CN107541339A - The product fractionating device and fractionation process of a kind of biodiesel - Google Patents
The product fractionating device and fractionation process of a kind of biodiesel Download PDFInfo
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- CN107541339A CN107541339A CN201610457308.8A CN201610457308A CN107541339A CN 107541339 A CN107541339 A CN 107541339A CN 201610457308 A CN201610457308 A CN 201610457308A CN 107541339 A CN107541339 A CN 107541339A
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Abstract
The present invention discloses the product fractionating device and fractionation process of a kind of biodiesel,The fractionating device includes main fractionating tower and side line treating column,Main fractionating tower sets four sections,Bottom sets two charging apertures,Main fractionating tower is the heavy constituent in biodiesel coarse product to be separated with the fatty acid methyl ester containing light component,Treating column is to the separation to light component in the fatty acid methyl ester containing light component and fatty acid methyl ester,And the serious air circulation gasification process of main fractionating tower and side line treating column and its light component circulating vaporization technique are set,To reduce the oil gas partial pressure of heavy constituent in main fractionating tower,Help heavy constituent vaporization,Column bottom temperature is reduced under the conditions of same vaporization rate so as to realize,The temperature of main fractionating tower bottom of towe of the present invention is down to 175~220 DEG C,Pressure is 1.0~11kpa,It is effectively prevented from material coking,Reduce oil and gas loss,So as to solve the problems, such as tower top oil and gas loss under coking problem caused by bottom of towe cut point height or high vacuum.
Description
Technical field
The present invention relates to biochemical industry separation field, the product purification separating technology of particularly a kind of biodiesel.
Background technology
Biodiesel is the regenerative resource of cleaning, greatly develops biodiesel to sustainable economic development, promotes the energy
Substitute, mitigate environmental pressure, control urban atmospheric pollution has important strategic importance.At present in industrialized production, biological bavin
Oil production uses ester exchange process, is using low-carbon alcohols materials such as methanol, the glycerine in the triglyceride in feedstock oil is sent out
Give birth to ester exchange and substitute to get off, form biodiesel coarse product（Fatty acid methyl ester）With byproduct glycerine, it is both needed to after the two separation
Further refining spearation is wanted just to obtain qualified products.
In existing biodiesel coarse product fractionation process, due to biodiesel coarse product（Fatty acid methyl ester）
In the feedstock oil triglyceride containing a certain amount of unreacted and partial reaction, two sweet ester components, it is necessary to the side for passing through rectifying
Method, which removes it, can just obtain qualified products.Biodiesel coarse product fractionation process uses common vacuum distillation at present, should
Method is primarily present following problem：（1）The boiling point of biodiesel oil product fatty acid methyl ester is very high, and the boiling point under 1kpa is
170~200 DEG C, even if using high vacuum in fractional distillation process, it is also difficult to realize and vaporize isolated qualified products, and coarse biometric
Unsaturated bond content is more in diesel oil, has the characteristic of easy coking at high temperature, conventional vacuum distillation bottom of towe temperature is typically all
At 250~290 DEG C so that material coking in actual fractional distillation process and influence product quality；（2）Solves column bottom temperature high material knot
Burnt Perfected process is to try to improve vacuum, but condition of high vacuum degree can cause substantial amounts of oil gas volatilization to lose, therefore vacuum
It is appropriate, should not be too high and cause to be lost；（3）Biodiesel coarse product also contains micro light component（Moisture, methanol component,
The light components such as glycerine, fixed gas）, light component separation can thoroughly not make in biodiesel oil product index flash-point and total glycerol content not
It is qualified, product quality is influenceed, therefore the height selection needs of product fractionating column vacuum are taken into account and obtained while removing light component
Qualified biodiesel oil product, also wants that column bottom temperature is relatively low, energy consumption is low, therefore is to be difficult to reality using conventional vacuum distillation method
Existing.
