CN106318645A - Method and equipment for gas-liquid two-phase esterification pretreatment of microbial lipids - Google Patents
Method and equipment for gas-liquid two-phase esterification pretreatment of microbial lipids Download PDFInfo
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- CN106318645A CN106318645A CN201610835043.0A CN201610835043A CN106318645A CN 106318645 A CN106318645 A CN 106318645A CN 201610835043 A CN201610835043 A CN 201610835043A CN 106318645 A CN106318645 A CN 106318645A
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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
-
- 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
- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/12—Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
-
- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/44—Deacidification step, e.g. in coal enhancing
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a method and equipment for gas-liquid two-phase esterification pretreatment of microbial lipids. A gas-liquid two-phase rector is a heatable low-pressure-resistant device and can allow low alcohols to have sufficient time to undergo contact reaction with the microbial lipids at a temperature higher than a boiling point and at a low pressure, and stirring, a baffle or a circulating device can be added according to specific needs. The microbial lipids and a catalyst are added into the conical reactor; stirring is started prior to temperature increase, and the low alcohols enter the reactor from the bottom thereof in a form of steam and fast reacts with free fatty acids with the help of a climbing height at a high temperature and at the lower pressure; in order to enable the reaction to be performed at the temperature higher than the boiling point of the low alcohols, the equipment is required to be resistant to pressure properly; an alcohol-water mixture flowing out of the reactor is subjected to condensation and then can be refined and recycled by means of rectification. The method is capable of decreasing the lipid acid value effectively, lipid conversion rate is not less than 95% and the oil yield is not less than 98%.
Description
Technical field
The present invention relates to the method and apparatus of a kind of gas-liquid two-phase esterification pretreatment microbial grease, relate to oil chemistry
Utilize, biodiesel is prepared and relevant device technical field.
Background technology
It is known that the reproducible biodiesel of environmental protection is to substitute the potential oil plant of existing fuel oil, have widely
Utilization prospect, but cross high reason due to production cost and cannot promote the use of at present.
Pretreating process for high-acid value grease is exactly one of restraining factors among these, at present, is used for producing biological bavin
The equipment of oil has: tank reactor, tubular reactor, trickle bed reactor, membrane reactor, micro passage reaction etc., except tradition
Reactor other devices outer be almost mainly used in ester exchange reaction, and one class rests on research and development or Chinese style stage.Still reaction
Device is exactly general reactor.It feeds intake conveniently, simple to operate, technical maturity.But mass transfer is poor, need on high-acid value grease reducing
Want reaction of high order to can be only achieved Expected Results, not only increase energy consumption, extend the time, add the usage amount of lower alcohol, and
Technique is loaded down with trivial details.
Additionally, oil source is to restrict its another principal element industrialized.Now with the development of industrial technology, micro-
Bio-oil progressively becomes the raw material of available preparation biodiesel, but high-quality be generally used for edible wait other high additional
Value field, and poor oil plant, its acid number is too high, and have has reached 30mgKOH/g, must drop before preparation biodiesel
The esterification pretreatment of acid number.
To design, principle is simple, step is integrated as can be seen here, energy-conservation few time, and a step can reduce microbial oil fat acid
The Processes and apparatus of valency seems the most urgent.
Summary of the invention
In order to solve the reaction of high order that prior art exists, the shortcomings such as energy consumption is high, the longest, complex procedures, the present invention carries
For the method and apparatus of a kind of gas-liquid two-phase esterification pretreatment microbial grease, this principle of peactor is simple, step is integrated, permissible
The step realizing high-acid value grease reduces the purpose of acid number.
The technical scheme is that the equipment of a kind of gas-liquid two-phase esterification pretreatment microbial grease, successively by reacting
Device, condenser, fraction collection tank, heater, rectifying column, alcohol storage tank, explosion-proof pump, carburator are composed in series circular response system；
Described reactor head is provided with mixed vapour outlet, is provided with gas distribution of net, under gas distribution of net at alcohol steam inlet, bottom
If check-valves.
Reactor is provided with in stirring, dividing plate or circulating device any one or a few.
