CN108949366A - A kind of ester exchange process and device can be used for producing biodiesel - Google Patents
A kind of ester exchange process and device can be used for producing biodiesel Download PDFInfo
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- CN108949366A CN108949366A CN201810768038.1A CN201810768038A CN108949366A CN 108949366 A CN108949366 A CN 108949366A CN 201810768038 A CN201810768038 A CN 201810768038A CN 108949366 A CN108949366 A CN 108949366A
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- reactor tank
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- methanol
- biodiesel
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
-
- 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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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Liquid Carbonaceous Fuels (AREA)
Abstract
The present invention relates to the synthetic technology of biodiesel, specifically a kind of ester exchange process and device that can produce fatty acid methyl ester.Device is integral type circular response device, including reactor tank body, contact tower, centrifuge and evaporator, contact tower is equipped with above the reactor tank body, bottom is equipped with discharge port, discharge port draws two conveying pipelines respectively, wherein a conveying pipeline is drawn from reactor tank base by discharge port, and being connected to extend at the top of contact tower with material-handling pump connect with conveying spray head；Another conveying pipeline is drawn from reactor tank base by discharge port, is successively connected with product delivery pump, centrifuge and film evaporator.The advantage of the invention is that reactant contact area can be increased, transesterification rate is improved, shortens the reaction time, and do not need methanol condensed device, is generated without exhaust gas waste water, it is pollution-free.
Description
Technical field
The present invention relates to the synthetic technology of biodiesel, specifically a kind of transesterification work that can produce fatty acid methyl ester
Skill and device.
Background technique
With the fast development of world economy, the problems such as energy shortage and environmental pollution for becoming increasingly conspicuous has become various countries must
The global problem that must be faced, presently preferred resolving ideas are to find and develop renewable, environmentally friendly alternative energy source.It is raw
Object biodiesel technology is rapidly developed in this context.
Biodiesel refers to by animal and plant fat (fatty acid triglycercide) and alcohol (methanol or ethyl alcohol) through ester exchange reaction
Obtained fatty acid monoalkyl ester, most typically fatty acid methyl ester.Compared with traditional fossil energy, sulphur and arene content
It is low, Cetane number is high, flash-point is high, have good lubricity, can partially be added in petrifaction diesel.Biodiesel is typical
" green energy resource " greatly develops biodiesel to sustainable economic development, promotes energy substitution, mitigate environmental pressure, control city
City's atmosphere pollution has important strategic importance.China is faced with the insufficient challenge of petroleum resources, and imported crude oil has been more than always to disappear
The 50% of consumption, with the rapid development of economy, the demand to fuel energy also can be increasing.China annual diesel oil at present
Consumption is more than 1.6 hundred million tons, if in petroleum based diesel mixture 5% biodiesel, should form a complete production network biological bavin every year
8,000,000 tons of oil, it is contemplated that future biological diesel product can also account for higher share.
Past produces biodiesel using traditional soda acid two-step method, and wherein acid catalyzed esterification adaptability to raw material is poor, ester
The industrialization key technical problems such as rate is low, the reaction time is long and contaminated wastewater is serious, proposition is using a kind of complete before us
New " esterification-transesterification " two-step method skill combined without catalyst high temperature glycerine esterification with the transesterification process of efficient base catalysis
It is anti-to carry out pre-esterification for art, the i.e. free fatty acid using glycerol under no catalyst high-temperature low-pressure reaction condition and in glyceride stock
It answers, so that glyceride stock is reached the requirement of base catalysis transesterification, and then produce biodiesel.It is carried out after pre-esterification transesterification
Reaction, also referred to as transesterification is the important method of biodiesel synthesis, is that grease and alcohol carry out ester exchange reaction and obtains fatty acid methyl
The process of ester, research base-catalyzed transesterification biodiesel synthesis have important theoretical and practical significance.It is asked existing for this method
Topic is, both methanol and glyceride compatibility are low, and mixed effect is bad, even if under agitation, the two contact is also not enough filled
Point, reaction efficiency is to be improved.