CN1869163A proposes a kind of method that biodiesel is produced using molecular distillation technique, and this method is using separation
Distillation technique, purification and the process for refining of biodiesel are realized and completed, the biology up to standard for meeting international standard can be produced
Diesel oil, washing and drying process are omitted, without contaminated wastewater.This method is a kind of preferably purification of biodiesel and refined work
Skill, but not only flow is complicated for the technique, including molecule evaporator, degassing system, feed system, heating system, cooling vacuum system
System and control system etc., and technology and equipment requires that high, equipment manufacturing cost is high, production scale is limited, thus constrain
The technology in industrial development and large-scale application.
CN102604665A discloses a kind of biodiesel continuous rectification system and technique based on multi-layer evaporation, the system
Including feed pump, heat exchanger, condenser, Multilayer evaporator, product pans, discharging pump, rectifying column, light component pans, return
Flow pump, the equipment such as preheater, the beneficial effect of this method be coarse biodiesel after Multilayer evaporator purifies light component, after promoting
Continuous rectifying column system maintains higher vacuum.The process system is essentially first by light component continuous evaporation, so as to improve
The vacuum of follow-up rectifying column, not only technological process is complicated, and the equipment being related to is more, and does not solve rectifying fundamentally
The problem of tower column bottom temperature is high, high energy consumption.
Analyzed more than, the knot that biodiesel coarse product fractional distillation process has column bottom temperature height and brought in the prior art
The high product quality etc. that influences of product volatilization loss caused by burnt problem, condition of high vacuum degree, light component content caused by rough vacuum is asked
Inscribe urgently to be resolved hurrily.
The content of the invention
To solve to have the high coking problem brought of column bottom temperature, Gao Zhen when biodiesel fractionation is refined in the prior art
Product volatilization loss caused by reciprocal of duty cycle, light component content caused by rough vacuum high the problems such as influenceing product quality, the present invention carries
For a kind of biodiesel coarse product fractionation process, by the way that biodiesel oil product main fractionating tower is combined and side line with side line tower
Tower light component circulating vaporization and vacuum gas circulating vaporization technique solve that bottom of towe cut point is high and coking problem, and reduce light component
Volatilization loss, obtain high-quality biodiesel oil product.
The technical purpose of the present invention is achieved through the following technical solutions：
In a first aspect, the invention provides a kind of product fractionating device of biodiesel, the fractionating device includes main fractionating tower
It is raw and treating column, the main fractionating tower are divided into stripping section, feedstock vaporisation section, rectifying section and condensing reflux section from bottom to up
Thing diesel oil crude product feed pipe connects the first vaporizer and the second vaporizer, the first charging of the first vaporizer and main fractionating tower respectively
Position connects, and the second feed entrance point of the second vaporizer and main fractionating tower connects, wherein, the second feed entrance point is between bottom of towe
Stripping section, it is feedstock vaporisation section between the first feed entrance point and the second feed entrance point；The top of main fractionating tower sets top of tower gas
Phase discharge nozzle, it is connected by vaccum-pumping equipment I with the first vaporizer, sets crude product to extract out above the rectifying section of main fractionating tower
Line, crude product extract the top that line is connected to main fractionating tower condensing reflux section by the reflux condenser of tower top out, and crude product is extracted out
Line is connected by treating column reboiler with treating column, and the top for the treatment of column sets light component discharge nozzle, and it passes through vaccum-pumping equipment
II is connected with the second vaporizer；The bottom of towe of main fractionating tower and treating column is respectively provided with collection device.
Further, the number of theoretical plate needed for the stripping section is 2 ~ 6 layers, number of theoretical plate needed for feedstock vaporisation section for 1 ~
3 layers, the number of theoretical plate needed for rectifying section 3 is 5 ~ 12 layers, and the number of theoretical plate needed for condensing reflux section is 2 ~ 5 layers.
Further, it is tower plate structure or filling-material structure in the tower of the main fractionating tower and treating column.The column plate is selected from
In bubble cap plate, sieve aperture shape column plate, linde sieve tray, multiple-downcomer sieve tray, float valve type column plate, combined trapezoid spray tray or composite plate
One or more；The filler is shaped as rectangular saddle ring, cascade ring, Pall ring, θ rings, flat ring, spiral shape, perforated plate corrugated, silk
At least one of net ripple.
