CN1215147C - Biological diesel oil and method for preparing same - Google Patents
Biological diesel oil and method for preparing same Download PDFInfo
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- CN1215147C CN1215147C CNB2004100344871A CN200410034487A CN1215147C CN 1215147 C CN1215147 C CN 1215147C CN B2004100344871 A CNB2004100344871 A CN B2004100344871A CN 200410034487 A CN200410034487 A CN 200410034487A CN 1215147 C CN1215147 C CN 1215147C
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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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- 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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- 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 present invention relates to biological diesel oil and method for preparing same. The technical program is the biological diesel oil contains Jatropha crucas L. seed oil; in said Jatropha crucas L. seed oil, stearic acid content is not more than 0.4 (wt) percents. The method for preparing biological diesel oil comprises production art of the biological diesel oil and refining, improving art of the biological diesel oil; said refining, improving art comprises steps of: a, hydrating and degumming; b, alkali refining and acid removing; c, dehydrating; d intermittent deodorizing; e, emulsification and esterification. The invention has good effect of recucing stearic acid content in the Jatropha crucas L. seed oil, eliminating aromatic compound such as phthalic acid etc., improving burning ability of the biological diesel oil, reducing carbon accumulation in motor cylinder, improving power ability of motor, and discharging index. And the invention has simple producing process and low producing cost.
Description
Technical field
The present invention relates to biofuel, particularly the biofuel that adopts Cortex jatrophae (Jatropha curcas L.) seed to refine.
Background technology
Biofuel more and more is subjected to people's favor with its unique feature of environmental protection and reproducibility.The biofuel of utilizing various oil plants or animal tallow to produce, what have enters the commercial applications stage.General biofuel, its economy can't be compared with petrifaction diesel.
Cortex jatrophae (Jatropha curcas L.) is Euphorbiaceae (Euphorbia L.) Cortex jatrophae platymiscium, machaka or a dungarunga.It is a kind of perennial woody oilseed plant.Jatropha seed oil content is very high, and oil yield is especially up to 40%.Cortex jatrophae plantation does not account for the arable land easily, the surviving rate height, and planting cost is low, and is distributed more widely in China, is particularly suitable for the dry-hot valley area plantation that economize in the Sichuan, Guizhou, Yunnan, Guangxi etc. in China southwest.In China's western development Cortex jatrophae industry, has positive effect for the geographic ecological construction of dry-hot valley, soil conservation.Simultaneously can promote the west area structural readjustment of rural industry, quicken development of rural economy.To regional aid-the-poor project, to increasing the poverty-stricken area farmers' income, increased taxes in countries and regions, national Oil Safety strategy etc. is had great significance.The development of Cortex jatrophae industry will bring huge economic benefit, social benefit and ecological benefits.The barbadosnut seed oil that squeezes with barbadosnut seed, as the substitute of petrifaction diesel, its economy near in addition be better than petrifaction diesel.
Adopt Cortex jatrophae (Jatropha curcas L.) the seed oil of vegetable oil production explained hereafter, its component is (wt%): oleic acid 37～63, linolic acid 19～40, palmitinic acid 12～17, stearic acid 5～7.The barbadosnut seed oil of above-mentioned component because stearic acid content is higher, can not fully burn in engine, and forms the carbide of high level, and carbide forms carbon distribution in engine oil nozzle and cylinder, cause spray nozzle clogging, has reduced the performance of engine.The CO of exhaust emissions is higher simultaneously, pollutes bigger.On the other hand, the biofuel that stearic acid content is high, its viscosity is bigger than normal, has also influenced the spray burning performance of biofuel.The barbadosnut seed oil of above-mentioned component when engine moves, particularly under the situation of on-load, the fixed phenomenon of the roughness of engine often occurs, and is also relevant greatly with its viscosity.So the barbadosnut seed oil of above-mentioned component generally only is suitable for more coarse and more crude engine such as farm machinery and makes fuel oil.Moreover the barbadosnut seed oil that has also contains 17% the phthalic acid of having an appointment, because the carinogenicity of its burning back tail gas also is a kind of pollutent of danger.