Summary of the invention
In view of grease existing for current ester-interchange method/methanol compatibility, insufficient contact is asked between material caused by low
Topic, it is an object of that present invention to provide ester exchange process and device that one kind can produce fatty acid methyl ester.
To achieve the above object, the invention adopts a technical scheme as:
A kind of transesterification device can be used for producing biodiesel, device are integral type circular response device, including reaction
Device tank body, contact tower, centrifuge and evaporator, the reactor tank body top are equipped with contact tower, and bottom is equipped with discharge port, discharging
Mouth draws two conveying pipelines respectively, wherein a conveying pipeline is drawn from reactor tank base by discharge port, with material-handling pump
It is connected to extend at the top of contact tower and is connect with conveying spray head；Another conveying pipeline is drawn from reactor tank base by discharge port
Out, successively it is connected with product delivery pump, centrifuge and film evaporator.
Feed inlet is equipped at the upper side of the reactor tank body, discharge port is equipped with drain hole valve, the object that discharge port is drawn
Expects pipe distinguishes valve；The materail tube being connected with material-handling pump be equipped with conveying valve, successively with product delivery pump, centrifuge and
The connected materail tube of film evaporator is equipped with product valve.
The film evaporator is the first film evaporator of methanol removal and the second film evaporator of distillation.
A kind of ester exchange process method using described device production biodiesel, glyceride and methanol, sodium methoxide is molten
Liquid is sent into mixing in reactor tank body, and heating makes methanol boil, send material to reactor tank body in the case where conveying pumping action
Tower top is contacted, material is sprayed from the top down along contact tower by spray head, is sufficiently mixed with gaseous methanol；After reaction, from out
Product is released to centrifuge by material mouth, is centrifugated thick methyl esters phase and raw glycerin phase, and thick methyl esters mutually steams after dealcoholation treatment again
It evaporates to get biodiesel.
Glyceride is sent into reactor tank body and is mixed with methanol, sodium methoxide solution, is heated at 70-80 DEG C, boils methanol
It rises, opening discharge port makes glyceride and sodium methoxide solution be pumped to reactor tank body overlying contact tower top by conveying, and material is logical
It crosses spray head and is sprayed from the top down along contact tower, is sufficiently mixed with gaseous methanol, react 1-3h；Product is from discharging after transesterification
Mouth enters centrifuge by delivery pump, is centrifuged off catalyst and bottom glycerol is centrifugated thick methyl esters phase and raw glycerin phase, slightly
Methyl esters mutually after dealcoholation treatment redistillation to get biodiesel.
The glyceride is the grease for being lower than 4mgKOH/g by pre-esterification treated waste grease or acid value；Glycerol
The molar ratio of ester and methanol is 1:4-9；Sodium methoxide quality is the 0.8%-1.2% of glyceride quality.
The centrifugation obtains thick methyl esters mutually successively by the first film evaporator of methanol removal and the evaporation of the second film of distillation
Device realizes dealcoholysis and distillation；Wherein, the condition of methanol removal is pressure 0.1-1mbar, temperature is 60-70 DEG C, the time；After dealcoholysis
Redistillation can be obtained the fat of purity 99.5-99.9% under the conditions of pressure is 0.01-0.1mbar, temperature is 150-180 DEG C
Sour methyl esters product.
The present invention having the advantage that compared with prior art
Apparatus of the present invention greatly increase two-phase contact area and then improve ester exchange reaction efficiency, using the method for the present invention
Raw materials glycerine ester and methanol can be significantly improved because compatibility is bad and the deficiency of insufficient contact, make the two gas-liquid two-phase
It is sufficiently mixed, increases contact area, improve ester exchange rate, be not necessarily to condensing unit, and it is pollution-free not generate exhaust gas waste water；In addition
The methyl esters that transesterification obtains mutually is carried out except alcohol, distilation, the available higher fatty acid of purity using film evaporation method
Methyl esters.