Further, the bottom of the main fractionating tower is also associated with main fractionating tower bottom reboiler.
Further, first vaporizer and the second vaporizer are in the prior art by aiding in mode of heating by liquid
The equipment of rapid vaporization, carburetor structure can be in shell and tube vaporizer, thin film evaporation formula vaporizer, jet-type carbureter etc.
Any one.
Further, the vaccum-pumping equipment I and vaccum-pumping equipment II are in screw vacuum pump, water ring pump and liquid rotary pump etc.
Any one, it can be one or more levels to vacuumize series, and its effect is to be made by vacuumizing in main fractionating tower and treating column
Produce negative pressure.
Second aspect, present invention also offers a kind of product fractionation process of biodiesel, in above-mentioned fractionating device,
The temperature for controlling tower top in main fractionating tower is 40~65 DEG C, and pressure is 0.5kpa~10kpa；Biodiesel crude product passes through biological bavin
Oily crude product feed pipe respectively enters the first vaporizer and the second vaporizer, fatty acid methyl ester for vaporizing to obtain through the first vaporizer etc.
Component enters feedstock vaporisation section from the first feed entrance point, introduces the bottom of rectifying section, realizes that rectifying separates subsequently into rectifying section；
The components such as the fatty acid methyl ester through the vaporization of the second vaporizer enter the top of stripping section from the second feed entrance point, to bottom of towe heavy constituent
Carry out after helping vaporization, be also upwardly into rectifying section and realize separation；The heavy constituent carried in the components such as rectifying section, fatty acid methyl ester
Be condensed separation, isolate heavy constituent fatty acid methyl ester component Parts cooled down into reflux condenser after return to tower top,
Line is extracted out from crude product treating column is entered by treating column reboiler in part；The gas part of main fractionating tower tower top passes through top of tower
Gas phase discharge nozzle and connected vaccum-pumping equipment I introduce the first vaporizer；Into the component for the treatment of column, then light component after boiling
Being circulated by light component discharge nozzle, vaccum-pumping equipment II into the second vaporizer, the component for the treatment of column bottom of towe is collected,
Produce biodiesel finished product.
Wherein, main fractionating tower tower top introduces vacuumize gas and account for main fractionating tower top gas the 1/10~1/2 of the first vaporizer；
The gas that light component at the top for the treatment of column enters the second vaporizer accounts for the 1/10~1/2 of refined tower overhead gas.
In the fractionation process of the present invention, the separation process to biodiesel crude product sets main fractionating tower and side line treating column,
Main fractionating tower is the heavy constituent in biodiesel coarse product to be separated with the fatty acid methyl ester containing light component, main fractionation
The tower overhead gas of tower is N2, vapor, the mixed gas of methanol gas and fatty acid methyl esters oil gas etc., treating column is to containing light
The separation of light component and fatty acid methyl ester in the fatty acid methyl ester of component, the tower overhead gas for the treatment of column is also N2, vapor, methanol gas
With the mixed gas of fatty acid methyl esters oil gas etc..
Further, in above-mentioned fractionation process, when biodiesel crude product is fed, the first vaporizer and the second vaporization are introduced
The mass ratio of device is 1:1~10：1.
Further, in above-mentioned fractionation process, the main fractionating tower tower top into the first vaporizer vacuumizes gas with entering
The mass ratio for entering the biodiesel crude product of the first vaporizer is 1:20~1:100.
Further, in above-mentioned fractionation process, the crude product of main fractionating tower is extracted out to return by condensing reflux in line and led
The mass ratio of gas of the gas with entering treating column at the top of fractionating column is 1:5~1：50.
Further, in above-mentioned fractionation process, the bottom of towe heavy constituent of main fractionating tower mainly include triglyceride, two sweet esters and
Other esters or fatty acid material, control charging, make heavy constituent account for 0.5wt%~5wt% of biodiesel crude product total feed.
Further, in above-mentioned fractionation process, the tower top temperature for controlling treating column is 120~160 DEG C, and pressure is
1.0kpa~15kpa, column bottom temperature are 140~180 DEG C, and pressure is 2.0~15kpa.
