CN106800976A - A kind of method that glycerine round-robin method continous way prepares biodiesel - Google Patents
A kind of method that glycerine round-robin method continous way prepares biodiesel Download PDFInfo
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- CN106800976A CN106800976A CN201710022520.6A CN201710022520A CN106800976A CN 106800976 A CN106800976 A CN 106800976A CN 201710022520 A CN201710022520 A CN 201710022520A CN 106800976 A CN106800976 A CN 106800976A
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- glycerine
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- biodiesel
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Classifications
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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
-
- 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
Abstract
A kind of method that glycerine round-robin method continous way prepares biodiesel, liquid material oil and glycerine are passed through in preheater simultaneously, and the feedstock oil and glycerine after preheating are passed through in flow reactor simultaneously, directly carry out esterification；Grease after esterification terminates is passed directly into continous way transesterification reactor after heat recovery heat exchanger and cooler cooling, while being passed through the methyl alcohol dissolved with potassium hydroxide catalyst, carries out ester exchange reaction；Reaction terminates to obtain biodiesel oil product and by-product glycerol through refinement treatment, and glycerine is passed through continous way esterifier interior circulation and uses as raw material.Make the complete process method that raw materials glycerine round-robin method continous way prepares biodiesel from high acid value waste oil fat the invention provides a kind of, realize reaction raw materials through waste heat recovery heat exchange, preheating, continous way esterification and ester exchange reaction integration process flow, continuous reaction of the invention, production efficiency is remarkably improved, helps to enhance production capacities；Be conducive to the industrialized production of scale.
Description
Technical field
The invention belongs to technical field of biodiesel preparation, and in particular to a kind of continous way prepares biodiesel process, especially
It is related to a kind of high-acid value grease glycerine round-robin method continous way to prepare the integrated artistic method of biodiesel.
Background technology
Biodiesel is a kind of renewable new energy of cleaning, and it is used as the petrochemical industry that a kind of new liquid fuel is high-quality
Substitute of diesel fuel, with great application prospect.Cost of material is the principal element for restricting Biodiesel development all the time, its
The 60% ~ 90% of totle drilling cost is accounted for, uses all kinds of high acid value waste oil fat for reclaiming to turn into study hotspot for raw material prepares biodiesel,
It is also the main trend for promoting Biodiesel development.But these waste grease raw materials generally have acid number higher, no
Traditional base-catalyzed transesterification can directly be carried out and prepare biodiesel, therefore, the waste grease of high acid value must before ester exchange reaction
Esterification deacidification treatment must be carried out；It is all through over-churning, ester exchange two to prepare biodiesel currently with the waste grease of high acid value
Step reaction is carried out, 1. the main catalytic esterification technology using acidic catalyst of traditional esterifications reaction, the acidic catalyst such as concentrated sulfuric acid
Use, easy etching apparatus so higher to equipment material requirement, and is susceptible to side reaction, causes biodiesel oil product
Sulfur content it is higher；2. esterification generally uses methyl alcohol, produces large quantity of moisture to exclude in time in course of reaction, esterifying efficiency
Low, methanol usage is big, and needs repeatedly to be dehydrated dealcoholysis in reaction and add methyl alcohol, and time-consuming；3. the pair that ester exchange reaction is generated
Produce the utilization that glycerine can not be effective and reasonable；And reaction major part uses intermittent mode, production process is various, and productivity ratio is relatively low；For
The energy consumption that overcomes the traditional batch mode of production to exist is big, time-consuming and the low defect of production capacity, continuously producing biodiesel
In the middle of constantly research and development, only ester exchange reaction can be continuously produced method at present, early stage esterification
All it is to use batch technology, efficiency is low, it is impossible to matched with ester exchange serialization, and studies the continuous preparation biodiesel of report
Method, severe reaction conditions, equipment cost is high, and production capacity is low, limits industrial applications, and such as CN101575285A discloses one kind
The process and special equipment of continuous production fatty glyceride, reaction need to be through special equipment mixing, emulsifying, circulation etc.
Multiple operations, and need the solid catalysts such as zinc powder and NaOH；As CN102010792B discloses a kind of continuous prodution
The method of biodiesel, it is needed in regular duct solid base integer catalyzer filling reactor；CN 1919973B are disclosed
A kind of method that use loop turbulent flow reactor and several second reactor continous ways prepare biodiesel, reaction temperature is
150 ~ 230 DEG C, reaction pressure is 1 ~ 7MP.