The preparation technology of existing biofuel generally is to add methyl alcohol or ethanol in animal and vegetable oil, under high temperature (230～250 ℃) and catalyzer condition, carries out so-called lactide reaction.This technology is the equipment complexity not only, and investment is big, and because temperature is higher, has bigger potential safety hazard in the operation.Prepare the domestic beyond example still of biofuel with the barbadosnut seed oil esterification.
Summary of the invention
Technical problem to be solved by this invention is exactly the shortcoming at above-mentioned prior art, provides a kind of and handles through refining, modification, and stearic acid content is low, and the environment-friendly type biodiesel of aromatic free compound.
The present invention solves its technical problem, and the technical scheme of employing is that biofuel contains Cortex jatrophae (Jatropha curcas L.) seed oil; Stearic acid content in the described barbadosnut seed oil≤0.4 (wt) %.
The preparation method of biofuel comprises barbadosnut seed oil production and barbadosnut seed oil refining, modified technique; It is characterized in that: described refining, modified technique comprise emulsification or esterification technique.
The invention has the beneficial effects as follows, reduced the stearic acid content in the barbadosnut seed oil, eliminated carcinogenic aromatic hydroxy compounds such as phthalic acid, improved the combustionproperty of biofuel, reduce the engine cylinder carbon distribution, improved engine power performance, improved discharge index.And it is simple to have production technique, the characteristics that production cost is low.
Description of drawings
The crazy tree olein refining of figure 1 Shi Ma, modified technique schema;
Fig. 2 is the hydration degum process flow sheet;
Fig. 3 is the alkali-refining deacidification process flow sheet;
Fig. 4 is the batch deodorization process flow sheet;
Fig. 5 is the emulsifying process schema;
Fig. 6 is the esterification technique schema.
Embodiment
Below in conjunction with drawings and Examples, describe technical scheme of the present invention in detail.
Technical scheme of the present invention is that biofuel contains Cortex jatrophae (Jatropha curcas L.) seed oil; It is characterized in that: stearic acid content in the described barbadosnut seed oil≤0.4 (wt) %; Further scheme is that stearic acid content is 0.05～0.1 (wt) % in the described barbadosnut seed oil; Concrete scheme is, it is 2～10% Fatty Alcohol(C12-C14 and C12-C18) that above-mentioned biofuel also contains with the barbadosnut seed oil volume ratio; Described Fatty Alcohol(C12-C14 and C12-C18) is methyl alcohol, ethanol or ethylene glycol; More suitable scheme is that biofuel and petrifaction diesel are used with, the volume ratio of petrifaction diesel and biofuel 〉=20%; Petrifaction diesel and biofuel optimum volume ratio are 20～40%; Described petrifaction diesel is 0
#Diesel oil.
The preparation method of biofuel comprises barbadosnut seed oil production and barbadosnut seed oil refining, modified technique; It is characterized in that: described refining, modified technique may further comprise the steps:
A. hydration degum;
B. alkali-refining deacidification;
C. dehydration;
D. batch deodorization;
E. emulsification or esterification
Concrete emulsifying process is, in above-mentioned steps e, is under 5～50 ℃ the condition in temperature, adds Fatty Alcohol(C12-C14 and C12-C18) in the ratio of Fatty Alcohol(C12-C14 and C12-C18) and barbadosnut seed refining oil volume ratio 2～10%; Preferred technology is that described Fatty Alcohol(C12-C14 and C12-C18) is methyl alcohol, ethanol or ethylene glycol; Another kind of preparation technology is to prepare biofuel with barbadosnut seed refining oil esterification; Promptly in the barbadosnut seed refining oil: the ratio of methyl alcohol or ethanol mol ratio=1: 3～1: 6 adds methyl alcohol or ethanol, is catalyzer with sodium hydroxide or sodium methylate, and temperature is controlled at 35～65 ℃, reacts 1～2.5 hour.The preparation biofuel.