Further, in above-mentioned fractionation process, the refined column overhead into the second vaporizer vacuumizes gas with entering
The mass ratio of the biodiesel crude product of second vaporizer is 1:10~1:50.
Compared with prior art, the present invention has the advantage that：
Due to the components such as unreacting material triglyceride, two sweet ester of intermediate product in biodiesel crude product be present, on the one hand make its boiling
Ten minutes height of point, and contain many saturated bonds, when using purified product is evaporated under reduced pressure, polymerization coking occurs in temperature >=220 DEG C
Phenomenon, in the prior art in order to reduce column bottom temperature, ultrahigh vacuum is typically taken, not only results in substantial amounts of oil gas volatilization damage
Lose, also high is required to equipment and operating process, i.e., it is uneconomical and do not save.The fractionating device and fractionation process of the present invention is set
The serious air circulation gasification process of main fractionating tower and side line treating column and its light component circulating vaporization technique, in suitable vacuum
Spend under operating condition, tower top is vacuumized to the feedstock vaporisation section of gas part introducing main fractionating tower, by side line tower light component part
Biodiesel main fractionating tower stripping section is introduced, to reduce the oil gas partial pressure of heavy constituent in main fractionating tower, helps heavy constituent vaporization, from
And column bottom temperature is reduced under the conditions of same vaporization rate can be realized, and under the technical scheme more than, main fractionating tower bottom of towe of the present invention
Temperature be down to 175~220 DEG C, pressure is 1.0~11kpa, is effectively prevented from material coking, oil and gas loss is reduced, so as to solve
Certainly tower top oil and gas loss problem under coking problem caused by bottom of towe cut point height or high vacuum.
High-quality biodiesel oil product can be obtained using the fractionating device and fractionation process of the present invention, in meeting and being better than
State national standard BD100 index request.
Brief description of the drawings
The width of accompanying drawing 1 of the present invention,
The fractionating device of Fig. 1 embodiments 1,
Wherein 1. main fractionating towers, 2. treating columns, 3. biodiesel crude product feed pipes, 4. first vaporizers, 5. second vaporizers, 6.
First feed entrance point, 7. second feed entrance points, 8. vaccum-pumping equipments I, 9. vaccum-pumping equipments II, 11. stripping sections, 12. charging vapour
Change section, 13. rectifying sections, 14. condensing reflux sections, 15. top of tower gas phase discharge nozzles, 16. crude products extraction line, 17. reflux condensation modes
Device, 18. main fractionating tower bottom reboilers, 21. light component discharge nozzles, 22. treating column reboilers.
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Embodiment 1
As shown in figure 1, it is the fractionating device of the present invention, including main fractionating tower 1 and treating column 2, the main fractionating tower 1 is from bottom to up
Stripping section 11, feedstock vaporisation section 12, rectifying section 13 and condensing reflux section 14 are divided into, biodiesel crude product feed pipe 3 is distinguished
The first vaporizer 4 and the second vaporizer 5 are connected, the first vaporizer 4 is connected with the first feed entrance point 6 of main fractionating tower 1, the second vapour
Change device 5 to be connected with the second feed entrance point 7 of main fractionating tower 1, wherein, the second feed entrance point 7 is to being stripping section 11 between bottom of towe, the
It is feedstock vaporisation section 12 between one feed entrance point 6 and the second feed entrance point 7；The top of main fractionating tower 1 sets top of tower gas phase to go out
Expects pipe 15, it is connected by vaccum-pumping equipment I 8 with the first vaporizer 4, and the top of rectifying section 13 of main fractionating tower 1 sets crude product
Extract line 16 out, crude product extracts line 16 out and is connected to the upper of the condensing reflux section 14 of main fractionating tower 1 by the reflux condenser 17 of tower top
Portion, crude product are extracted line 16 out and are connected by treating column reboiler 22 with treating column 2, and the top for the treatment of column 2 sets light component to discharge
Pipe 21, it is connected by vaccum-pumping equipment II 9 with the second vaporizer 5；The bottom of towe of main fractionating tower 1 and treating column 2 is respectively provided with collection
Device.