Described gas distribution of net includes distribution of net structure netted, poroid.
The top of reactor is additionally provided with microorganism oil plant and catalyst inlet, observation panel, and the bottom of reactor is additionally provided with product
Product export.
The method of equipment based on described a kind of gas-liquid two-phase esterification pretreatment microbial grease, microorganism oil plant is from micro-
Bio-oil materials import enters in reactor, and lower alcohol steam is entered by the alcohol steam inlet of reactor bottom, and it is low that bottom enters
Level alcohol vapor microorganism oil plant haptoreaction in the presence of acid catalyst in gas distribution of net with reactor, unreacted
Lower alcohol steam and the mixed vapour outlet from top of the water vapour of generation discharge, water that the condensation of condensed device obtains and rudimentary
Alcohol mixed liquor enters in fraction collection tank, and enters in alcohol storage tank after processing by rectifying column stand-by, when in reactor, oil plant is sour
Valency is reduced to acid number less than stopped reaction during 2mgKOH/g；Recovery lower alcohol in alcohol storage tank enters carburator by explosion-proof pump
In, react in being controlled to reenter reactor by check-valves after gasification.
Temperature in reactor is 101～260 DEG C, and the temperature of carburator is 65～150 DEG C.
Described acid catalyst includes concentrated sulphuric acid, p-methyl benzenesulfonic acid, Al2O3、SiO2、TiO2、TiO2-SiO2、Al2O3-
SiO2、ZrSO4、ZrO2/SiO2、SO4 2-/TiO2Any one or a few mixture in solid acid.
The outlet of fraction collection tank delivers to rectifying column rectification after being preheated by mixed liquor heater via by explosion-proof pump, and rectification is low
It is stand-by that level alcohol is back to alcohol storage tank.
Described lower alcohol includes methanol or ethanol.
Beneficial effect:
The present invention uses novel gas-liquid two-phase reactor to be esterified microbial grease, equipment generally taper, this gas-liquid two-phase
Reactor is heatable pressure-resistant apparatus, can make at low pressures low boiling lower alcohol in the case of higher than its boiling point with
Microbial grease has time enough haptoreaction, and reactor can add stirring, dividing plate or circulating device according to specific needs.Rudimentary
Alcohol steam inlet is equipped with gas distribution of net, and this design can make lower alcohol enter reactor also from reactor bottom as a vapor
Climb altitude is utilized to realize fast reaction under low-voltage high-temperature with free fatty；For making the reaction can be higher than lower alcohol boiling point
At a temperature of react, equipment need the most pressure (1MPa)；Can be by rectification after in reactor, alcohol-water mixture out is condensed
The refined also reuse of mode.The method can effectively reduce acid value of oil and fat, oils and fats conversion ratio >=95%, oil yield >=98%.This equipment
Effectively water byproduct can be discharged at any time reaction system, and by rectification method by lower alcohol reuse, high acid value oil can be effectively improved
The esterification yied of fat and minimizing lower alcohol usage amount.
Accompanying drawing explanation
Fig. 1: one embodiment flow process simple illustration figure.
Wherein, 1 is check-valves, and 2 is gas distribution of net, and 3 is reactor, and 4 is carburator, and 5 is explosion-proof pump, and 6 is alcohol storage tank,
7 is rectifying column, and 8 is fraction collection tank, and 9 is heater, and 10 is condenser.
Specific implementation method
If not specializing, the conventional means that technological means used in embodiment is well known to those skilled in the art.
In conjunction with accompanying drawing, the following is specific embodiment.