Detailed description of the invention
Fig. 1 is ester exchange process device figure of the present invention, in which: 1, reactor tank body, 2, contact tower, and 3, conveying spray head, 4,
Material dehvery pump, 5, product dehvery pump, 6, centrifuge, 7, the first film evaporator, the 8, second thin film evaporator, 9, feed inlet,
10, drain hole valve, 11, conveying valve, 12, product valve.
Specific embodiment
The present invention will be further explained with reference to the accompanying drawings and examples explanation, but the present invention be not limited in it is as follows
Embodiment.
Glyceride and methanol, sodium methoxide solution are sent into Hybrid Heating in reaction unit by the present invention, so that methanol is boiled, defeated
It send and send mixed material to contact tower top to reaction unit from reaction unit bottom under pumping action, material is by spray head along connecing
Touching tower sprays from the top down, is sufficiently mixed with gaseous methanol；After reaction, it is released to centrifuge from discharge port by material, from
Heart separation methyl esters phase and glycerol phase, methyl esters are mutually sent into thin film evaporator, and first dealcoholysis redistillation obtains biodiesel.In the technique
Reaction unit used in Exchange Ester Process be integral type recirculation reactor, including reactor tank body, contact tower, feed inlet, discharge port,
Delivery pump, conveying pipeline, conveying spray head, contact tower are located above reactor tank body, and conveying pipeline is drawn from reactor bottom, and process is defeated
It send pump to extend at the top of contact tower and is connect with conveying spray head.The advantage of the invention is that reactant contact area can be increased,
Transesterification rate is improved, shortens the reaction time, and do not need methanol condensed device, is generated without exhaust gas waste water, it is pollution-free.
Embodiment 1
Device is integral type circular response device, including reactor tank body 1, contact tower 2, centrifuge 6 and evaporator are described
Contact tower 2 is equipped with above reactor tank body 1, bottom is equipped with discharge port, and discharge port draws two conveying pipelines respectively, wherein one defeated
Expects pipe is drawn from reactor tank base by discharge port, is connected to extend at the top of contact tower with material-handling pump 4 and be sprayed with conveying
First 3 connection；Another conveying pipeline is drawn from reactor tank base by discharge port, successively with product delivery pump 5, centrifuge 6 and
Film evaporator is connected.
Feed inlet is equipped at the upper side of the reactor tank body, discharge port is equipped with drain hole valve 10, what discharge port was drawn
Materail tube is respectively equipped with conveying valve 11 and product valve 12.
The film evaporator is the second film evaporator 8 of the first film evaporator 7 and distillation of methanol removal.
Embodiment 2
50kg glyceride is mixed (molar ratio 1:6) with 10.9kg methanol, and 0.5kg sodium methoxide catalyst (glycerol is added
The 1% of ester quality), it is added in reactor tank body, 70 DEG C of heating make methanol boil.Drain hole valve and conveying valve are opened,
And open material dehvery pump and transport material to contact tower top, it is sprayed from top to bottom by conveying spray head along contact tower, with methanol
Steam is sufficiently mixed, and reacts 1.3h.After reaction, product valve is opened, product dehvery pump is opened and conveys product after reaction
To centrifuge, it is centrifugated thick methyl esters phase and raw glycerin phase；Thick methyl esters is mutually delivered to first order thin film evaporator, presses in 1mbar
Lower 68 DEG C of power are sloughed methanol, are delivered to second level thin film evaporator again after dealcoholysis, are distilled, obtain at 0.05mbar pressure, 160 DEG C
Obtain the biodiesel oil product 45.3kg that purity is 99.8%.