The content of the invention
The technical problem of solution：In order to solve traditional biological diesel oil batch process for preparing, time-consuming, energy consumption big, and methanolic acid is urged
The cumbersome process such as dealcoholysis are dehydrated in change esterification process, product sulfur content is too high, and a large amount of glycerine of by-product can not be utilized rationally；It is existing continuous
Change preparation method high cost, severe reaction conditions, it is difficult to which the defect such as industrialization, the present invention provides a kind of glycerine round-robin method continous way
The method for preparing biodiesel.
Technical scheme：A kind of method that glycerine round-robin method continous way prepares biodiesel, comprises the following steps：（1）Continuously
Without catalyzing glycerol esterification：Liquid material oil and glycerine are passed through in preheater simultaneously, preheating temperature is 120-150 DEG C, in advance
Feedstock oil and glycerine after heat are passed through in flow reactor simultaneously with following current or reflux type, are not added with directly being carried out under catalyst
Esterification, controls reactor temperature for 210-230 DEG C, and vacuum is -0.03-0.05MPa, and feedstock oil and glycerine are passed through
Flow-rate ratio is 6:1~12:1, split time surveys acid number, regulation and control charging total flow so that feedstock oil goes out after flowing through flow reactor
Material acid value of oil and fat is less than 2.0 mgKOH/g；（2）Ester exchange reaction and refinement treatment：Esterification terminate after grease through waste heat
It is passed directly into continous way transesterification reactor after reclaiming heat exchanger and cooler cooling, while being passed through dissolved with potassium hydroxide catalysed
The methyl alcohol of agent, carries out ester exchange reaction；Reaction terminates to obtain biodiesel oil product and by-product glycerol, glycerine conduct through refinement treatment
Raw material is passed through continous way esterifier interior circulation and uses.
Above-mentioned raw materials oil is at least one in waste oil, soap stock acidification oil or fatty acid waste products, by plate-frame filtering and
Pretreated high-acid value grease is flashed, acid number is 25 ~ 170 mgKOH/g.
Step（1）Described in continous way esterifier be pipeline reactor or series connection tank reactor；Duct type
There is liquid redistribution device in reactor inside pipeline, be conducive to reaction mass to be well mixed, fully reaction；Series connection still reaction
Device；It is made up of the kettle of 2 ~ 6 series connection, is heated by heat conduction oil lagging, and with mechanical stirring device.
Methanol usage is the 25 ~ 40% of oil quality in above-mentioned ester exchange reaction, and potassium hydroxide consumption is oil quality
0.5 ~ 0.8%, 63 ~ 65 DEG C of reaction temperature.
Above-mentioned refinement treatment is that the grease after ester exchange carried out into dealcoholation treatment, the grease of dealcoholysis be transferred to standing tank carry out it is quiet
Layering is put, upper strata is coarse biodiesel, and lower floor is crude glycerine, and coarse biodiesel is directly evaporated in vacuo, product after distillation
Further alkali cleaning, washing, dry, the high-quality biological diesel oil finished product of acquisition low sulfur content；Crude glycerine is carried out into acid neutralization, and
Distilled after removal of impurities, obtained glycerine finished product.
Beneficial effect：（1）The present invention provides a kind of high-acid value grease glycerine round-robin method continous way and prepares biodiesel process,
High acid value waste oil fat is reacted using continous way glycerine esterification, and esterification is carried out under vacuo, you can prevent from reacting grease quilt
Oxidation, in time can take outside reactor the moisture for reacting production out of again, promote reaction forward to carry out, and improve reaction efficiency, and ester
Change terminates not needing dealcoholysis operation, can directly carry out ester exchange reaction, simplifies production procedure；
（2）High-acid value grease glycerine esterification reaction of the present invention, it is not necessary to the addition of the acid class catalyst such as sulfuric acid, it is cost-effective,
And the sulfur content of product is reduced, improve the quality of biodiesel oil product；
（3）The present invention realizes the efficient utilization and recycling of substantial amounts of by-product glycerol of biological diesel oil, it is to avoid the wasting of resources and
Environmental pollution；Be esterified under the grease condition of high temperature after terminating directly carries out pre- recuperation of heat and energy exchange through fuel oil preheating device,
Heat makes full use of, reducing energy consumption；
（4）Make the complete of raw materials glycerine round-robin method continous way preparation biodiesel from high acid value waste oil fat the invention provides a kind of
Whole process, realizes reaction raw materials through waste heat recovery heat exchange, preheating, continous way esterification and ester exchange reaction integration operation stream
Journey, continuous reaction of the invention, is remarkably improved production efficiency, helps to enhance production capacities；Be conducive to the industrialization of scale
Production.
Brief description of the drawings
Fig. 1 is technological process of production schematic diagram of the invention.
