CN106479683A - A kind of apparatus and method preparing biodiesel - Google Patents
A kind of apparatus and method preparing biodiesel Download PDFInfo
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- CN106479683A CN106479683A CN201510526956.XA CN201510526956A CN106479683A CN 106479683 A CN106479683 A CN 106479683A CN 201510526956 A CN201510526956 A CN 201510526956A CN 106479683 A CN106479683 A CN 106479683A
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000003225 biodiesel Substances 0.000 title claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000003921 oil Substances 0.000 claims abstract description 28
- 235000014593 oils and fats Nutrition 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 125000004185 ester group Chemical group 0.000 claims abstract description 8
- 238000004062 sedimentation Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 7
- 150000002148 esters Chemical class 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000004519 grease Substances 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 238000007701 flash-distillation Methods 0.000 claims description 5
- 230000020477 pH reduction Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000012043 crude product Substances 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 50
- 235000019198 oils Nutrition 0.000 description 23
- 239000002994 raw material Substances 0.000 description 13
- 230000008569 process Effects 0.000 description 10
- 241000196324 Embryophyta Species 0.000 description 5
- 235000011187 glycerol Nutrition 0.000 description 5
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 description 4
- 239000008158 vegetable oil Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 239000002283 diesel fuel Substances 0.000 description 3
- -1 fatty acid ester Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000006136 alcoholysis reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 208000012839 conversion disease Diseases 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 2
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
Classifications
-
- 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
Landscapes
- Liquid Carbonaceous Fuels (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention provides a kind of production method of biodiesel, including：(1) by oils and fatss and alcohol extraction supplied reactor, carry out ester exchange reaction；(2) by reactor, reacting coarse product entrance heat exchanger out carries out heat exchange cooling, and the locus of heat exchanger are significantly higher than the lowest part of reactor and heat exchanger connecting pipeline；(3) obtain biodiesel after the reacting coarse product after heat exchanger heat exchange is separated；(4) lowest part in reactor lower part and/or reactor and heat exchanger connecting pipeline arranges settling tank, is dissolved in impurity sedimentation in oil in settling tank.Present invention also offers the device of preparation biodiesel.The inventive method can extension fixture continuous operation time.
Description
Technical field
The present invention relates to one kind prepares fatty acid ester (i.e. biological bavin by oils and fatss and monohydric alcohol reaction
Oil) apparatus and method.
Background technology
Biodiesel can carry out ester exchange reaction by oils and fatss and methanol and be obtained, and ester exchange reaction refers to
Be triglyceride and another kind of alcohol (usually low-carbon alcohols, such as C1- C8Monohydric alcohol) enter
The reaction of row.There is fatty acid ester, i.e. biodiesel, monoglyceride, two sweet in its product
Ester, glycerol, alcohol and triglyceride are raw material.
Chinese patent application 2014102611461 discloses a kind of process units of biodiesel
And production method, process units includes tower reactor integrated apparatus and rectifying column, flash column, separation
Tower；Production method includes：Oils and fatss are anti-with gas-phase methanol counter current contacting down through catalyst reaction layer
Should, unreacted methanol recycles, and product enters to be layered kettle further through temperature raising sulfate layer flows downhill
Isolate polarity and crude oil product, after rectification or separating-purifying, obtain biodiesel.
Chinese patent application 2014101989410 discloses supercritical catalyst method and continuously prepares life
The method of thing diesel oil, carries out continuous prodution using solid catalyst fixed bed type reactor biological
Diesel oil.Ester exchange reaction is in temperature 260-330 DEG C, pressure 10-19MPa, molar ratio of methanol to oil
35：1-70：1, product accesses in gas-liquid separator and carries out initial gross separation, upper strata Methanol Recovery
It is coarse biodiesel and crude glycerine using, middle level and lower floor, each subsequently refined respectively,
Coarse biodiesel obtains biodiesel after refining.