Embodiment
One. the barbadosnut seed oil production technique
1. raw material: Cortex jatrophae (Jatropha curcas L.) seed
After Cortex jatrophae bore fruit, pericarp was yellow and can gathers.The Cortex jatrophae of gathering is really carried out artificial or machine barking, obtain barbadosnut seed, require peeling rate＞99%.Barbadosnut seed makes moisture content＜6% through airing, and the barbadosnut seed shell is light tone darkly, can put in storage.
2. pre-treatment
2.1 remove impurity
By cleaning, screening, selection by winnowing, magnetic separation etc., remove the various impurity in the barbadosnut seed.
2.2 peel off
Unit mahine is peeled off～separated to utilization with the shell strip off of barbadosnut seed, and separating husk benevolence, obtains barbadosnut seed benevolence.Require hulling rate＞95%.
2.3 it is broken
With toothed roll crusher barbadosnut seed benevolence is carried out break process.
2.4 it is softening
Regulate the moisture and the temperature of barbadosnut seed benevolence, make it softening, increase plasticity.
2.5 roll embryo
Also claim " compressing tablet ", " rolling sheet ".Utilize mechanical pressure, the barbadosnut seed benevolence after softening is pressed into sheet, obtain giving birth to embryo.
2.6 slaking
Give birth to embryo through moistening, heat treated, certain physics chemical takes place change, make cooked flake.
3. oil expression
With above-mentioned barbadosnut seed benevolence cooked flake, put into hydraulic oil press, squeezing obtains barbadosnut seed oil continuously.According to the model difference of selected hydraulic oil press, the oil cake residual oil content does not wait 4～12%.For further improving oil yield, after oil cake can being pulverized, leach Residual oil with organic solvent again, promptly obtain barbadosnut seed behind the recovery organic solvent and leach oil.Remaining barbadosnut seed waste matter oil length＜1.5%.
Test by analysis, the barbadosnut seed oil component concentration that adopts above-mentioned production technique to make is (WT%):
Oleic acid 43.64;
Linolic acid 30.79;
Palmitinic acid 16.47;
Stearic acid 6.85;
Linolenic acid 1.52;
Peanut diluted acid 0.66;
Myristic acid 0.07.
Because the difference of Cortex jatrophae kind, 17% the phthalic acid of having an appointment also containing of having in its component, other component content are also different.
Two. barbadosnut seed oil refining, modified technique
1. technical process
Fig. 1 is seen in technical process.
2. master operation key points for operation
A. hydration degum
Fig. 2 is seen in technical process
(1) preheating: barbadosnut seed oil after filtration, the metering after, pump into oil refining cauldron, under agitation use the steam indirect heating, oily temperature is preheating to 75～80 ℃.
(2) Jia Shui and salt: be 0.2～0.3% of barbadosnut seed weight of oil with salt (sodium-chlor) amount, general barbadosnut seed oil amount of water is about 3%; Add water temp and should be higher than 5～10 ℃ of oil temperature, add water speed and be advisable with per minute 10～15kg, all under agitation carry out, the about per minute 60 of stirring velocity changes, add water intact after restir about 10 minutes.
(3) precipitation insulation: regulate heating steam, make oily temperature remain on 80 ℃, precipitate 6～8 hours, precipitation finishes, and discharges upper strata edible vegetable oil to the pond of coming unstuck from oil exit pipe, and oil foot enters the oil foot pot or the oil foot treating pond is handled.
(4) thermal dehydration operates in dehydration pot or the deodorization pot and carries out, and with vacuum degummed oil is drawn to the dehydration pot, and its amount must not surpass dehydration pot volumetrical 70%.Open steam and carry out indirect heating, oily temperature remains on 90～95 ℃, and vacuum tightness must not be lower than 0.09MPa, can change next procedure over to after the dehydration.