Embodiment 3
50kg glyceride is mixed (molar ratio 1:8) with 14.5kg methanol, and 0.55kg sodium methoxide catalyst (glycerol is added
The 1.1% of ester quality), it is added in reactor tank body, 74 DEG C of heating make methanol boil.Open drain hole valve and feeding valve
Door, and open material dehvery pump and transport material to contact tower top, it is sprayed from top to bottom by conveying spray head along contact tower, with first
Alcohol steam is sufficiently mixed, and reacts 2.8h.After reaction, product valve is opened, dehvery pump is opened and is delivered to reacting rear material
Centrifuge is centrifugated thick methyl esters phase and raw glycerin phase；Thick methyl esters is mutually delivered to first order thin film evaporator, presses in 0.5mbar
Lower 66 DEG C of power are sloughed methanol, are delivered to second level thin film evaporator again after dealcoholysis, are distilled, obtain at 0.02mbar pressure, 155 DEG C
Obtain the biodiesel oil product 44.9kg that purity is 99.5%.
Embodiment 4
50kg glyceride is mixed (molar ratio 1:5) with 9kg methanol, and 0.45kg sodium methoxide catalyst (glyceride is added
The 0.9% of quality), it is added in reactor tank body, 78 DEG C of heating make methanol boil.Drain hole valve and conveying valve are opened,
And open material dehvery pump and transport material to contact tower top, it is sprayed from top to bottom by conveying spray head along contact tower, with methanol
Steam is sufficiently mixed, and reacts 2h.After reaction, product valve is opened, product dehvery pump is opened and is delivered to reacting rear material
Centrifuge is centrifugated thick methyl esters phase and raw glycerin phase；Thick methyl esters is mutually delivered to first order thin film evaporator, presses in 0.2mbar
Lower 62 DEG C of power are sloughed methanol, are delivered to second level thin film evaporator again after dealcoholysis, are distilled, obtain at 0.09mbar pressure, 178 DEG C
Obtain the biodiesel oil product 46.2kg that purity is 99.7%.
Claims (7)
1. a kind of transesterification device that can be used for producing biodiesel, it is characterised in that: device is integral type circular response device,
Including reactor tank body, contact tower, centrifuge and evaporator, contact tower is equipped with above the reactor tank body, bottom is equipped with
Material mouth, discharge port draw two conveying pipelines respectively, wherein a conveying pipeline is drawn from reactor tank base by discharge port, with object
Material conveying pump is connected to extend at the top of contact tower to be connect with conveying spray head；Another conveying pipeline is from reactor tank base by going out
Material mouth is drawn, and is successively connected with product delivery pump, centrifuge and film evaporator.
2. the transesterification device according to claim 1 that can be used for producing biodiesel, it is characterised in that: the reactor tank
Feed inlet is equipped at the upper side of body, discharge port is equipped with drain hole valve, and the materail tube that discharge port is drawn is respectively equipped with valve.
3. the transesterification device according to claim 1 that can be used for producing biodiesel, it is characterised in that: the film evaporator
For the first film evaporator of methanol removal and the second film evaporator of distillation.
4. a kind of ester exchange process method using claim 1 described device production biodiesel, it is characterised in that: by glycerol
Ester is sent into reactor tank body and is mixed with methanol, sodium methoxide solution, heats, so that methanol is boiled, in the case where conveying pumping action by material
It send to reactor tank body overlying contact tower top, material is sprayed by spray head along contact tower from the top down, sufficiently mixed with gaseous methanol
It closes；After reaction, it is released to centrifuge from discharge port by product, is centrifugated thick methyl esters phase and raw glycerin phase, thick methyl esters phase
Redistillation is after dealcoholation treatment to get biodiesel.