The invention mainly relates to the method and apparatus of a kind of gas-liquid two-phase esterification pretreatment microbial grease.Its key step
For by microorganism oil plant, acid catalyst puts into cone-shaped reactor from material inlet, is heated to design temperature 101 DEG C～260 DEG C,
Ensure that water generation reaction departs from cone-shaped reactor in time with this, improve Esterification of Free Fat Acid rate；By lower alcohol steam by reacting
Low boiling feedstock vapor import bottom device enters, the lower alcohol steam that bottom enters micro-life in distribution of net with reactor
Thing oils and fats haptoreaction, the water vapour of unreacted lower alcohol steam and generation exports from the mixed vapour of reactor and discharges, enters
Entering in condenser and condense, water and lower alcohol mixed liquor that the condensation of condensed device obtains enter in fraction collection tank, and pass through rectification
Tower enters reuse in alcohol storage tank after processing, the stopped reaction release product when oil plant acid value is reduced to a certain degree in reactor
Product.A kind of gas-liquid two-phase reactor, reactor body is by reactor and agitator, condenser, gas distribution of net and check valve set
Becoming, other corollary equipments are made up of carburator, explosion-proof pump, alcohol storage tank, rectifying column, fraction collection tank etc..Lower alcohol in reactor
Gas access is the uniform distributor such as netted, poroid；This design can make lower alcohol enter from reactor bottom as a vapor
Reactor also utilizes climb altitude to realize fast reaction under low-voltage high-temperature with free fatty.
The mixed vapour outlet of reactor is connected with the import of condenser, and the outlet of condenser is connected with fraction collection tank,
The outlet of fraction collection tank can deliver to rectifying column rectification after being preheated by mixed liquor heater via by explosion-proof pump, its rectification lower alcohol
It is back to alcohol storage tank stand-by.
The import of the raw material lower alcohol explosion-proof pump of tank egress links and carburator connects, the outlet of carburator and the end of reactor
Portion connects and passes through gas distribution of net and carries lower alcohol gas in reactor, for preventing oil plant adverse current, under gas distribution of net
End is provided with check-valves；Reactor and heater are provided with heater；The top of reactor is provided with microorganism oil plant and catalysis
Agent import, mixed vapour outlet, observation panel, agitator etc., the bottom of reactor is provided with lower alcohol steam inlet and products export.
Reactor is provided with in stirring, dividing plate or circulating device any one or a few.
A kind of method and apparatus of gas-liquid two-phase esterification pretreatment microbial grease, by microorganism oil plant, acid catalyst from
Material inlet puts in cone-shaped reactor, and lower alcohol steam is entered by the low boiling feedstock vapor import of reactor bottom, bottom
The lower alcohol steam entered microbial grease haptoreaction in distribution of net and reactor, unreacted lower alcohol steam and
The water vapour generated exports from the mixed vapour of reactor and discharges, and enters in condenser and condenses, and condensed device condenses the water obtained
Enter in fraction collection tank with lower alcohol mixed liquor, and reuse in entrance alcohol storage tank after processing by rectifying column, when in reactor
Stopped reaction release product when oil plant acid value is reduced to a certain degree.
Water in rectifying column periodically byproduct discharge from bottom is discharged.
Temperature in reactor is 101～260 DEG C, and the temperature of carburator is 65～150 DEG C, it is ensured that the gasification of lower alcohol.
The carrier of described solid acid catalyst is molecular sieve, silica gel, adsorbent resin, porous ceramics, kieselguhr or Pumex
In any one.
The acid catalyst that can be used for this reaction is concentrated sulphuric acid, p-methyl benzenesulfonic acid, Al2O3、SiO2、TiO2、TiO2-SiO2、
Al2O3-SiO2、ZrSO4、ZrO2/SiO2、SO4 2-/TiO2In any one or a few mixture in solid acid.
Microbial grease (acid number is 26mgKOH/g), catalyst, methanol, ethanol are commercial.
Embodiment 1:
Raw material: microbial grease (Dalian Inst of Chemicophysics, Chinese Academy of Sciences), methanol, concentrated sulphuric acid
In reactor 3, inject appropriate microbial grease and the concentrated sulfuric acid catalyst of 0.8% mass ratio, rise high-temperature extremely
110 DEG C, starting to inject methanol steam from lower end, carburator 4 temperature is 80 DEG C.When fraction collection tank has a large amount of alcohol-water mixture
Shi Kaiqi rectifying column, control reflux ratio is 1:1, and tower top temperature is 65 DEG C, and the oil product acid value released when reactor lower end reaches
Methanol can be stopped during 1mgKOH/g enter and continue to heat methanol in elimination reaction device, open baiting valve both low acid number oils
Fat.The conversion ratio recording methyl esterification of fatty acid reaches 96.1%, and oil yield is 98.3%.