(5) oil foot is handled: adopt the indirect steam heating, the oil foot temperature is raised to 80～90 ℃, in the thin oil pin, stir the salt that adds oil foot weight 2～3% down.It is 70～80 ℃ that the viscous crude pin can add temperature, and concentration is 3～5%, and quantity is the salt solution of oil foot weight 20%.When treating that temperature is raised to 100 ℃, stop heated and stirred, precipitate 24 hours, reclaim the upper strata oil slick, after oil slick reclaims, discharge the oil-poor pin of lower floor about 1/2, the oil foot that upper strata oil-containing oil foot was discharged with next time is handled again.
B. alkali-refining deacidification
(1) degummed oil of handling through above-mentioned operation is adjusted to 25～30 ℃ with oily temperature, leaves standstill bubble is overflowed.
(2) add alkali (sodium hydroxide): it is definite that concentration of lye is looked the degummed oil acid number, or little sample testing is determined concentration of lye.Excess alkali is by 0.14～0.25% heavy interpolation of oil.
(3) add alkali lye speed: all alkali lye added in 5～10 minutes, stirring velocity per minute 60 right side of turning left, continue to stir 20～25 minutes, to oil, when soap obviously separates, reduce stirring velocity to per minute 30 right side of turning left, open steam heating, raise 1 ℃ with the per minute temperature and be advisable, whole temperature control is about 60 ℃.
(4) staticly settle disengaging time, be generally 6～8 hours, settling process is noted insulation (being incubated about 60 ℃).
(5) wash temperature: 80 ℃ of oil temperature, water temperature is not less than 85 ℃, soft water is preferably adopted in washing, and each water consumption is 5～15% of an oil mass, and washing times is 2～3 times (be washed till residual soap amount meets till the technic index in the oil), stirring velocity is minutes 30 right sides of turning left when adding water, add water and finish, stop to stir, staticly settle, each washing, settling time are 0.5～1 hour, and post precipitation can carry out washing next time after draining the waste water pin.
(6) change the deodorization of dewatering of deodorization pot over to.
(7) isolated soap stock under agitation adds the salt of soap stock amount 4～5% and is heated to about 80 ℃ (repeatedly heat up, leave standstill skimming), skims oil and enters washing pool and wash.
D. batch deodorization
(1) borrow vacuum to suck the deodorization pot oil of pre-treatment, soakage is about 60% of a pot body cubic capacity.
(2) heat up: the standard width of a room in an old-style house connects steam and is warming up to 100 ℃, opens the stripping open steam, and oily temperature is heated to about 180 ℃, and working pressure＜667Pa, deodorization time were controlled at 5～8 hours, and stripped vapor should be dry, is not with stove water.
(3) after deodorization finishes, under vacuum, carry out heat exchange, make below the oily temperature drop to 70 ℃, abolish vacuum then, eliminating deodorization processed oil---Cortex jatrophae refining oil through heat-transfer pipe and cold water.
Test above-mentioned barbadosnut seed refining oil component concentration by analysis and be (WT%):
Oleic acid 45.74;
Linolic acid 34.84;
Palmitinic acid 18.39;
Stearic acid 0.05;
Linolenic acid 0.96;
Peanut diluted acid 0;
Myristic acid 0.02.
By the barbadosnut seed refining oil that aforesaid method makes, stearic acid content has been lower than 0.1%.Above-mentioned technology contains the barbadosnut seed oil of phthalic acid for those, also can be removed.
E. emulsifying process
2～10% ratio adds Fatty Alcohol(C12-C14 and C12-C18) by volume in above-mentioned barbadosnut seed refining oil, as methyl alcohol, ethanol or ethylene glycol etc., fully stirs, and mixes, and carries out emulsification.In the emulsion process, temperature is controlled at 5～50 ℃.The emulsification method that the present invention adopts need not special catalyst and hot conditions, and it is simple to have technology, and production cost is low, the characteristics of emulsify well.Fig. 5 is seen in technical process.