Specific embodiment
The following examples are expanded on further to of the invention, but the invention is not restricted to this.
Embodiment 1
（1）Will be through plate-frame filtering and the pretreated waste oil of flash distillation by pump（The mgKOH/g of acid number 48）It is passed through simultaneously with glycerine
Preheated in heat recovery heat exchanger, the heating source in heat exchanger is the high temperature esterification oil that esterification terminates, real in heat exchanger
Existing reaction raw materials preheating, the purpose of cooling down high-temperature esterised oil makes specific energy consumption reduction by more than 45%, and preheating temperature is 120-150
DEG C, the raw material after preheating is squeezed into carries out esterification, temperature in control reactor in two continous way esterifiers of kettle series connection
It is 210 DEG C to spend, and reaction vacuum is -0.03 MPa, and the flow-rate ratio that is passed through of grease and glycerine is 6:1, split time surveys acid number, adjusts
Control charging total flow so that feedstock oil discharges acid value of oil and fat less than 2 mgKOH/g after flowing through flow reactor.The continuous esterification
Technique significantly improves production efficiency, yield in the unit interval is reached 4 t/more than h.
（2）Grease after esterification terminates is passed directly into continous way ester exchange after heat recovery heat exchanger and cooler cooling
In reactor, while being passed through the methyl alcohol dissolved with potassium hydroxide catalyst, ester exchange reaction is carried out, methanol usage is oil quality
25%, potassium hydroxide consumption is the 0.5% of oil quality, 63 DEG C of reaction temperature；The grease of ester exchange is carried out into dealcoholation treatment, dealcoholysis
Grease be transferred to standing tank carry out stratification, upper strata is coarse biodiesel, and lower floor is crude glycerine, and coarse biodiesel is directly entered
Row distillation, product carries out the refinement treatments such as alkali cleaning, washing, drying after distillation, obtains biodiesel finished product, analyzes biological after testing
The methyl ester content of diesel oil is more than 98.5%, and sulfur content is less than 30 ppm；Crude glycerine is carried out into acid neutralization, and is carried out after removal of impurities
Distillation, obtains glycerine finished product, and glycerine is simultaneously used as raw material into continous way esterifier interior circulation.
Embodiment 2
（1）Will be through plate-frame filtering and the pretreated soap stock acidification oil of flash distillation by pump（The mgKOH/g of acid number 78）With glycerine simultaneously
It is passed through in heat recovery heat exchanger and is preheated, the heating source in heat exchanger is the high temperature esterification oil that esterification terminates, in heat exchanger
In realize reaction raw materials preheat, the purpose of cooling down high-temperature esterised oil, make specific energy consumption reduction by more than 45%, preheating temperature is 120-
150 DEG C, the raw material after preheating is squeezed into carries out esterification in three continous way esterifiers of kettle series connection, in control reactor
Temperature is 220 DEG C, and reaction vacuum is -0.04MPa, and the flow-rate ratio that is passed through of grease and glycerine is 8:1, split time surveys acid number,
Regulation and control charging total flow so that feedstock oil discharges acid value of oil and fat less than 2 mgKOH/g after flowing through flow reactor.The continuous ester
Chemical industry skill significantly improves production efficiency, yield in the unit interval is reached 6 t/more than h.
（2）Grease after esterification terminates is passed directly into continous way ester exchange after heat recovery heat exchanger and cooler cooling
In reactor, while being passed through the methyl alcohol dissolved with potassium hydroxide catalyst, ester exchange reaction is carried out, methanol usage is oil quality
30%, potassium hydroxide consumption is the 0.6% of oil quality, 64 DEG C of reaction temperature；The grease of ester exchange is carried out into dealcoholation treatment, dealcoholysis
Grease be transferred to standing tank carry out stratification, upper strata is coarse biodiesel, and lower floor is crude glycerine, and coarse biodiesel is directly entered
Row distillation, product carries out the refinement treatments such as alkali cleaning, washing, drying after distillation, obtains biodiesel finished product, analyzes biological after testing
The methyl ester content of diesel oil is more than 98.0%, and sulfur content is less than 35 ppm；Crude glycerine is carried out into acid neutralization, and is carried out after removal of impurities
Distillation, obtains glycerine finished product, and glycerine is simultaneously used as raw material into continous way esterifier interior circulation.