In above-mentioned fractionating device, the bottom of main fractionating tower 1 connection main fractionating tower bottom reboiler 18, for the sake of another safety, take out
Vacuum equipment I 8 and vaccum-pumping equipment II 9 are also associated with vacuum protection tank.
In embodiment 2 ~ 4, the fractionation of coarse biodiesel is carried out using the fractionating device described in embodiment 1.
Coarse biodiesel raw material is that tung oil obtains the mixture of fatty acid methyl ester and glycerine with methanol by ester exchange reaction,
Fatty acid methyl ester phase, i.e. coarse biodiesel raw material are obtained after two-phase laminated flow again, tung oil property is shown in Table 1.
Table 1
Embodiment 2
The process conditions being fractionated using above fractionating device to biodiesel crude product are as follows：
The biodiesel crude product come first from biodiesel reaction and phase separation process is divided by biodiesel crude product feed pipe 3 is
The component such as two-way, the fatty acid methyl ester all the way through the vaporization of the first vaporizer 4 enters feedstock vaporisation section 12 from the first feed entrance point 6,
The bottom of rectifying section 13 is introduced, realizes that rectifying separates subsequently into rectifying section 13；The fat that another way vaporizes through the second vaporizer 5
The components such as sour methyl esters enter the top of stripping section 11 from the second feed entrance point 7, and bottom of towe heavy constituent is carried out after helping vaporization（It is stripped off
The fatty acid methyl ester component contained in bottom of towe heavy constituent）, also it is upwardly into rectifying section 13 and realizes separation.In rectifying section 13, fat
The heavy constituent carried in sour methyl esters component is condensed separation, and the fatty acid methyl ester component Parts for isolating heavy constituent enter returned cold
Condenser 17 returns to tower top after being cooled down, partly extracting line 16 out from crude product enters treating column reboiler 22.
This fractionation process also has two circulations to vacuumize gas, and the gas part of the tower top of main fractionating tower 1 passes through top of tower gas
Phase discharge nozzle 15 and connected vaccum-pumping equipment I 8 introduce the first vaporizer 4；It is light into the component for the treatment of column 2, then after boiling
Component is circulated by light component discharge nozzle 21, vaccum-pumping equipment II 9 into the second vaporizer 5.
In above-mentioned fractionation process, main fractionating tower 1 is the heavy constituent in biodiesel coarse product and containing light component
Fatty acid methyl ester separated, the tower overhead gas of main fractionating tower 1 is N2, vapor, methanol gas and fatty acid methyl esters oil gas etc.
Mixed gas.Treating column 2 refines to the separation to light component in the fatty acid methyl ester containing light component and fatty acid methyl ester
The tower overhead gas of tower 2 is also N2, vapor, the mixed gas of methanol gas and fatty acid methyl esters oil gas etc., obtained from the bottom of towe for the treatment of column 2
To biodiesel oil product.
Concrete technology condition is as follows：
Tower diameter：φ 300mm, tower height：9620mm；Stripping section 11 and rectifying section 13 use stainless steel Pall ring filler, condensing reflux
Section 14 and feedstock vaporisation section 12 use ripple silk net filler.
Biodiesel crude product inlet amount：540kg/h, fatty acid methyl ester component therein account for the 95.8% of inlet amount；Into
The biodiesel crude product quality ratio of one vaporizer 4 and the second vaporizer 5 is 5:1.
Feeding temperature is 98 DEG C；
The tower top temperature of main fractionating tower 1 is 52 DEG C, 5~5.5kpa of tower top pressure；
In main fractionating tower 1, the material at the top about 20% of rectifying section 13 is back to tower top as overhead reflux, about 80% after cooling
Material enter treating column 2 carry out lights removal；
In treating column 2, tower top temperature is 132~134.5 DEG C, and pressure is 5.3kpa~5.8kpa, and column bottom temperature is 151~155
DEG C, pressure is 6.8~7.3kpa.
The two-way circulation of this technique vacuumizes gas, and the part that the tower overhead gas of main fractionating tower 1 introduces the first vaporizer 4 accounts for main point
Evaporate the 1/5 of tower overhead gas；The part that the tower overhead gas for the treatment of column 2 introduces the second vaporizer 5 accounts for the 1/2.5 of refined tower overhead gas.