CN101935593B discloses Supercritical methanol continuous processing and prepares biodiesel
Method and device, methanol, oils and fatss are 24: 1-42: 1 dozen in molar ratio by dosing pump respectively
Enter static mixer, through static mixer mixing, enter to surpass in methanol in tubular reactor and face
Reacted under boundary's state, temperature controlling range is 240-320 DEG C, pressure control range is
15-20Mpa, time control scope is 4-15min；Enter gas-liquid separator separates afterwards,
Gas-liquid separator upper strata gas phase is methanol；Gas-liquid separator middle level is coarse biodiesel, coarse biometric
It is biodiesel that diesel oil removes rectifying column vacuum fractionation, rectifying column tower top and side line, rectifying tower bottom
For fuel oil.
Chinese patent application 2013105982242 is disclosed a kind of coal-based methanol and is surpassed with Petiolus Trachycarpi oil
Critical method prepares the method and device of biodiesel.The present invention is continuous with Petiolus Trachycarpi oil by coal-based methanol
Send into preheater, mixing preheating, be then fed into tubular reactor, make coal-based methanol in supercritical
Carry out ester exchange reaction, product enters gas-liquid separation after air relief valve decompression under state
Device, is divided into coarse biodiesel and crude carbinol；Coarse biodiesel feeding vacuum rectification tower is carried out essence
Evaporate and obtain biodiesel and residual oil.
Be can be seen that by above-mentioned：Biodiesel preparation generally adopts high temperature, the continuity method of high pressure,
Economically consider, most of raw material is the leftover bits and pieces during waste grease or oil refinery
Or hair vegetable oil, this quasi-grease general acid number height, meanwhile, containing substantial amounts of organic and inorganic miscellaneous
Matter, is being esterified or during ester exchange reaction, is being prolonged with the device duration of runs using this kind of raw material
Long, the heat exchange efficiency of heat exchanger declines, and the resistance drop of reactor increases, and makes device cannot grow week
Phase stable operation.
Content of the invention
The present invention provides a kind of device preparing biodiesel.
The present invention also provides a kind of Process preparing biodiesel, and the method can extension fixture connect
The continuous duration of runs.
The device of the preparation biodiesel that the present invention provides, including：
(1) reactor 1；
(2) heat exchanger 2, the locus of heat exchanger are significantly higher than reactor with heat exchanger even
The lowest part of adapter line；
(3) connecting pipeline 3 of reactor outlet and heat exchanger entrance, and reactor inlet
Connecting pipeline 4 with heat exchanger exit；
(4) settling tank 5, the position of settling tank is located at reactor lower part and/or pipeline 3 He
/ or pipeline 4 lowest part.
(5) feedstock pipeline 6 and feedstock pipeline 7；
(6) crude product discharging pipeline 8.
According to device of the present invention, heat exchanger should be placed in the higher position of device, for example, changes
The position of hot device should be significantly higher than the lowest part of connecting pipeline in device, and described lowest part is permissible
One section of horizontal pipeline being in minimum point can also be the minimum point of pipeline.
According to device of the present invention, settling tank is placed on device compared with low spot or minimum point as far as possible,
The position of such as settling tank can be located at the company of reactor lower part, reactor outlet and heat exchanger entrance
The lowest part of adapter line, and/or reactor inlet is minimum with the connecting pipeline of heat exchanger exit
Place, can all there be settling tank these three positions at optionally wherein one, at two or at three at best three.
Settling tank quantity can be one or more, preferably two, can switch between two.
According to device of the present invention, reaction raw materials can be directly entered reaction by feeding line 7
Device 1, also can be introduced into heat exchanger 2 through pipeline 6 and preheat, enter instead through pipeline 4 after preheating
Device 1 is answered to be reacted.
According to device of the present invention, pipeline 3 and 4 at least or one section of low spot can be used to
Setting settling tank, after leaving the low spot at settling tank place, pipeline 3 and 4 can extend upwardly to
Reactor or heat exchanger entrance, also can first extend upwardly to peak, still further below with reactor or
Heat exchanger entrance is connected, and wherein the position of peak can be higher than, be equal to or less than reactor and change
The high point of hot device, in this case, the material time of staying in a device is longer, contributes to
The abundant sedimentation of impurity.