Biofuel of the present invention, another kind of preparation technology are barbadosnut seed refining oil esterification techniques.Promptly carry out esterification and prepare biofuel with excessive methyl alcohol and barbadosnut seed refining oil.Fig. 6 is seen in technical process.Concrete operation method is, the Cortex jatrophae refining oil: the methyl alcohol mol ratio is 1: 3～1: 6, with sodium hydroxide is catalyzer, catalyst levels is 0.5～2% (weight percent) of barbadosnut seed refining oil, control reaction temperature is 35～65 ℃, mixing and stirring was reacted 1～2.5 hour, generated barbadosnut seed oil methyl esters and glycerine.Isolate the barbadosnut seed oil methyl esters and promptly obtain biofuel.Wherein barbadosnut seed oil methyl esters major ingredient is a Witconol 2301, methyl linoleate and Uniphat A60.
Adopt the biofuel of above-mentioned prepared, can use with arbitrary proportion and petrifaction diesel.Experiment shows, the volume ratio of petrifaction diesel and biofuel 〉=20% o'clock can further improve combustionproperty.Optimum volume ratio is 20～40%.Such blending ratio both can demonstrate fully the advantage of biofuel, can also further improve the spray characteristics in diesel motor, made in the cylinder mist of oil more tiny, and it is easier, more abundant to burn, thereby further promotes running of an engine efficient.
It is after 0.05% barbadosnut seed refining oil adds the Fatty Alcohol(C12-C14 and C12-C18) emulsification of volume ratio 2～10%, again with 0 of volume ratio 30% that table 1 has been listed stearic acid content
#Diesel oil blended physical and chemical index.As can be seen from the table, every index of this biofuel meets the requirement of company standard " Q/72036234～1.1～2003 " fully.The particularly improvement of remaining carbon, viscosity and cetane value all has significant effect to the dynamic performance and the exhaust emissions index of biofuel.And remaining carbon, viscosity and cetane value are relevant with stearic acid content, and along with stearic acid content reduces, remaining carbon descends, and viscosity reduces, and cetane value also can improve.
Try department through provincial constitutional law location survey, by standard " QC/T524～1999 " motor car engine performance test method and " GB1105～1987 " oil engine test stand performance experimental technique, use the 2S1100 diesel engine, GW100 electric eddy current dynamometer and test macro, FBY～2 auto smokemeters, to the biofuel of said ratio, with 0
#The engine pedestal contrast experiment of diesel oil proves that the biofuel of said ratio is as 0
#The substitute of diesel oil, its dynamic performance, specific fuel oil consumption etc. and 0
#Diesel oil does not have significant difference, but the exhaust emissions smoke intensity value has significant improvement.Particularly eliminated carcinogenic substances such as polycyclic aromatic hydrocarbon compounds in the tail gas basically, reduced the discharging of sulfide, carbide, nitride significantly, environment-friendly advantage is obvious.
Biofuel of the present invention, exhaust emissions index are improved obviously, have the remarkable environmental advantage, and production technique are simple, and production cost is low, can be widely used in senior diesel motor such as high-grade car and make fuel oil.And engine need not anyly change.