Under the operating pressure, the column bottom temperature of realization is 196.4 DEG C, tower bottom pressure 6.2kPa；From the bottom of towe for the treatment of column 2
Biodiesel oil product is obtained, obtained biodiesel flow is 492.6kg/h, and biodiesel oil product yield is 95.22%, product
Property is shown in Table 2.
Table 2
As can be seen here, carrying out biodiesel oil product fractionation using this method has advantages below；The column bottom temperature of fractionating column is significantly
Degree reduces, it is possible to prevente effectively from material coking；Vacuum reduces, and is advantageous to energy-conservation and oil gas volatilization loss；Material coking is lost
And oil gas volatilization loss is few, biodiesel oil product quality is good, high income（＞ 95%）.
Embodiment 3
It is as follows with embodiment 2, concrete technology condition to the operating process that biodiesel crude product is fractionated：
Tower diameter：φ 300mm, tower height：9620mm；Stripping section 11 and rectifying section 13 use stainless steel Pall ring filler, condensing reflux
Section 14 and feedstock vaporisation section 12 use ripple silk net filler.
Biodiesel crude product inlet amount：540kg/h, fatty acid methyl ester component therein account for the 95.8% of inlet amount；Into
The biodiesel crude product quality ratio of one vaporizer 4 and the second vaporizer 5 is 1:1；
Feeding temperature is 110 DEG C；
The tower top temperature of main fractionating tower 1 is 49 DEG C, 2.5~3.5kpa of tower top pressure；
In main fractionating tower 1, the material at the top about 20% of rectifying section 13 is back to tower top as overhead reflux, about 80% after cooling
Material enter treating column 2 carry out lights removal；
In treating column 2, tower top temperature is 126.6~128 DEG C, and pressure be 2.8kpa~3.5kpa, column bottom temperature for 145.1~
146.5 DEG C, pressure is 3.0~3.8kpa.
The two-way circulation of this technique vacuumizes gas, and the part that the tower overhead gas of main fractionating tower 1 introduces the first vaporizer 4 accounts for main point
Evaporate the 1/3 of tower overhead gas；The part that the tower overhead gas for the treatment of column 2 introduces the second vaporizer 5 accounts for the 1/2 of refined tower overhead gas.
Under the operating pressure, the column bottom temperature of realization is 212.5 DEG C, pressure 4.4kPa；Obtained from the bottom of towe for the treatment of column 2
Biodiesel oil product, obtained biodiesel flow are 477.23kg/h, and biodiesel oil product yield is 92.25%, product property
It is shown in Table 3.
Table 3
As can be seen here, when carrying out biodiesel oil product fractionation using this method, the more conventional fractional distillation process of column bottom temperature of fractionating column
Decrease, it is possible to reduce material coking；The more conventional fractional distillation process of vacuum has a little reduction, and energy-conservation and oil gas volatilization are lost
There is certain help；Material coking loss and oil gas volatilization lose more conventional fractional distillation process and reduced, biodiesel yield compared with
Conventional fractionation process is high.
Embodiment 4
It is as follows with embodiment 2, concrete technology condition to the operating process that biodiesel crude product is fractionated：
Tower diameter：φ 300mm, tower height：9620mm；Stripping section 11 and rectifying section 13 use stainless steel Pall ring filler, condensing reflux
Section 14 and feedstock vaporisation section 12 use ripple silk net filler.
