CN100547056C - Utilize rectifying tower or distillation tower purification production method of bio-diesel oil - Google Patents
Utilize rectifying tower or distillation tower purification production method of bio-diesel oil Download PDFInfo
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- CN100547056C CN100547056C CNB2006100368678A CN200610036867A CN100547056C CN 100547056 C CN100547056 C CN 100547056C CN B2006100368678 A CNB2006100368678 A CN B2006100368678A CN 200610036867 A CN200610036867 A CN 200610036867A CN 100547056 C CN100547056 C CN 100547056C
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- distillation tower
- rectifying tower
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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 discloses a kind of rectifying tower or distillation tower purification production method of bio-diesel oil utilized.This method may further comprise the steps: be raw material with one of vegetables oil or animal oil or mixture 1., carry out esterification; 2. esterification reaction product is carried out roughing out and get thick methyl esters or thick ethyl ester; 3. thick methyl esters or thick ethyl ester are carried out rectifying tower or distillation tower purification, make the biofuel product; The rectifying tower or the distillation tower purification temperature of thick methyl esters or thick ethyl ester are 100-280 ℃, and vacuum tightness is 5000-100Pa, isolates methyl alcohol or ethanol, glycerine, obtains biofuel.This method can also be with step 1. esterification products carry out rectifying tower or distillation tower and purify, make biofuel.The biofuel purity of the present invention's preparation can reach more than 98%, meets the biofuel up to standard of international standard, has omitted washing and drying process simultaneously, and technical process is simple, does not have contaminated wastewater, saves the water treatment expense.
Description
Technical field
The present invention relates to the preparation of high-purity biodiesel, particularly relate to and utilize rectifying tower or distillation tower purification production method of bio-diesel oil.
Background technology
Along with the overexploitation of petroleum resources, oil engine has huge commercial promise with the development of biofuel.At present, the domestic technology of taking usually with the technology of biofuel (methyl esters) at the production oil engine is:
Esterification obtains intermediate product → static layering → get upper strata liquid → washing → drying tower → product (biofuel).
Using this production technique production biofuel exists following several respects to get problem: 1. adopt washing process, be difficult to impurity is thoroughly removed, the content of product fatty acid methyl ester etc. is relatively low, generally do not reach 95%, thereby the fatty acid methyl ester that does not reach standard biological diesel oil such as Europe discharging III is greater than 98% requirement, therefore make biofuel be difficult to apply, can not in high-grade automobile, use, require lower industry relatively and can only be applied in Industrial Boiler, farm machinery etc.; 2. produce a large amount of waste water in washing is handled, both environment was caused severe contamination, waste water resource does not meet environmental requirement now again; 3. adopt washing back product needed to carry out drying, increase equipment cost and processing cost by drying tower; 4. washing process removes and takes away most impurity (methyl alcohol, glycerine etc.), also takes away the methyl esters of part simultaneously, makes output capacity reduce.
The foreign biomolecule diesel production except that reaction (esterification) process, all needs the rapid separation and purification of multistep can finish the requirement of using purity.
Summary of the invention
Problem for the existence that overcomes above-mentioned prior art, of the present inventionly provide a kind of rectifying tower or distillation tower purification production method of bio-diesel oil utilized, can produce purity reaches more than 98%, the automobile biofuel that meets Europe discharging III standard, omit washing process simultaneously, solved industrial wastewater problem.
Purpose of the present invention is achieved through the following technical solutions:
Utilize rectifying tower or distillation tower purification production method of bio-diesel oil, it is characterized in that may further comprise the steps: be raw material 1., carry out esterification with one of vegetables oil or animal oil or mixture; 2. esterification reaction product is carried out roughing out and get thick methyl esters or thick ethyl ester; 3. thick methyl esters or thick ethyl ester are carried out rectifying tower or distillation tower purification, make the biofuel product; The rectifying tower or the distillation tower purification temperature of described thick methyl esters or thick ethyl ester are 100-280 ℃, and vacuum tightness is 5000-100Pa, isolates methyl alcohol or ethanol, glycerine, obtains biofuel.
Described step 2. in, roughing out is static layering or separates with high speed centrifugation.
