CN109207210A - Coarse biodiesel slows down the method and device of back reaction - Google Patents

Coarse biodiesel slows down the method and device of back reaction Download PDF

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Publication number
CN109207210A
CN109207210A CN201811318366.8A CN201811318366A CN109207210A CN 109207210 A CN109207210 A CN 109207210A CN 201811318366 A CN201811318366 A CN 201811318366A CN 109207210 A CN109207210 A CN 109207210A
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CN
China
Prior art keywords
dealcoholysis
glycerol
tank
methanol
coarse biodiesel
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Pending
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CN201811318366.8A
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Chinese (zh)
Inventor
叶活动
陈文敏
王长南
阙锋才
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LONGYAN ZHUOYUE NEW ENERGY CO Ltd
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LONGYAN ZHUOYUE NEW ENERGY CO Ltd
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Priority to CN201811318366.8A priority Critical patent/CN109207210A/en
Publication of CN109207210A publication Critical patent/CN109207210A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS 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
    • C10L1/00Liquid carbonaceous fuels
    • C10L1/02Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

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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)
  • Liquid Carbonaceous Fuels (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses the method and device that a kind of coarse biodiesel slows down back reaction, the device is by pre- dealcoholysis mechanism, glycerol separating mechanism and again dealcoholysis mechanism three is connected in series.The pre- dealcoholysis of the operating procedure first step: being pumped into pre- dealcoholysis falling film heating flash vessel for the coarse biodiesel containing excessive methanol and distill, and cools down after excessive methanol vaporization and flows into recycling methanol tank again through surge tank;Second step separates glycerol: the coarse biodiesel of pre- dealcoholysis, which enters in settling tank, is precipitated to bottom glycerol settling zone, and the opening and closing of automatic valve is adjusted by controller, and glycerol is discharged into glycerol receiving tank;Third step dealcoholysis again: being pumped into again the distillation of dealcoholysis falling film heating flash vessel for the coarse biodiesel after pre- dealcoholysis and separation glycerol, through surge tank and flows into recycling methanol tank again after excessive methanol is cooling;Step 4: the coarse biodiesel after dealcoholysis successively flow to tubulation cooler and coarse biodiesel storage tank certainly again.Operation of the present invention convenience and high-efficiency, solve the problems, such as coarse biodiesel occur in dealcoholysis back reaction cause raw oil material to convert insufficient, product monoglyceride content is higher.