Biodiesel crude product inlet amount：540kg/h, fatty acid methyl ester component therein account for the 95.8% of inlet amount；Into
The biodiesel crude product quality ratio of one vaporizer 4 and the second vaporizer 5 is 9:1；
Feeding temperature is 85 DEG C；
The tower top temperature of main fractionating tower 1 is 40 DEG C, 0.5~0.8kpa of tower top pressure；
In main fractionating tower 1, the material at the top about 20% of rectifying section 13 is back to tower top as overhead reflux, about 80% after cooling
Material enter treating column 2 carry out lights removal；
In treating column 2, top temperature is 120.2~121.0 DEG C, and pressure be 0.9kpa~1.2kpa, column bottom temperature for 137.5~
138.2 DEG C, pressure is 1.2~1.5kpa.
The two-way circulation of this technique vacuumizes gas, and the part that the tower overhead gas of main fractionating tower 1 introduces the first vaporizer 4 accounts for main point
Evaporate the 1/2 of tower overhead gas；The part that the tower overhead gas for the treatment of column 2 introduces the second vaporizer 5 accounts for the 1/3 of refined tower overhead gas.
Under the operating pressure, the column bottom temperature of realization is 176.5 DEG C, pressure 1.6kPa；Obtained from the bottom of towe for the treatment of column 2
Biodiesel oil product, obtained biodiesel flow are 509.56kg/h, and biodiesel oil product yield is 98.49%, product property
It is shown in Table 4.
Table 4
When as can be seen here, using the operating condition almost identical with conventional fractionation technique, the fractionating column column bottom temperature drop of method
It is low nearly to reduce 66 DEG C, material coking can be avoided completely；The biodiesel that the more conventional fractional distillation process of this method obtains is received
Rate is higher by 16 percentage points, and the energy consumption simply obtained using the vacuum height of this method is higher, it is necessary to adjust product yield and energy
The economic balance point of consumption.
Comparative example 1
Using the biodiesel oil product fractionation process of routine（Feedstock property is shown in Table 1）, tower top vacuumizes, the condensed cooling of tower overhead gas
After carry out gas-liquid separation, the liquid portion isolated is as overhead reflux, partly as biodiesel oil product.Loaded in fractionating column
Stainless steel Pall ring filler, tower diameter：φ 350mm, tower height：7850mm.
Operating condition is as follows：
Inlet amount：540kg/h, fatty acid methyl ester component therein account for the 95.8% of inlet amount；
Feeding temperature is 85 DEG C；
Tower top temperature is 40 DEG C；
0.5~0.8kpa of tower top pressure.
Under the operating pressure, the column bottom temperature of realization is 242.6 DEG C, and obtained biodiesel flow is 424.5kg/h,
Product main character is shown in Table 5, and biodiesel yield is 82.10%.
Table 5
As can be seen here, biodiesel oil product fractionation is carried out using this method, the column bottom temperature of one side fractionating column is higher, can cause
Material coking and lose and influence product quality, under conditions of another aspect condition of high vacuum degree oil gas volatilization lose method, obtained life
Thing production of diesel oil is relatively low.
Claims (11)
1. the product fractionating device of a kind of biodiesel, it is characterised in that the fractionating device includes main fractionating tower（1）With it is refined
Tower（2）, the main fractionating tower 1 is divided into stripping section from bottom to up（11）, feedstock vaporisation section（12）, rectifying section（13）It is and cold
Solidifying reflux section（14）, biodiesel crude product feed pipe（3）The first vaporizer is connected respectively（4）With the second vaporizer（5）, the first vapour
Change device（4）With main fractionating tower（1）The first feed entrance point（6）Connection, the second vaporizer（5）With main fractionating tower（1）Second enter
Discharge position（7）Connection, wherein, the second feed entrance point（7）To being stripping section between bottom of towe（11）, the first feed entrance point（6）With
Two feed entrance points（7）Between be feedstock vaporisation section（12）；Main fractionating tower（1）Top set top of tower gas phase discharge nozzle（15）,
It passes through vaccum-pumping equipment I（8）With the first vaporizer（4）It is connected, main fractionating tower（1）Rectifying section（13）Top sets crude product
Extract line out（16）, crude product extraction line（16）Pass through the reflux condenser of tower top（17）It is connected to main fractionating tower（1）Condensing reflux
Section（14）Top, crude product extract out line（16）Pass through treating column reboiler（22）With treating column（2）Connection, treating column（2）'s
Top sets light component discharge nozzle（21）, it passes through vaccum-pumping equipment II（9）With the second vaporizer（5）It is connected；Main fractionating tower（1）
And treating column（2）Bottom of towe be respectively provided with collection device.
