Process for co-preparing biodiesel by ultrasonic and microwave |
| TWI383043B (en) * | 2008-09-12 | 2013-01-21 | ||
| CN101381613B (en) * | 2008-09-26 | 2011-11-02 | 中国科学院西双版纳热带植物园 | Method for continuously producing biodiesel using jatropha curcas oil as raw material and apparatus thereof |
| WO2010130006A1 (en) * | 2009-05-15 | 2010-11-18 | Ausbiodiesel Pty Ltd | Method and apparatus for the making of a fuel |
| US9428703B2 (en) | 2009-05-15 | 2016-08-30 | Ausbiodiesel Pty Ltd | Method and apparatus for the making of a fuel |
| CN102676308B (en) * | 2012-06-04 | 2014-04-02 | 昆明理工大学 | Method for preparing biodiesel fuel with kitchen waste |
| CN102676308A (en) * | 2012-06-04 | 2012-09-19 | 昆明理工大学 | Method for preparing biodiesel fuel with kitchen waste |
| CN103122278A (en) * | 2013-03-07 | 2013-05-29 | 中国石油大学(华东) | Preparation method of biodiesel |
| WO2015122428A1 (en) * | 2014-02-14 | 2015-08-20 | マイクロ波化学株式会社 | Method for producing organic compound, and method for producing ester |
| CN106520383A (en) * | 2016-11-22 | 2017-03-22 | 上海应用技术大学 | Ultrasonic-assisted process optimization method for preparing biodiesel |
| WO2018115296A1 (en) | 2016-12-22 | 2018-06-28 | Antofenol | Preparation of a dry biomass extract rich in polyphenols |
| US11517015B2 (en) | 2016-12-22 | 2022-12-06 | Antofenol | Preparation of a dry biomass extract rich in polyphenols |
| CN108795511A (en) * | 2018-06-28 | 2018-11-13 | 鹿寨知航科技信息服务有限公司 | A kind of composite biodiesel and its efficient lactate synthesis method |
| CN108841422A (en) * | 2018-06-28 | 2018-11-20 | 鹿寨知航科技信息服务有限公司 | A kind of hybrid diesel fuel and preparation method thereof |
| CN108865447A (en) * | 2018-06-29 | 2018-11-23 | 鹿寨知航科技信息服务有限公司 | The method of catalysis of metalloporphyrin gutter oil biodiesel synthesis |
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