Embodiment 3
（1）Will be through plate-frame filtering and the pretreated fatty acid waste products of flash distillation by pump（The mgKOH/g of acid number 125）It is same with glycerine
When be passed through in heat recovery heat exchanger and preheated, the heating source in heat exchanger is the high temperature esterification oil that esterification terminates, in heat exchange
Realize that reaction raw materials are preheated in device, the purpose of cooling down high-temperature esterised oil makes specific energy consumption reduction by more than 45%, and preheating temperature is
120-150 DEG C, the raw material after preheating is squeezed into carries out esterification, control reaction in four continous way esterifiers of kettle series connection
Temperature is 225 DEG C in device, and reaction vacuum is -0.05MPa, and the flow-rate ratio that is passed through of grease and glycerine is 10:1, split time is surveyed
Acid number, regulation and control charging total flow so that feedstock oil discharges acid value of oil and fat less than 2 mgKOH/g after flowing through flow reactor.Should
Continuous esterification technique significantly improves production efficiency, yield in the unit interval is reached 8 t/more than h.
（2）Grease after esterification terminates is passed directly into continous way ester exchange after heat recovery heat exchanger and cooler cooling
In reactor, while being passed through the methyl alcohol dissolved with potassium hydroxide catalyst, ester exchange reaction is carried out, methanol usage is oil quality
36%, potassium hydroxide consumption is the 0.7% of oil quality, 65 DEG C of reaction temperature；The grease of ester exchange is carried out into dealcoholation treatment, dealcoholysis
Grease be transferred to standing tank carry out stratification, upper strata is coarse biodiesel, and lower floor is crude glycerine, and coarse biodiesel is directly entered
Row distillation, product carries out the refinement treatments such as alkali cleaning, washing, drying after distillation, obtains biodiesel finished product, analyzes biological after testing
The methyl ester content of diesel oil is more than 98.8%, and sulfur content is less than 25 ppm；Crude glycerine is carried out into acid neutralization, and is carried out after removal of impurities
Distillation, obtains glycerine finished product, and glycerine is simultaneously used as raw material into continous way esterifier interior circulation.
Embodiment 4
（1）By pump by through the mixing of plate-frame filtering and the pretreated waste oil of flash distillation, soap stock acidification oil and fatty acid waste products
Grease（The mgKOH/g of acid number 165）It is passed through in heat recovery heat exchanger simultaneously with glycerine and is preheated, the heating source in heat exchanger
For the high temperature esterification oil that esterification terminates, realize that reaction raw materials are preheated in heat exchanger, the purpose of cooling down high-temperature esterised oil makes unit
Energy consumption reduction by more than 45%, preheating temperature is 120-150 DEG C, and the continous way esterification that the raw material after preheating squeezes into six kettle series connection is anti-
Answering carries out esterification in device, control reactor temperature for 230 DEG C, and reaction vacuum is -0.05MPa, grease and glycerine
It is 12 to be passed through flow-rate ratio:1, split time surveys acid number, regulation and control charging total flow so that feedstock oil goes out after flowing through flow reactor
Material acid value of oil and fat is less than 2 mgKOH/g.The continuous esterification technique significantly improves production efficiency, yield in the unit interval is reached 12
T/more than h.
（2）Grease after esterification terminates is passed directly into continous way ester exchange after heat recovery heat exchanger and cooler cooling
In reactor, while being passed through the methyl alcohol dissolved with potassium hydroxide catalyst, ester exchange reaction is carried out, methanol usage is oil quality
40%, potassium hydroxide consumption is the 0.8% of oil quality, 65 DEG C of reaction temperature；The grease of ester exchange is carried out into dealcoholation treatment, dealcoholysis
Grease be transferred to standing tank carry out stratification, upper strata is coarse biodiesel, and lower floor is crude glycerine, and coarse biodiesel is directly entered
Row distillation, product carries out the refinement treatments such as alkali cleaning, washing, drying after distillation, obtains biodiesel finished product, analyzes biological after testing
The methyl ester content of diesel oil is more than 99.2%, and sulfur content is less than 10 ppm；Crude glycerine is carried out into acid neutralization, and is carried out after removal of impurities
Distillation, obtains glycerine finished product, and glycerine is simultaneously used as raw material into continous way esterifier interior circulation.
Claims (5)
1. a kind of method that glycerine round-robin method continous way prepares biodiesel, it is characterised in that comprise the following steps：
（1）Continuously without catalyzing glycerol esterification：Liquid material oil and glycerine are passed through in preheater simultaneously, preheating temperature is
120-150 DEG C, feedstock oil and glycerine after preheating are passed through in flow reactor simultaneously with following current or reflux type, are not added with catalysis
Esterification is directly carried out under agent, it is 210-230 DEG C to control reactor temperature, and vacuum is -0.03-0.05MPa, feedstock oil
The flow-rate ratio that is passed through with glycerine is 6:1~12:1, split time surveys acid number, regulation and control charging total flow so that feedstock oil is flowed through continuously
The acid value of oil and fat that discharged after formula reactor is less than 2.0 mgKOH/g；
（2）Ester exchange reaction and refinement treatment：Grease after esterification terminates is straight after heat recovery heat exchanger and cooler cooling
Connect in continous way transesterification reactor, while being passed through the methyl alcohol dissolved with potassium hydroxide catalyst, carry out ester exchange reaction；Instead
Should terminate to obtain biodiesel oil product and by-product glycerol through refinement treatment, glycerine is passed through in continous way esterifier as raw material
Recycle.