Description

Coarse biodiesel slows down the method and device of back reaction
Technical field
The present invention relates to method for producing biodiesel and equipment, and in particular to a kind of coarse biodiesel slows down the side of back reaction Method and device.
Background technique
Country's biodiesel (fatty acid methyl ester) is produced using waste oil as primary raw material at present, and the glyceride in waste oil exists By the way that transesterification occurs with methanol under alkaline condition, biodiesel and glycerol are generated;Since the reaction belongs to reversible reaction, because This, for the conversion ratio for improving glyceride, generallys use in biodiesel actual production process and is passed through excessive methanol, thus make Contain excessive methanol at the coarse biodiesel that reaction generates, needs to be recycled by dealcoholysis, and reduce to distillation It influences.
The transesterification of glyceride is reversible reaction, and before dealcoholysis, entire transesterification system is in equilibrium state, but in coarse biometric Diesel oil dealcoholysis process, with the reduction of reactant methanol, system balance is destroyed, and back reaction can occur for biodiesel and glycerol, Glyceride is generated, to reduce grease conversion ratio, and causes the glyceride contents such as monoglyceride in biodiesel on the high side;In addition, by In solubility of the methanol in glycerol much higher than the solubility in biodiesel, transesterification, which generates glycerol, can dissolve a large amount of first Alcohol causes glycerol relative density low, small with biodiesel density contrast, and such as without dealcoholysis, such glycerol is not easily separate.
In the prior art, coarse biodiesel does not efficiently separate glycerol generally before thorough dealcoholysis to slow down back reaction, Lead to that grease conversion ratio is relatively low, the higher defect of monoglyceride content in coarse biodiesel.
Summary of the invention
The object of the present invention is to provide the method and device that a kind of easy to operate efficient coarse biodiesel slows down back reaction, Back reaction occurs to solve existing coarse biodiesel in dealcoholysis, causing raw oil material to convert, insufficient, utilization rate is relatively low, product The higher problem of monoglyceride content.
In order to achieve the above object, in the present invention coarse biodiesel slow down the method for back reaction operating procedure it is as follows:
The pre- dealcoholysis of the first step: the first containing excess that biodiesel synthesis reaction vessel discharge port is discharged by pre- dealcoholysis feed pump The coarse biodiesel of alcohol is distilled via steam-heated pre- dealcoholysis falling film heating flash vessel, material distributing disc in falling film heating device After distribution, flowed from top to bottom with filminess to improve heat exchange efficiency along inner tubal wall, after the heated vaporization of excessive methanol and slightly Biodiesel separation leads to the cooling of spiral plate cooler, and methanol after cooling flows into recycling methanol tank after surge tank, completes pre- Dealcoholysis;Surge tank is vacuumized using vacuum pump so that the methanol after vaporizing is extracted out much sooner;
Second step separates glycerol: the coarse biodiesel of pre- dealcoholysis enters settling tank, due to methanol content in pre- dealcoholysis glycerol Less, density is big, can separate very well with coarse biodiesel in settling tank and be precipitated to bottom glycerol settling zone, by settling zone Density sensor real-time measurement and transmit signal into controller, after via controller processing again will instruction output to automatic valve Door, adjusts the open and close of automatic valve, and separation gives off glycerol into glycerol receiving tank;
Third step dealcoholysis again: still there is part methanol in the coarse biodiesel after pre- dealcoholysis and separation glycerol, in order to reduce Influence of production is distilled to subsequent processing, dealcoholysis again need to be carried out;Using dealcoholysis feed pump again by the coarse biodiesel of separated glycerol By the steam heated falling film heating flash vessel of dealcoholysis again distill, material through in falling film heating device distributing disc distribution after, along Inner tubal wall is flowed with filminess from top to bottom to improve heat exchange efficiency, is divided after the heated vaporization of excessive methanol with coarse biodiesel From leading to that spiral plate cooler is cooling, and methanol after cooling flows into recycling methanol tank, completion dealcoholysis again after surge tank;Buffering Tank is vacuumized using vacuum pump so that the methanol after vaporizing is extracted out much sooner;
Step 4: the coarse biodiesel after dealcoholysis flows automatically to coarse biodiesel from tubulation cooler is flow to after cooling again Storage tank.