The method of the preparation biodiesel that the present invention provides comprises the following steps：
(1) oils and fatss and monohydric alcohol are supplied to reactor, carry out ester exchange reaction；
(2) by reactor, reacting coarse product entrance heat exchanger out carries out heat exchange cooling, changes
The locus of hot device are significantly higher than the lowest part of reactor and heat exchanger connecting pipeline；
(3) obtain biodiesel after the reacting coarse product after heat exchanger heat exchange is separated；
(4) minimum in reactor lower part and/or reactor and heat exchanger connecting pipeline
Place's setting settling tank, the impurity sedimentation isolated from oil is in settling tank.
According to the method for the invention, react front or reacted material and occur deposition right in entrance
Before the influential equipment of function (as reactor or heat exchanger etc.), it is both needed to first pass around and is arranged on
The settling tank of device low spot, makes impurity sedimentation.
According to the method for the invention, heat exchanger should be placed in the higher position of device, for example, changes
The position of hot device should be significantly higher than the low spot of connecting pipeline and minimum point in device.
According to the method for the invention, settling tank is placed on device minimum point as far as possible, for example, settle
The position of tank can be located at the connecting pipeline of reactor lower part, reactor outlet and heat exchanger entrance
Lowest part, or the connecting pipeline lowest part of reactor inlet and heat exchanger exit, these three positions
Putting can be at optionally wherein one, at two or at three.Settling tank quantity can be one or more, best
For two, can switch between two.Two settling tanks in plant running can one open one standby,
Peace and quiet empty settling tank need to be pressurized to after system pressure the system that is incorporated to during switching, reduce device
Fluctuation.
Described oils and fatss are triglycerides, are mainly derived from animal oil or vegetable oil, Ke Yishi
High acid value and high impurity grease, for example various refined oils, unrefined oil (hair vegetable oil), useless
Abandon oils and fatss, acidification oil etc., acid number can change in the larger context, for example, it may be
0-130mgKOH/g, preferably soybean oil, Oleum Brassicae campestriss, Oleum Gossypii semen, Oleum Cocois, Petiolus Trachycarpi oil etc.
Refined plant oil.
Described monohydric alcohol refers to the fatty alcohol that carbon number is 1～6, can be single fatty alcohol,
Can also be the mixture of one or more fatty alcohol, preferably methanol and/or ethanol.
The preferred tubular reactor of described reactor.Oils and fatss and alcohol can be provided independently to reactor, or
It is supplied to reactor by after their premixings.Before being supplied to reactor, preferably use heat exchanger
Material is preheated, so, heat exchanger had both played the effect of preheater, also functioned to the work of reactor
With.As using preheating by the way of, after oils and fatss being preheated respectively or mix with alcohol together with preheat.
170-350 DEG C of temperature of reactor, best 220-300 DEG C, pressure 4-12MPa, best
5-10MPa, alcohol/molar equivalent is 3-60：1, preferably 4-12：1.Liquid hourly space velocity (LHSV) is
0.1～2h-1.Under these conditions, whole thing system or one of oils and fatss and alcohol material can be located
In supercriticality it is also possible to be near critical state.
Temperature raises and is conducive to improving reaction conversion ratio, but when temperature is too high, product color
Black, have burnt matter to produce.Therefore, temperature is maintained at 170-350 DEG C, best 220-320 DEG C
It is advisable.
Pressure is higher more favourable to reaction, but pressure is too high, makes investment and the operating cost of device
Improve more, so, pressure should be in 4.0-12MPa, and best 5-10MPa is advisable.
The reaction generating fatty acid ester is reversible balancing response, for improving the conversion ratio of grease, fits
When improving alcohol/molar equivalent, balance can be made to move to product direction, but improve alcohol/molar equivalent
Make material shorter residence time in the reactor, conversion ratio declines, and also makes plant energy consumption and operation
Expense increases, and so that the utilization rate of equipment is declined.So, alcohol/molar equivalent is maintained at 3-60：1,
Preferably 4-12：1.