2. a kind of method that glycerine round-robin method continous way prepares biodiesel according to claim 1, it is characterised in that described
Feedstock oil is at least one in waste oil, soap stock acidification oil or fatty acid waste products, by after plate-frame filtering and flash distillation pretreatment
High-acid value grease, acid number be 25 ~ 170 mgKOH/g.
3. a kind of method that glycerine round-robin method continous way prepares biodiesel according to claim 1, it is characterised in that step
（1）Described in continous way esterifier be pipeline reactor or series connection tank reactor；Pipeline in pipeline reactor
There is liquid redistribution device inside；Series connection tank reactor；It is made up of the kettle of 2 ~ 6 series connection, is heated by heat conduction oil lagging,
And with mechanical stirring device.
4. a kind of method that glycerine round-robin method continous way prepares biodiesel according to claim 1, it is characterised in that described
Methanol usage is the 25 ~ 40% of oil quality in ester exchange reaction, and potassium hydroxide consumption is the 0.5 ~ 0.8% of oil quality, reaction
63 ~ 65 DEG C of temperature.
5. a kind of method that glycerine round-robin method continous way prepares biodiesel according to claim 1, it is characterised in that described
Refinement treatment is that the grease after ester exchange is carried out into dealcoholation treatment, and the grease of dealcoholysis is transferred to standing tank carries out stratification, upper strata
It is coarse biodiesel, lower floor is crude glycerine, and coarse biodiesel is directly evaporated in vacuo, the further alkali cleaning of product after distillation,
Washing, dry, the high-quality biological diesel oil finished product of acquisition low sulfur content；Crude glycerine is carried out into acid neutralization, and it is laggard through removal of impurities
Row distillation, obtains glycerine finished product.
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Cited By (12)
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| CN107459997A (en) * | 2017-07-21 | 2017-12-12 | 中国林业科学研究院林产化学工业研究所 | A kind of high acid value waste oil glycerine is without catalytic esterification deacidification continuous production technology |
| CN108277090A (en) * | 2018-01-30 | 2018-07-13 | 浙江工业大学 | A kind of preparation method of low-sulphur biodiesel |
| CN109293476A (en) * | 2018-11-29 | 2019-02-01 | 浙江工业大学 | Glycerol separating technology and device in a kind of glycerine esterification production waste water |
| CN109306276A (en) * | 2017-07-26 | 2019-02-05 | 新疆大森化工有限公司 | A kind of synthesis technology of unsaturated fatty acid ester type diesel antiwear additive |
| CN111500373A (en) * | 2020-04-27 | 2020-08-07 | 浙江工业大学 | Preparation method of biodiesel |
| WO2020188608A1 (en) * | 2019-03-20 | 2020-09-24 | Ymir Technologies Ehf. | Continuous flow system for the production and purification of biodiesel |
| CN112159730A (en) * | 2020-09-09 | 2021-01-01 | 湖北天基生物能源科技发展有限公司 | Method for treating esterified oil |
| CN112481041A (en) * | 2020-12-15 | 2021-03-12 | 浙江工业大学 | Device and method for continuously preparing biodiesel |
| CN112852552A (en) * | 2021-01-25 | 2021-05-28 | 茂名市凯跃特种油剂有限公司 | Method for preparing bunker fuel oil by using illegal cooking oil based on glycerol esterification process |
| CN113499749A (en) * | 2021-07-20 | 2021-10-15 | 浙江工业大学 | Method and device for continuously preparing biodiesel by multiple towers in series connection |
| CN115612553A (en) * | 2022-10-31 | 2023-01-17 | 上海中器环保科技有限公司 | Process for recovering biodiesel from crude glycerol |
| CN115820342A (en) * | 2022-11-04 | 2023-03-21 | 江苏强林生物能源材料有限公司 | Method for continuously preparing neutral grease for biodiesel without catalyst |
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| CN109306276A (en) * | 2017-07-26 | 2019-02-05 | 新疆大森化工有限公司 | A kind of synthesis technology of unsaturated fatty acid ester type diesel antiwear additive |
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