It includes pre- dealcoholysis mechanism, glycerol separating mechanism and dealcoholysis again that coarse biodiesel, which slows down the device of back reaction, in the present invention Mechanism, three are connected in series;The pre- dealcoholysis mechanism includes pre- dealcoholysis feed pump, pre- dealcoholysis falling film heating flash vessel, spiral plate Cooler and surge tank, the discharge port of the import connection biodiesel synthesis reaction vessel of the pre- dealcoholysis feed pump, pre- dealcoholysis charging The outlet of pump is connected to the top of pre- dealcoholysis falling film heating flash vessel with pipeline, from the side of the pre- dealcoholysis falling film heating flash vessel Methanol efferent duct is drawn, is connect after spiral plate cooler with the top of surge tank, the bottom of surge tank is passed to back by pipeline Methanol tank is received, the bottom of the pre- dealcoholysis falling film heating flash vessel is connected to the glycerol separating mechanism by pipeline;It is described sweet Oily separating mechanism includes settling tank, glycerol settling zone, density sensor, controller, automatic valve and glycerol receiving tank, the glycerol Settling zone is located at the bottommost of settling tank and is linked to be an entirety with settling tank, and density sensor insertion is used in glycerol settling zone In measurement material density, the bottom of the glycerol settling zone is connected to the glycerol being disposed below after connecting automatic valve with pipeline and connects Closed cans, the input signal cable of the controller is connected to density sensor, output signal line is connected to automatic valve;The dealcoholysis again Mechanism includes again dealcoholysis feed pump, again dealcoholysis falling film heating flash vessel, spiral plate cooler and surge tank, from the settling tank Side introduction pipe is connect after dealcoholysis feed pump again with the top of dealcoholysis falling film heating flash vessel again, and from this, dealcoholysis falling liquid film adds again Methanol efferent duct is drawn in the side of heat-lightening steaming device, connect after spiral plate cooler with the top of surge tank, the bottom of surge tank Recycling methanol tank is passed to by pipeline, after the bottom of the falling film heating flash vessel of dealcoholysis again connects tubulation cooler by pipeline Pass to coarse biodiesel storage tank;The pre- dealcoholysis mechanism connects very with the top of the surge tank of dealcoholysis mechanism again each by pipeline Sky pump.
Above controller was provided by Longyan Tian Hong computer technology Co., Ltd in 2014, included the macro industrial configuration in day Software, CompanyAddress are Longyan commercial affairs operation centres F 404, belong to the prior art.Its main function be receive and process it is close The signal of sensor transmissions, then output order are spent to automatic valve, when specific gravity is greater than the set value the upper limit, automatic valve is opened, when Automatic valve is closed when specific gravity is lower than setting value lower limit.
Coarse biodiesel of the present invention slows down the technical characterstic of the method and device of back reaction and has the beneficial effect that:
1, coarse biodiesel empties glycerol before thorough dealcoholysis, reduces the generation of coarse biodiesel back reaction, improves Conversion ratio;
2, the content for reducing monoglyceride in coarse biodiesel improves the quality of biodiesel;
3, the impurity contents such as glycerol are few in coarse biodiesel, can reduce equipment wash number, improve utilization rate of equipment and installations;
4, steam service efficiency is improved, steam consumption is reduced;
5, the apparatus structure is simple, production is low with maintenance cost, easy to operate efficiently.
Detailed description of the invention
Fig. 1 is the apparatus structure schematic diagram that coarse biodiesel reduces back reaction in the present invention.
Appended drawing reference: pre- dealcoholysis feed pump 1, pre- dealcoholysis falling film heating flash vessel 2, spiral plate cooler 3, surge tank 4, true Sky pump 5, settling tank 6, glycerol settling zone 7, density sensor 8, controller 9, automatic valve 10, glycerol receiving tank 11, again dealcoholysis Feed pump 12, again dealcoholysis falling film heating flash vessel 13, tubulation cooler 14, coarse biodiesel storage tank 15, recycling methanol tank 16.
Specific embodiment
The method and device for slowing down back reaction to coarse biodiesel of the present invention with reference to the accompanying drawings and detailed description is made It is further described.