Reacting coarse product after heat exchanger heat exchange leaves compression system, can first pass through flash distillation and steam
Monohydric alcohol, under conditions of flash distillation can be in 150 DEG C of ＜, more than an atmospheric pressure, normal pressure or vacuum
Carry out.Mixed ester phase and the separation of glycerol phase are carried out to the mixture after flash distillation monohydric alcohol, then
Mixed methyl phase and glycerol are distilled respectively, can get the higher biodiesel of purity and sweet
Oil.
Present inventor is had been surprisingly found that by many experiments：The reaction of oils and fatss and alcohol be one anti-
Should with separate (sedimentation) simultaneous process, after oils and fatss contact with alcohol, except by be esterified,
Ester exchange reaction generates outside biodiesel, other side reactions also occurs, makes to be originally dissolved in oil
Impurity (as metal, phosphorus etc.) in fat is separated from oils and fatss and is settled, precipitum
Amount experiences the rising of temperature with material and increases, and sedimentation can occur laggard anti-in oil plant and alcohol mixing
Before answering device, in the reactor and material go out reactor after flow process in, this will lead to
Pipe blocking, device resistance fall increase, device cannot stable operation, heat exchanger heat transfer be deteriorated,
Raw material cannot be preheated to reaction temperature, affects continuously running of device.
The present invention passes through at the low spot of reactor lower part and heat exchanger and reactor connecting pipeline
Set up settling tank, so that deposit in reactor and heat exchanger is substantially reduced, reactor and heat exchanger
Frequency of removing contamination substantially reduce, extend device continuous operation time.
The manufacturer of biodiesel solves reactor and the method for heat exchanger deposition at present is to tear open
Opening apparatus clean, and change damaged parts simultaneously, dismount a somewhat expensive, also want stop work and production.
The present invention solves the technical barrier of puzzlement those skilled in the art, and method is practical, effect is significant, greatly
Width improves device operation efficiency, is that enterprise brings notable benefit.
The present invention is respectively provided with pervasive to various refined oils and unrefined oil, waste grease, acidification oil
Property, even if adopting high acid value, the raw material of high impurity, also capable of direct processing, save operation
Numerous and diverse pretreatment, makes energy consumption, equipment investment decline.
According to the present invention provide method, reaction conversion ratio up to 95%, even more high, fat
Fatty acid monoester purity is up to more than 99.0%.
The basic three-waste free discharge of this technique, is an eco-friendly friendly process, and environment is protected
Shield is favourable.
The present invention may also apply to the low serialization biodiesel preparation flow of temperature, pressure.
Brief description
Fig. 1 is the schematic diagram of some embodiments of the present invention, does not represent whole realities of the present invention
Apply mode.
(1) raw oil material and monohydric alcohol enter reactor 1, carry out ester exchange reaction.Reaction
Raw material can be directly entered reactor 1 by feeding line 7, may also pass through pipeline 6 and be introduced into and change
Hot device 2 preheats, and enters reactor reaction through pipeline 4 after preheating；
(2) by reactor 1, reacting coarse product out enters heat exchanger 2 through pipeline 3 and changes
Heat drop temperature, the locus of heat exchanger should be significantly higher than reactor with heat exchanger connecting pipeline
Lower；
(3) reacting coarse product after heat exchanger 2 heat exchange leave compression system separated after
To biodiesel；
(4) in reactor 1 bottom and/or reactor 1 outlet and heat exchanger 2 entrance
Connecting pipeline 3, and the connecting pipeline 4 of reactor 1 entrance and heat exchanger 2 outlet is
Lower arranges settling tank 5, is dissolved in impurity sedimentation in oil in settling tank.
Specific embodiment
Further illustrate the present invention below by example, but the present invention is not limited to this.