Table 1
| Sequence number | The technical indicator title | Actual value |
| 1 | Sulphur content % (m/m) | ≤0.02 |
| 2 | 10% steams excess carbon residue % (m/m) | ≤0.45 |
| 3 | Ash content % (m/m) | ≤0.004 |
| 4 | Moisture (V/V) % | Do not have |
| 5 | Kinematic viscosity (20 ℃) mm 2/s | 24.71～25.36 |
| 6 | Copper corrosion (50 ℃, 3h) | ≤ 1 grade |
| 7 | Mechanical impurity | Do not have |
| 8 | Condensation point ℃ | ≤～3 |
| 9 | Cold filter clogging temperature ℃ | ≤2 |
| 10 | Flash-point (remaining silent) ℃ | ≥30 |
| 11 | Cetane value | ≥45 |
| 12 | Density (20 ℃) mg/m 3 | 887.9～889.0 |
| 13 | Colourity number | ≤1.0 |
| 14 | Acidity mgKOH/100ml | 91.67～92.35 |
Claims (11)
1. biofuel contains barbadosnut seed oil; It is characterized in that: stearic acid weight percent content≤0.4 in the described barbadosnut seed oil.
2. biofuel according to claim 1 is characterized in that: the stearic acid weight percent content is 0.05～0.1 in the described barbadosnut seed oil.
3. biofuel according to claim 1 is characterized in that: also containing with the barbadosnut seed oil volume ratio is 2～10% methyl alcohol, ethanol or ethylene glycol.
4. according to claim 1,2 or 3 described biofuel, it is characterized in that: also contain petrifaction diesel with barbadosnut seed oil volume ratio 〉=20%.
5. biofuel according to claim 4 is characterized in that: the volume ratio of petrifaction diesel and barbadosnut seed oil is 20～40%.
6. biofuel according to claim 4 is characterized in that: described petrifaction diesel is 0
#Diesel oil.
7. according to the preparation method of the described biofuel of claim 1, comprise barbadosnut seed oil production and barbadosnut seed oil refining, modified technique.
8. biodiesel oil preparing process according to claim 7 is characterized in that: also comprise emulsification or esterification technique.
9. biodiesel oil preparing process according to claim 8 is characterized in that: described emulsifying process is: be under 5～50 ℃ the condition in temperature, add methyl alcohol, ethanol or ethylene glycol in the ratio of Fatty Alcohol(C12-C14 and C12-C18) and barbadosnut seed refining oil volume ratio 2～10%.
10. biodiesel oil preparing process according to claim 8 is characterized in that: described esterification technique is: in the barbadosnut seed refining oil: the ratio of methyl alcohol or ethanol mol ratio≤1: 3 adds methyl alcohol or ethanol, carries out esterification under catalyst action.
11. biodiesel oil preparing process according to claim 10, it is characterized in that: described esterification technique is: in the barbadosnut seed refining oil: methyl alcohol or ethanol mol ratio are that 1: 3～1: 6 ratio adds methyl alcohol or ethanol, are catalyzer with sodium hydroxide or sodium methylate; Be to react 1～2.5 hour under 35～65 ℃ the condition in temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100494316C (en) * | 2006-06-02 | 2009-06-03 | 中国农业科学院油料作物研究所 | Process for preparing biological diesel oil using palm oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462420C (en) * | 2005-04-30 | 2009-02-18 | 王嵬 | Biological diesel oil and its preparing method |
| CN100390251C (en) * | 2006-04-05 | 2008-05-28 | 贵州大学 | Preparation of curcas biological diesel oil by solid phase catalytic method |
| CN101440298B (en) * | 2008-12-09 | 2012-09-12 | 湘潭昭山油化科技有限公司 | Method for preparing -20 DEC C biodiesel from waste lipid by distillation process |
| CN102899157B (en) * | 2012-10-26 | 2013-08-14 | 四川大学 | Barbadosnut biological aviation fuel crude oil and preparation method thereof |
| CN105779105A (en) * | 2016-04-21 | 2016-07-20 | 哈尔滨工业大学 | Method for extracting biodiesel based on waste coffee grounds |
| CN107312578A (en) * | 2016-04-27 | 2017-11-03 | 广东博大新能源科技有限公司 | A kind of preparation method of gutter oil methanol cleaning fuel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100494316C (en) * | 2006-06-02 | 2009-06-03 | 中国农业科学院油料作物研究所 | Process for preparing biological diesel oil using palm oil |
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