Shown in Fig. 1, the device that coarse biodiesel of the invention slows down back reaction includes pre- dealcoholysis mechanism, glycerol separating mechanism Dealcoholysis mechanism again, three are connected in series;The pre- dealcoholysis mechanism includes pre- dealcoholysis feed pump 1, the flash distillation of pre- dealcoholysis falling film heating Device 2, spiral plate cooler 3 and surge tank 4, the discharging of the import connection biodiesel synthesis reaction vessel of the pre- dealcoholysis feed pump 1 Mouthful, the outlet of pre- dealcoholysis feed pump 1 is connected to the top of pre- dealcoholysis falling film heating flash vessel 2 with pipeline, from the pre- dealcoholysis falling liquid film Methanol efferent duct is drawn in the side of heating flash evaporation device 2, connect after spiral plate cooler 3 with the top of surge tank 4, surge tank 4 Bottom by pipeline pass to recycling methanol tank 16, the bottom of the pre- dealcoholysis falling film heating flash vessel 2 is connected to by pipeline The glycerol separating mechanism;The glycerol separating mechanism include settling tank 6, glycerol settling zone 7, density sensor 8, controller 9, Automatic valve 10 and glycerol receiving tank 11, the glycerol settling zone 7 are located at the bottommost of settling tank 6 and are linked to be one with settling tank 6 It is whole, for measuring material density in the density sensor 8 insertion glycerol settling zone 7, the bottom pipeline of the glycerol settling zone 7 It is connected to the glycerol receiving tank 11 being disposed below after connection automatic valve 10, the input signal cable of the controller 9 is connected to close Degree sensor 8, output signal line are connected to automatic valve 10;The mechanism of dealcoholysis again includes dealcoholysis feed pump 12, again dealcoholysis again Falling film heating flash vessel 13, spiral plate cooler 3 and surge tank 4, from the side introduction pipe of the settling tank 6 through dealcoholysis again into It connect after material pump 12 with the top of dealcoholysis falling film heating flash vessel 13 again, draws from the side of the dealcoholysis falling film heating flash vessel 13 again Methanol efferent duct out is connect after spiral plate cooler 3 with the top of surge tank 4, and the bottom of surge tank 4 is passed to back by pipeline Methanol tank 16 is received, the bottom of the falling film heating of the dealcoholysis again flash vessel 13 passes to thick life after connecting tubulation cooler 14 by pipeline Object diesel oil tank 15;The pre- dealcoholysis mechanism connects vacuum pump each by pipeline with the top of the surge tank 4 of dealcoholysis mechanism again 5。
In the present invention coarse biodiesel slow down the method for back reaction specific steps are as follows:
Step 1: pre- dealcoholysis.Contained excessively by pre- dealcoholysis feed pump 1 by what biodiesel synthesis reaction vessel discharge port was discharged The coarse biodiesel of methanol is distilled via steam-heated pre- dealcoholysis falling film heating flash vessel 2, and material divides in falling film heating device After the distribution of cloth disk, flowed to improve heat exchange efficiency, after the heated vaporization of excessive methanol from top to bottom along inner tubal wall with filminess It is separated with coarse biodiesel, leads to the cooling of spiral plate cooler 3, methanol after cooling flows into recycling methanol tank after surge tank 4 16, complete pre- dealcoholysis;Surge tank 4 vacuumizes the methanol extraction after can making vaporization using vacuum pump 5 much sooner;
Step 2: separation glycerol.The coarse biodiesel of pre- dealcoholysis enters settling tank 6, since methanol contains in pre- dealcoholysis glycerol Amount less, density it is big, bottom glycerol settling zone 7 can be separated very well and is precipitated to coarse biodiesel in settling tank, passes through precipitating 8 real-time measurement of density sensor in area simultaneously transmits signal into controller 9, after via controller processing again will instruction output to from Movable valve 10, adjusts the open and close of automatic valve 10, and separation gives off glycerol into glycerol receiving tank 11;
Step 3: dealcoholysis again.Still there is part methanol in coarse biodiesel after pre- dealcoholysis and separation glycerol, in order to reduce Influence of production is distilled to subsequent processing, dealcoholysis again need to be carried out;Using dealcoholysis feed pump 12 again by the coarse biometric bavin of separated glycerol Oil by the steam heated falling film heating of dealcoholysis again flash vessel 13 distill, material through in falling film heating device distributing disc be distributed after, Flowed from top to bottom with filminess along inner tubal wall to improve heat exchange efficiency, after the heated vaporization of excessive methanol with coarse biodiesel Separation leads to the cooling of spiral plate cooler 3, and methanol after cooling flows into recycling methanol tank 16 after surge tank 4, and completion takes off again Alcohol;Surge tank 4 vacuumizes the methanol extraction after can making vaporization using vacuum pump 5 much sooner;
Step 4: the coarse biodiesel after dealcoholysis flows automatically to coarse biometric bavin from tubulation cooler 14 is flow to after cooling again Oily storage tank 15.