Embodiment 1
Carry out alcoholysis process of pressurizeing according to Fig. 1 flow process, by the hair plant of acid number 7mgKOH/g
, respectively with 600 Grams Per Hours, the speed of 152 Grams Per Hours provides high pressure heat exchanger for oil and methanol
In 2, the material after heating is continuously provided in tubular reactor 1, in reactor
258 DEG C of temperature, pressure 5MPa, the connecting pipeline that reactor 1 entrance is exported with heat exchanger 2
4 lowest part setting settling tank 5, reactor 1 bottom installs settling tank 5, outflow reactor additional
After high pressure heat exchanger 2 heat exchange, reacting coarse product enters flash column to material, and in ＜, 150 DEG C are removed
Remove methanol, and methanol carried out reclaiming, reuses, leftover materials carry out settlement separate, point
Ester output phase and glycerol phase, ester phase enters membrane evaporator, in pressure 6mmHg, 240 DEG C of temperature
Under conditions of, steam the yield 94% of biodiesel.Reaction unit runs 2 months, opens
Reactor lower part deposit height about 4cm is found after reactor.
Comparative example 1
Using 1 mao of vegetable oil of embodiment as raw material, it is under reactor 1 with embodiment 1 difference
Portion does not install settling tank 5 additional, and the raw material after heat exchanger heat exchange do not pass through along pipeline 4 U-shaped
Curved be directly entered reactor lower part, the lowest part of connecting pipeline 4 does not install settling tank 5 additional, and real
Apply the raw material after example 1 heat exchange to bend into into reactor lower part along pipeline 4 by U-shaped, and U
The curved lowest part of type installs settling tank 5 additional.Other same as Example 1, through same reaction conditions fortune
After row 2 months, after opening reactor, find reactor 1 bottom deposit height about 10cm,
Now reactor inlet and outlet pressure difference substantially rises, reaction unit cannot even running, biological bavin
The yield of oil drops to 76%.
Embodiment 2
Carry out alcoholysis process of pressurizeing, 240 DEG C of temperature of reactor, pressure according to Fig. 1 flow process
7MPa, temperature, acid number 91mgKOH/g acidification oil and the first required for reaching reaction as early as possible
Respectively with 600 Grams Per Hours, the speed of 139 Grams Per Hours provides in high pressure heat exchanger 2 alcohol,
Connecting pipeline 3 lowest part of reactor 1 outlet and heat exchanger 2 entrance installs settling tank 5 additional, instead
Answer plant running 1 month, raw material still can reach through high pressure heat exchanger 2 temperature after heating
237℃.
Comparative example 2
Using embodiment 2 acidification oil as raw material, it is reacting coarse product along pipe with embodiment 2 difference
Line 3 do not pass through U-shaped curved be directly entered heat exchanger, wherein, connecting pipeline 3 lowest part does not add
Dress settling tank, and embodiment 2 reacting coarse product bends into into heat exchanger along pipeline 3 by U-shaped,
Install settling tank in U-shaped curved lowest part additional, other same as Example 2, through same reaction bar
After part runs 1 month, because the wall of high pressure heat exchanger has deposit to adhere to, heat exchange efficiency is bright
Aobvious decline, raw material can only achieve 190 DEG C through high pressure heat exchanger 2 temperature after heating.
Claims (12)
1. a kind of device preparing biodiesel, including：
(1) reactor 1；
(2) heat exchanger 2, the locus of heat exchanger are significantly higher than reactor and heat exchanger connecting tube
The lowest part of line；
(3) connecting pipeline 3 of reactor outlet and heat exchanger entrance, and reactor inlet with change
The connecting pipeline 4 of hot device outlet；
(4) settling tank 5, the position of settling tank is located at reactor lower part and/or pipeline 3 and/or pipe
The lowest part of line 4；
(5) feedstock pipeline 6 and feedstock pipeline 7；
(6) crude product discharging pipeline 8.
2. according to the device described in claim 1, wherein, settling tank quantity is one or more.
3. according to the device described in claim 1, wherein, pipeline 3 and 4 at least one or one
Section low spot, after leaving low spot, pipeline 3 and 4 extends upwardly to reactor or heat exchanger
Entrance, or first extend upwardly to peak, still further below with reactor or heat exchanger entrance phase
Even, wherein the position of peak can be higher than, be equal to or less than the height of reactor and heat exchanger
Point.