Embodiment 2:
Raw material: microbial grease, methanol, p-methyl benzenesulfonic acid
In reactor 3, inject the Catalyzed by p-Toluenesulfonic Acid agent of appropriate microbial grease and 1% mass ratio, rise high-temperature
To 150 DEG C, starting to inject methanol steam from lower end, carburator 4 temperature is 75 DEG C.Mix when fraction collection tank has a large amount of alcohol water
Opening rectifying column during thing, control reflux ratio is 1.2:1, and tower top temperature is 64.8 DEG C, when the oil product acid value that reactor lower end releases
Stop methanol when reaching 1.1mgKOH/g and enter and continue to heat methanol in elimination reaction device, unlatching baiting valve both low acid number oils
Fat.The conversion ratio recording methyl esterification of fatty acid reaches 95.7%, and oil yield is 98%.
Embodiment 3
Raw material: microbial grease, methanol, solid acid catalyst
Reactor will inject appropriate microbial grease, and add the SO of 15% mass ratio4 2-/TiO2Catalyst, raises
Temperature, to 200 DEG C, starts to inject methanol steam, carburettor temperature 100 DEG C from lower end.Mix when fraction collection tank has a large amount of alcohol water
Opening rectifying column during compound, control reflux ratio is 1.1:1, and tower top temperature is 64.9 DEG C, when the oil acid that reactor lower end releases
Stop methanol when valency reaches 1.2mgKOH/g and enter and continue to heat methanol in elimination reaction device, unlatching baiting valve both low
Acid number oils and fats.The conversion ratio recording methyl esterification of fatty acid reaches 95.3%, and oil yield is 98.1%.
Embodiment 4:
Raw material: microbial grease, ethanol, mixed catalyst
Reactor will inject appropriate microbial grease, and add p-methyl benzenesulfonic acid and 20% matter of 0.5% mass ratio
The ZrO of amount ratio2/SiO2Catalyst, liter high-temperature, to 230 DEG C, starts to inject lower alcohol steam, carburettor temperature 90 DEG C from lower end.
Open rectifying column when there being a large amount of alcohol-water mixture in fraction collection tank, control reflux ratio is 1.2:1, and tower top temperature is 78.2
DEG C, stop lower alcohol when the oil product acid value released when reactor lower end reaches 0.9mgKOH/g and enter and continue heating removing
Lower alcohol in reactor, open baiting valve both low acid number oils and fats.The conversion ratio recording methyl esterification of fatty acid reaches 96.5%, oil
Yield is 97.6%.
Claims (9)
1. the equipment of a gas-liquid two-phase esterification pretreatment microbial grease, it is characterised in that successively by reactor (3), condensation
Device (10), fraction collection tank (8), heater (9), rectifying column (7), alcohol storage tank (6), explosion-proof pump (5), carburator (4) series connection group
Become circular response system；Described reactor (3) top is provided with mixed vapour outlet, is provided with gas and divides at alcohol steam inlet, bottom
Arranging net (2), gas distribution of net (2) divides into check-valves (1).
The equipment of a kind of gas-liquid two-phase the most according to claim 1 esterification pretreatment microbial grease, it is characterised in that anti-
Answer any one or a few that be provided with in device in stirring, dividing plate or circulating device.
The equipment of a kind of gas-liquid two-phase the most according to claim 1 esterification pretreatment microbial grease, it is characterised in that institute
State gas distribution of net and include distribution of net structure netted, poroid.
The equipment of a kind of gas-liquid two-phase the most according to claim 1 esterification pretreatment microbial grease, it is characterised in that anti-
The top answering device (3) is additionally provided with microorganism oil plant and catalyst inlet, observation panel, and the bottom of reactor (3) is additionally provided with product and goes out
Mouthful.