2. fractionating device according to claim 1, it is characterised in that the stripping section（11）Required number of theoretical plate be 2 ~
6 layers, feedstock vaporisation section（12）Required number of theoretical plate is 1 ~ 3 layer, rectifying section（13）Required number of theoretical plate is 5 ~ 12 layers, condensation
Reflux section（14）Required number of theoretical plate is 2 ~ 5 layers.
3. fractionating device according to claim 1, it is characterised in that main fractionating tower（1）And treating column（2）Tower in be tower
Harden structure or filling-material structure.
4. fractionating device according to claim 1, it is characterised in that the main fractionating tower（1）Bottom be also associated with leading
Fractionator Bottom reboiler（18）.
5. the product fractionation process of a kind of biodiesel, it is characterised in that utilize the fractionation described in claim 1 ~ 4 any one
Device, control main fractionating tower（1）The temperature of interior tower top is 40~65 DEG C, and pressure is 0.5kpa~10kpa；Biodiesel crude product leads to
Cross biodiesel crude product feed pipe（3）Respectively enter the first vaporizer（4）With the second vaporizer（5）, through the first vaporizer（4）Vapour
Change the components such as obtained fatty acid methyl ester from the first feed entrance point（6）Into feedstock vaporisation section（12）, introduce rectifying section（13）'s
Bottom, subsequently into rectifying section（13）Realize that rectifying separates；Through the second vaporizer（5）The components such as the fatty acid methyl ester of vaporization are from
Two feed entrance points（7）Into stripping section（11）Top, bottom of towe heavy constituent is carried out after helping vaporization, is also upwardly into rectifying section
（13）Realize separation；In rectifying section（13）, the heavy constituent that carries in the component such as fatty acid methyl ester is condensed separation, isolates restructuring
The fatty acid methyl ester component Parts divided enter reflux condenser（17）Tower top is returned after being cooled down, partly extracts line out from crude product
（16）Pass through treating column reboiler（22）Into treating column（2）；Main fractionating tower（1）The gas part of tower top passes through top of tower gas phase
Discharge nozzle（15）With connected vaccum-pumping equipment I（8）Introduce the first vaporizer（4）；Into treating column（2）Component, then
Light component passes through light component discharge nozzle after boiling（21）, vaccum-pumping equipment II（9）Into the second vaporizer（5）Circulated, refined
Tower（2）The component of bottom of towe is collected, and produces biodiesel finished product；
Wherein, main fractionating tower（1）Tower top introduces the first vaporizer（4）Vacuumize gas and account for main fractionating tower top gas 1/10~1/
2；Treating column（2）The light component at top enters the second vaporizer（5）Gas account for the 1/10~1/2 of refined tower overhead gas.
6. fractionation process according to claim 5, it is characterised in that when biodiesel crude product is fed, introduce the first vaporization
Device（4）With the second vaporizer（5）Mass ratio be 1:1~10：1.
7. fractionation process according to claim 5, it is characterised in that into the first vaporizer（4）Main fractionating tower（1）Tower
Top vacuumizes gas with entering the first vaporizer（4）Biodiesel crude product mass ratio be 1:20~1:100.
8. fractionation process according to claim 5, it is characterised in that main fractionating tower（1）Crude product extract out line（16）In
Main fractionating tower is returned to by condensing reflux（1）The gas at top is with entering treating column（2）Gas mass ratio be 1:5~1：
50。
9. fractionation process according to claim 5, it is characterised in that control charging, make main fractionating tower（1）The restructuring of bottom of towe
Divide the 0.5wt%~5wt% for accounting for biodiesel crude product total feed.
10. fractionation process according to claim 5, it is characterised in that control treating column（2）Tower top temperature for 120~
160 DEG C, pressure is 1.0kpa~15kpa, and column bottom temperature is 140~180 DEG C, and pressure is 2.0~15kpa.
11. fractionation process according to claim 5, it is characterised in that into the second vaporizer（5）Treating column（2）Tower
Top vacuumizes gas with entering the second vaporizer（5）Biodiesel crude product mass ratio be 1:10~1:50.
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