Utilizing rectifying tower or distillation tower purification production method of bio-diesel oil can also be may further comprise the steps: be raw material with one of vegetables oil or animal oil or mixture 1., carry out esterification; 2. esterification reaction product is carried out rectifying tower or distillation tower purification, make the biofuel product; The temperature that described esterification reaction product rectifying tower or distillation tower are purified is 100-280 ℃, and vacuum tightness is 5000-100Pa, isolates methyl alcohol or ethanol, glycerine, obtains biofuel.
Above-mentioned two kinds of method stepss 1. in, vegetables oil or animal oil raw material and methyl alcohol or ethanol carry out esterification, its reaction product mainly comprises methyl esters or ethyl ester, glycerine, methyl alcohol or ethanol.Described vegetables oil is Oleum Cocois, plam oil, rapeseed oil, Jatropha curcas oil, soybean oil or peanut oil; Described animal oil is lard, butter, fowl poultry oil or fish oil.
Thick methyl esters of the present invention is meant that the purity that obtains by roughing out is lower than 95% methyl esters.Thick ethyl ester is meant that the purity that obtains by roughing out is lower than 95% ethyl ester.Distillation tower of the present invention is meant common distillation tower.Rectifying tower be meant in the distillation column of distillation tower, can add have various types of fillers as. ring, screen waviness, porcelain ring, conjugate ring filler etc. also are the rectifying tower of using always.
With respect to prior art, the present invention has following advantage:
The present invention utilizes rectifying tower or distillation tower purification techniques, realize and finish the purification and the process for refining of biofuel (methyl esters or ethyl ester), the biofuel purity of purifying can reach more than 98%, thereby produce the biofuel up to standard that meets international standard, washing and drying process have been omitted simultaneously, technical process is simple, does not have contaminated wastewater, saves the water treatment expense.
Description of drawings
Fig. 1 utilizes rectifying tower or distillation tower purification techniques production biofuel schematic flow sheet for the present invention.
Shown in the figure: 1 heating kettle, 2 hot oil furnaces, 3 rectifying columns or distillation column, 4 methyl alcohol receiving tanks, 5 glycerine receiving tanks, 6 methyl esters receiving tanks, 7 condensers.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples, but the scope of protection of present invention is not limited to the scope that embodiment represents.
The present invention is a kind of method of utilizing rectifying tower or distillation tower purification techniques production biofuel stream, and the main technique step is: raw material → reaction back intermediate product → roughing out → rectifying tower or distillation tower purification → finished product (biofuel) and byproduct (glycerine).Or, raw material → reaction back intermediate product → rectifying tower or distillation tower purification → finished product (biofuel) and byproduct (glycerine).
Fig. 1 utilizes rectifying tower or distillation tower purification production biofuel schematic flow sheet for the present invention.As shown in Figure 1,1 heating kettle, 2 hot oil furnaces, 3 rectifying columns or distillation column, 4 methyl alcohol receiving tanks, 5 glycerine receiving tanks, 6 methyl esters receiving tanks, 7 condensers
According to above-mentioned processing step, at first, be to be the feedstock production coarse biodiesel with one of vegetables oil or animal oil or mixture.Vegetables oil can adopt Oleum Cocois, plam oil, rapeseed oil, Jatropha curcas oil (numb maple), soybean oil or peanut oil or the like, and animal oil can adopt lard, butter, fowl poultry oil or fish oil etc., does not enumerate one by one at this.
The preparation biofuel mainly comprises following four kinds of methods at present: enzymolysis, pyrolysis, supercritical esterification and transesterify and esterification.The transesterify esterification is the main method of producing fatty acid methyl ester at present.Transesterify is to utilize methyl alcohol or ethanol, and the glyceryl in the triglyceride is replaced to get off, and forms the longer chain fatty acid methyl esters, increases mobile and reduction viscosity, makes it to be suitable as fuel and uses.This reaction can be very low in temperature, carry out under the normal pressure, and the reaction conditions gentleness is easy to control, can add catalyzer simultaneously and shorten reaction time, improves productive rate.Vegetables oil or animal oil and methyl alcohol (or ethanol) are carried out esterification (or transesterification reaction), and its reaction back intermediate product contains methyl esters (or ethyl ester), glycerine (glycerol), excessive methyl alcohol (or ethanol) and a small amount of impurity.Its reaction equation is as follows:
After carrying out above-mentioned esterification, esterification reaction product is carried out roughing out by static layering or with high speed centrifugation, then thick methyl esters is carried out rectifying tower or distillation tower purification processes, temperature is 100-280 ℃, vacuum tightness is 5000-100Pa, isolate methyl alcohol or ethanol, glycerine, obtain biofuel.Distilling kettle base solution at last is nonesterified dimension E, plant sterol, lipid, impurity etc.