5. the method for equipment based on the arbitrary described a kind of gas-liquid two-phase esterification pretreatment microbial grease of Claims 1 to 4,
It is characterized in that, microorganism oil plant enters reactor (3) from microorganism oil plant import, and lower alcohol steam is by reactor (3) end
The alcohol steam inlet in portion enters, the lower alcohol steam that bottom enters microbial oil in gas distribution of net (2) with reactor
Expecting haptoreaction in the presence of acid catalyst, the water vapour of unreacted lower alcohol steam and generation is from the mixed vapour at top
Outlet is discharged, and water and lower alcohol mixed liquor that condensed device (10) condensation obtains enter in fraction collection tank (8), and pass through rectification
Tower (7) enters in alcohol storage tank (6) stand-by after processing, when in reactor (3), oil plant acid value acid number is less than 2mgKOH/g, stopping is anti-
Should；Recovery lower alcohol in alcohol storage tank is entered in carburator (4) by explosion-proof pump (5), is controlled again to enter by check-valves after gasification
Enter reaction in reactor.
The method of a kind of equipment based on gas-liquid two-phase esterification pretreatment microbial grease the most according to claim 5, its
Being characterised by, the temperature in reactor (3) is 101～260 DEG C, and the temperature of carburator (4) is 65～150 DEG C.
The method of a kind of equipment based on gas-liquid two-phase esterification pretreatment microbial grease the most according to claim 5, its
Being characterised by, described acid catalyst includes concentrated sulphuric acid, p-methyl benzenesulfonic acid, Al2O3、SiO2、TiO2、TiO2-SiO2、Al2O3-
SiO2、ZrSO4、ZrO2/SiO2、SO4 2-/TiO2Any one or a few mixture in solid acid.
The method of a kind of equipment based on gas-liquid two-phase esterification pretreatment microbial grease the most according to claim 5, its
Being characterised by, the outlet of fraction collection tank (8) delivers to rectifying column (7) after being preheated by mixed liquor heater via (9) by explosion-proof pump
Rectification, it is stand-by that rectification lower alcohol is back to alcohol storage tank (6).
The method of a kind of equipment based on gas-liquid two-phase esterification pretreatment microbial grease the most according to claim 5, its
Being characterised by, described lower alcohol includes methanol or ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610835043.0A CN106318645A (en) | 2016-09-19 | 2016-09-19 | Method and equipment for gas-liquid two-phase esterification pretreatment of microbial lipids |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610835043.0A CN106318645A (en) | 2016-09-19 | 2016-09-19 | Method and equipment for gas-liquid two-phase esterification pretreatment of microbial lipids |
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| CN201610835043.0A Pending CN106318645A (en) | 2016-09-19 | 2016-09-19 | Method and equipment for gas-liquid two-phase esterification pretreatment of microbial lipids |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202099261U (en) * | 2011-05-12 | 2012-01-04 | 种传学 | Esterification and directional separation integrated device for biodiesel production |
| CN102311342A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Method for producing 1,6-dimethyl adipate |
| CN202297557U (en) * | 2011-11-02 | 2012-07-04 | 昆明理工大学 | Gas-phase esterification and deacidification device for catalyzing high-acid value oil with mesoporous solid acid |
| CN203833916U (en) * | 2014-05-23 | 2014-09-17 | 安徽增源生物能源有限公司 | Esterification treatment system capable of effectively recycling methyl alcohol |
-
2016
- 2016-09-19 CN CN201610835043.0A patent/CN106318645A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311342A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Method for producing 1,6-dimethyl adipate |
| CN202099261U (en) * | 2011-05-12 | 2012-01-04 | 种传学 | Esterification and directional separation integrated device for biodiesel production |
| CN202297557U (en) * | 2011-11-02 | 2012-07-04 | 昆明理工大学 | Gas-phase esterification and deacidification device for catalyzing high-acid value oil with mesoporous solid acid |
| CN203833916U (en) * | 2014-05-23 | 2014-09-17 | 安徽增源生物能源有限公司 | Esterification treatment system capable of effectively recycling methyl alcohol |
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Application publication date: 20170111 |