Claims (2)

1. a kind of method that coarse biodiesel slows down back reaction, it is characterized in that operating according to the following steps:
The pre- dealcoholysis of the first step: by pre- dealcoholysis feed pump by biodiesel synthesis reaction vessel discharge port be discharged containing excessive methanol Coarse biodiesel is distilled via steam-heated pre- dealcoholysis falling film heating flash vessel, and material distributing disc in falling film heating device is distributed Afterwards, flowed from top to bottom along inner tubal wall with filminess to improve heat exchange efficiency, after the heated vaporization of excessive methanol with coarse biometric Diesel oil separation leads to the cooling of spiral plate cooler, and methanol after cooling flows into recycling methanol tank after surge tank, completes pre- de- Alcohol;Surge tank is vacuumized using vacuum pump so that the methanol after vaporizing is extracted out much sooner;
Second step separates glycerol: the coarse biodiesel of pre- dealcoholysis enters settling tank, since methanol content is few, close in pre- dealcoholysis glycerol Degree is big, can separate very well with coarse biodiesel in settling tank and be precipitated to bottom glycerol settling zone, by close in settling zone Degree sensor real-time measurement simultaneously transmits signal into controller, again adjusts instruction output to automatic valve after via controller processing The open and close of automatic valve is saved, separation gives off glycerol into glycerol receiving tank;
Third step dealcoholysis again: still there is part methanol in the coarse biodiesel after pre- dealcoholysis and separation glycerol, in order to reduce under One process distills Influence of production, need to carry out dealcoholysis again;The coarse biodiesel of separated glycerol is passed through using dealcoholysis feed pump again The steam heated falling film heating flash vessel of dealcoholysis again distillation, material is after distributing disc distribution in falling film heating device, along inner tube Wall is flowed with filminess from top to bottom to improve heat exchange efficiency, is separated, is drawn with coarse biodiesel after the heated vaporization of excessive methanol Cooling to spiral plate cooler, methanol after cooling flows into recycling methanol tank after surge tank, completes dealcoholysis again;Surge tank uses Vacuum pump vacuumizes so that the methanol after vaporizing is extracted out much sooner;
Step 4: the coarse biodiesel after dealcoholysis flows automatically to coarse biodiesel storage tank from tubulation cooler is flow to after cooling again.
2. a kind of device realized coarse biodiesel described in claim 1 and slow down the method for back reaction, it is characterized in that: it includes pre- Dealcoholysis mechanism, glycerol separating mechanism and dealcoholysis mechanism again, three are connected in series;The pre- dealcoholysis mechanism includes pre- dealcoholysis charging The import of pump, pre- dealcoholysis falling film heating flash vessel, spiral plate cooler and surge tank, the pre- dealcoholysis feed pump connects biodiesel The discharge port of synthesis reaction vessel, the outlet of pre- dealcoholysis feed pump are connected to the top of pre- dealcoholysis falling film heating flash vessel with pipeline, Methanol efferent duct is drawn from the side of the pre- dealcoholysis falling film heating flash vessel, is connected after spiral plate cooler with the top of surge tank It connects, the bottom of surge tank passes to recycling methanol tank by pipeline, and the bottom of the pre- dealcoholysis falling film heating flash vessel passes through pipeline It is connected to the glycerol separating mechanism;The glycerol separating mechanism includes settling tank, glycerol settling zone, density sensor, control Device, automatic valve and glycerol receiving tank, the glycerol settling zone are located at the bottommost of settling tank and are linked to be an entirety with settling tank, For measuring material density in density sensor insertion glycerol settling zone, the bottom of the glycerol settling zone is connected automatic with pipeline The glycerol receiving tank being disposed below is connected to after valve, the input signal cable of the controller is connected to density sensor, output Signal wire is connected to automatic valve;The mechanism of dealcoholysis again includes again dealcoholysis feed pump, again dealcoholysis falling film heating flash vessel, spiral Plate cooler and surge tank dodge after dealcoholysis feed pump again with dealcoholysis falling film heating again from the side introduction pipe of the settling tank The top of steaming device connects, and methanol efferent duct is drawn from the side of the dealcoholysis falling film heating flash vessel again, after spiral plate cooler It is connect with the top of surge tank, the bottom of surge tank passes to recycling methanol tank, the falling film heating of the dealcoholysis again flash distillation by pipeline The bottom of device passes to coarse biodiesel storage tank after connecting tubulation cooler by pipeline;The pre- dealcoholysis mechanism and again dealcoholysis mechanism Surge tank top each by pipeline connect vacuum pump.
CN201811318366.8A 2018-11-07 2018-11-07 Coarse biodiesel slows down the method and device of back reaction Pending CN109207210A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113881507A (en) * 2021-11-12 2022-01-04 龙岩卓越新能源股份有限公司 Device for producing biodiesel by continuous ester exchange

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104353257A (en) * 2014-10-30 2015-02-18 厦门卓越生物质能源有限公司 Heating flash distillation device for biodiesel
CN105833556A (en) * 2016-06-02 2016-08-10 龙岩卓越新能源股份有限公司 Method and device for continuous dealcoholization of crude biodiesel
CN206799571U (en) * 2017-05-24 2017-12-26 龙岩卓越新能源股份有限公司 Ester exchange automatic-discharging glycerine device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104353257A (en) * 2014-10-30 2015-02-18 厦门卓越生物质能源有限公司 Heating flash distillation device for biodiesel
CN105833556A (en) * 2016-06-02 2016-08-10 龙岩卓越新能源股份有限公司 Method and device for continuous dealcoholization of crude biodiesel
CN206799571U (en) * 2017-05-24 2017-12-26 龙岩卓越新能源股份有限公司 Ester exchange automatic-discharging glycerine device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113881507A (en) * 2021-11-12 2022-01-04 龙岩卓越新能源股份有限公司 Device for producing biodiesel by continuous ester exchange

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Application publication date: 20190115