After carrying out above-mentioned esterification, also esterification reaction product can be carried out rectifying tower or distillation tower purification processes to esterification reaction product, temperature is 100-280 ℃, vacuum tightness is 5000-100Pa, isolates methyl alcohol or ethanol, glycerine, obtains biofuel.
Comparatively speaking, carry out rectifying tower again after the roughing out or the distillation tower purification processes is better.Owing to by comparatively economic roughing out a large amount of methyl alcohol or esterification reaction products such as ethanol, glycerine are separated from object, can be improved follow-up rectifying tower or distillation tower purification processes efficient greatly.
Embodiment 1
Adopt Oleum Cocois and methyl alcohol to carry out esterification, the mol ratio of Oleum Cocois and methyl alcohol is 1: 6.Esterification reaction product passes through static layering, as shown in Figure 1, get upper strata liquid (thick methyl esters) 800ml and enter heating kettle 1, through hot oil furnace 2 heating, enter distillation column 3 then and distill processing, temperature rises to 280 ℃ from 100 ℃, vacuum tightness is 2000Pa, through the cooling of condenser 7, purify out successively methyl alcohol, glycerine and methyl esters, fractionation is in methyl alcohol receiving tank 4, glycerine receiving tank 5, methyl esters receiving tank 6 respectively.Wherein, temperature is at 100-120 ℃, the methyl alcohol of purifying out; Temperature is at the 120-180 ℃ of glycerine of purifying out; Temperature is at 180-280 ℃ of methyl esters 683 grams of purifying out, and residual impurity is stayed the heating kettle surge tank.After tested, prepared methyl esters purity is 98.6%.
Embodiment 2
Adopt butter and ethanol to carry out esterification, butter and alcoholic acid mol ratio are 1: 6.5.Esterification reaction product passes through static layering, as shown in Figure 1, get upper strata liquid (thick ethyl ester) 720mL and enter heating kettle 1, enter distillation column 3 then and distill processing, be filled with screen waviness packings in the distillation column 3, temperature rises to 280 ℃ from 100 ℃, vacuum tightness is 2000Pa, through the cooling of condenser 7, purify out successively methyl alcohol, glycerine and methyl esters, fractionation is in methyl alcohol receiving tank 4, glycerine receiving tank 5, methyl esters receiving tank 6 respectively.Wherein, temperature is at 100-120 ℃, the methyl alcohol of purifying out; Temperature is at the 120-180 ℃ of glycerine of purifying out; Temperature is at 180-280 ℃ of methyl esters 611 grams of purifying out, and residual impurity is stayed in the heating kettle surge tank.After tested, prepared methyl esters purity is 99%.
Embodiment 3
Adopt rapeseed oil and methyl alcohol to carry out esterification, the mol ratio of rapeseed oil and methyl alcohol is 1: 7.Esterification reaction product carries out roughing out by high speed centrifugation, get thick methyl esters 650mL and enter heating kettle 1, as shown in Figure 1, through hot oil furnace 2 heating, enter distillation column 3 then and distill processing, temperature rises to 280 ℃ from 100 ℃, vacuum tightness is 2000Pa, through the cooling of condenser 7, purify out successively methyl alcohol, glycerine and methyl esters, fractionation is in 4 methyl alcohol receiving tanks, 5 glycerine receiving tanks, 6 methyl esters receiving tanks respectively.Wherein, temperature is at 100-120 ℃, the methyl alcohol of purifying out; Temperature is at the 120-180 ℃ of glycerine of purifying out; Temperature is at 180-280 ℃ of methyl esters 510 grams of purifying out, and residual impurity is stayed in the heating kettle surge tank.After tested, prepared methyl esters purity is 98.3%.