5. the ester exchange process method of production biodiesel according to claim 4, it is characterised in that: by glyceride and first
Alcohol, sodium methoxide solution are sent into mixing in reactor tank body, heat at 70-80 DEG C, methanol is made to boil, and opening discharge port makes glyceride
Reactor tank body overlying contact tower top is pumped to by conveying with sodium methoxide solution, material by spray head along contact tower from the top down
It sprays, is sufficiently mixed with gaseous methanol, react 1-3h；Product enters centrifugation by delivery pump from discharge port after transesterification
Machine, is centrifuged off catalyst and bottom glycerol is centrifugated thick methyl esters phase and raw glycerin phase, and thick methyl esters is mutually after dealcoholation treatment
Redistillation is to get biodiesel.
6. by the ester exchange process method of production biodiesel described in claim 4 or 5, it is characterised in that: the glyceride
It is the grease for being lower than 4mgKOH/g by pre-esterification treated waste grease or acid value；The molar ratio of glyceride and methanol is
1:4-9；Sodium methoxide quality is the 0.8%-1.2% of glyceride quality.
7. by the ester exchange process method of production biodiesel described in claim 4 or 5, it is characterised in that: the centrifugation obtains
Thick methyl esters is obtained mutually successively by the first film evaporator of methanol removal and the realization dealcoholysis of the second film evaporator of distillation and distillation；Its
In, the condition of methanol removal is pressure 0.1-1mbar, temperature is 60-70 DEG C, the time；After dealcoholysis in pressure be 0.01-
Redistillation can be obtained the fatty acid methyl ester product of purity 99.5-99.9% under the conditions of 0.1mbar, temperature are 150-180 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810768038.1A CN108949366A (en) | 2018-07-13 | 2018-07-13 | A kind of ester exchange process and device can be used for producing biodiesel |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810768038.1A CN108949366A (en) | 2018-07-13 | 2018-07-13 | A kind of ester exchange process and device can be used for producing biodiesel |
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| CN201810768038.1A Pending CN108949366A (en) | 2018-07-13 | 2018-07-13 | A kind of ester exchange process and device can be used for producing biodiesel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574826A (en) * | 2020-11-21 | 2021-03-30 | 贵州锦江生物能源科技有限公司 | Device and method for preparing fatty acid methyl ester by continuous ester exchange |
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| CN101805673A (en) * | 2010-04-01 | 2010-08-18 | 江苏大学 | Airlifting biodiesel ester exchange reactor |
| CN101921631A (en) * | 2009-06-15 | 2010-12-22 | 尉氏县挺凯植物胶化工厂有限公司 | Production method of biodiesel |
| JP2014122317A (en) * | 2012-12-23 | 2014-07-03 | Chube Univ | Biodiesel fuel production system and biodiesel fuel production method |
| CN104031747A (en) * | 2014-06-13 | 2014-09-10 | 太原理工大学 | Production device and method of biodiesel |
| CN204607961U (en) * | 2015-04-28 | 2015-09-02 | 广东河山环保有限公司 | A kind of reaction unit manufacturing biofuel |
| CN106190591A (en) * | 2015-08-27 | 2016-12-07 | 上海中器环保科技有限公司 | The esterification of a kind of biodiesel, ester exchange reaction method |
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2018
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101921631A (en) * | 2009-06-15 | 2010-12-22 | 尉氏县挺凯植物胶化工厂有限公司 | Production method of biodiesel |
| CN101805673A (en) * | 2010-04-01 | 2010-08-18 | 江苏大学 | Airlifting biodiesel ester exchange reactor |
| JP2014122317A (en) * | 2012-12-23 | 2014-07-03 | Chube Univ | Biodiesel fuel production system and biodiesel fuel production method |
| CN104031747A (en) * | 2014-06-13 | 2014-09-10 | 太原理工大学 | Production device and method of biodiesel |
| CN204607961U (en) * | 2015-04-28 | 2015-09-02 | 广东河山环保有限公司 | A kind of reaction unit manufacturing biofuel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574826A (en) * | 2020-11-21 | 2021-03-30 | 贵州锦江生物能源科技有限公司 | Device and method for preparing fatty acid methyl ester by continuous ester exchange |
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Application publication date: 20181207 |