4. a kind of method preparing biodiesel, comprises the following steps：
(1) oils and fatss and monohydric alcohol are supplied to reactor, carry out ester exchange reaction；
(2) by reactor, reacting coarse product entrance heat exchanger out carries out heat exchange cooling, heat exchanger
Locus be higher than reactor and heat exchanger connecting pipeline lowest part；
(3) obtain biodiesel after the reacting coarse product after heat exchanger heat exchange is separated；
(4) set with the lowest part of heat exchanger connecting pipeline in reactor lower part and/or reactor
Put settling tank, the impurity sedimentation isolated from oil is in settling tank.
5. according to the method described in claim 4, wherein, oils and fatss and monohydric alcohol are being supplied to reaction
Before device, with heat exchanger, material is preheated.
6. according to the method described in claim 4, wherein, described oils and fatss are selected from refined oil, non-
Refined oil, waste grease or acidification oil, acid number is 0-130mgKOH/g.
7. according to the method described in claim 4, wherein, described monohydric alcohol refer to carbon number be 1～
6 fatty alcohol.
8. according to the method described in claim 4, wherein, described reactor is tubular reactor.
9. according to the method described in claim 4, wherein, 170-350 DEG C of temperature of reactor, pressure
Power 4-12MPa.
10. according to the method described in claim 4, wherein, 220-300 DEG C of temperature of reactor,
Pressure 5-10MPa.
11. according to the method described in claim 4, and wherein, alcohol/molar equivalent is 3-60：1,
Liquid hourly space velocity (LHSV) is 0.1～2h-1.
12. according to the method described in claim 4, and wherein, the reaction after heat exchanger heat exchange is thick
Product leaves compression system, first passes through flash distillation, steams monohydric alcohol, then to flash distillation unitary
Mixture after alcohol carries out mixed ester phase and the separation of glycerol phase, then to mixed methyl
Mutually distilled respectively with glycerol, obtained the higher biodiesel of purity and glycerol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108929787A (en) * | 2017-05-27 | 2018-12-04 | 中国石油化工股份有限公司 | Tubular type-alternating temperature continuity method preparation biodiesel method and system |
| CN108929785A (en) * | 2017-05-27 | 2018-12-04 | 中国石油化工股份有限公司 | Alternating temperature-continuity method preparation biodiesel method and system |
| CN108949365A (en) * | 2017-05-27 | 2018-12-07 | 中国石油化工股份有限公司 | Alternating temperature-transformation continuity method preparation biodiesel method and system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102477357A (en) * | 2010-11-25 | 2012-05-30 | 中国石油化工股份有限公司 | Method for preparing biodiesel |
| CN102533455A (en) * | 2012-01-18 | 2012-07-04 | 山东锦江生物能源科技有限公司 | Method for preparing biodiesel from oil with high acid value |
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2015
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102477357A (en) * | 2010-11-25 | 2012-05-30 | 中国石油化工股份有限公司 | Method for preparing biodiesel |
| CN102533455A (en) * | 2012-01-18 | 2012-07-04 | 山东锦江生物能源科技有限公司 | Method for preparing biodiesel from oil with high acid value |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108929787A (en) * | 2017-05-27 | 2018-12-04 | 中国石油化工股份有限公司 | Tubular type-alternating temperature continuity method preparation biodiesel method and system |
| CN108929785A (en) * | 2017-05-27 | 2018-12-04 | 中国石油化工股份有限公司 | Alternating temperature-continuity method preparation biodiesel method and system |
| CN108949365A (en) * | 2017-05-27 | 2018-12-07 | 中国石油化工股份有限公司 | Alternating temperature-transformation continuity method preparation biodiesel method and system |
| CN108929785B (en) * | 2017-05-27 | 2021-10-08 | 中国石油化工股份有限公司 | Method and system for preparing biodiesel by variable-temperature-continuous method |
| CN108929787B (en) * | 2017-05-27 | 2021-10-08 | 中国石油化工股份有限公司 | Method and system for preparing biodiesel by tubular-temperature-variable continuous method |
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