Embodiment 4
Adopt fish oil and methyl alcohol to carry out esterification, the mol ratio of fish oil and methyl alcohol is 1: 6.5.As shown in Figure 1, esterification reaction product 720mL enters heating kettle 1, distillation column 3 distills processing then, temperature rises to 280 ℃ from 100 ℃, vacuum tightness is 2000Pa, through the cooling of condenser 7, purify out successively methyl alcohol, glycerine and methyl esters, fractionation is in 4 methyl alcohol receiving tanks, 5 glycerine receiving tanks, 6 methyl esters receiving tanks respectively.Wherein, temperature is at 100-120 ℃, the methyl alcohol of purifying out; Temperature is at the 120-180 ℃ of glycerine of purifying out; Temperature is at 180-280 ℃ of methyl esters 310 grams of purifying out, and residual impurity is stayed in the heating kettle surge tank.After tested, prepared methyl esters purity is 98.8%.
Claims (5)
1, utilizes rectifying tower or distillation tower purification production method of bio-diesel oil, it is characterized in that may further comprise the steps: be raw material 1. with vegetables oil or animal oil, carry out esterification, vegetables oil or animal oil and methyl alcohol or alcoholic acid mol ratio are 1: 6,1: 6.5 or 1: 7; 2. esterification reaction product is carried out roughing out and get thick methyl esters or thick ethyl ester; 3. thick methyl esters or thick ethyl ester are carried out rectifying tower or distillation tower purification, make the biofuel product; The rectifying tower or the distillation tower purification temperature of described thick methyl esters or thick ethyl ester are 100-280 ℃, and vacuum tightness is 5000-100Pa, isolates methyl alcohol or ethanol, glycerine, obtains biofuel.
2, according to described rectifying tower or the distillation tower purification production method of bio-diesel oil utilized of claim 1, it is characterized in that described step is 2., roughing out is static layering or separates with high speed centrifugation.
3, according to described rectifying tower or the distillation tower purification production method of bio-diesel oil utilized of claim 1, in it is characterized in that described step 1., vegetables oil or animal oil raw material and methyl alcohol or ethanol carry out esterification, and its reaction product mainly comprises methyl esters or ethyl ester, glycerine, methyl alcohol or ethanol.
4, according to described rectifying tower or the distillation tower purification production method of bio-diesel oil utilized of claim 3, it is characterized in that described vegetables oil is Oleum Cocois, plam oil, rapeseed oil, Jatropha curcas oil, soybean oil or peanut oil; Described animal oil is lard, butter or fish oil.
5, utilize rectifying tower or distillation tower purification production method of bio-diesel oil, it is characterized in that may further comprise the steps: be raw material 1. with vegetables oil or animal oil, carry out esterification, vegetables oil or animal oil and methyl alcohol or alcoholic acid mol ratio are 1: 6,1: 6.5 or 1: 7; 2. esterification reaction product is carried out rectifying tower or distillation tower purification, make the biofuel product; The temperature that described esterification reaction product rectifying tower or distillation tower are purified is 100-280 ℃, and vacuum tightness is 5000-100Pa, isolates methyl alcohol or ethanol, glycerine, obtains biofuel.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100368678A CN100547056C (en) | 2006-08-01 | 2006-08-01 | Utilize rectifying tower or distillation tower purification production method of bio-diesel oil |
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| CNB2006100368678A CN100547056C (en) | 2006-08-01 | 2006-08-01 | Utilize rectifying tower or distillation tower purification production method of bio-diesel oil |
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| CN1931965A CN1931965A (en) | 2007-03-21 |
| CN100547056C true CN100547056C (en) | 2009-10-07 |
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| CN105001997B (en) * | 2015-08-06 | 2018-05-11 | 天津大学 | The method and device of high added value fatty acid methyl ester in electromagnetic wave rectification under vacuum separating-purifying animal and plant fat |
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Granted publication date: 20091007 Termination date: 20170801 |