CN105586154A - Continuous esterification method for preparing biodiesel from waste grease - Google Patents
Continuous esterification method for preparing biodiesel from waste grease Download PDFInfo
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- CN105586154A CN105586154A CN201511028355.2A CN201511028355A CN105586154A CN 105586154 A CN105586154 A CN 105586154A CN 201511028355 A CN201511028355 A CN 201511028355A CN 105586154 A CN105586154 A CN 105586154A
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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
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- 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
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- 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
The invention discloses a continuous esterification method for preparing biodiesel from waste grease. According to the method, a continuous esterification reaction tower is utilized as a main reaction unit to realize continuous production in the whole esterification reaction process under the normal pressure condition, the production efficiency of the biodiesel is greatly improved, heat produced in the reaction process is used for preheating fine methanol and the waste grease, so that the heat is recycled, energy consumption is reduced, meanwhile, unreacted methanol is recycled, and the production cost is reduced. The acid value of the utilized raw material has a wide range and ranges from 15 mgKOH/g to 180 mgKOH/g, the dosage of a catalyst is small, the catalyst can be recycled and has little corrosion on equipment, the reaction time is short, the energy consumption is low, the production cost is low, the yield of coarse methyl ester is high, waste animal and plant grease with a high acid value can be subjected to one-time esterification until the acid value is lower than 1 mgKOH/g, then the waste animal and plant grease is directly subjected to next ester exchange reaction for preparation of the biodiesel, and the continuous esterification method is suitable for industrial production of the biodiesel.
Description
Technical field
The invention belongs to the preparing technical field of biodiesel, be specifically related to one and utilize waste grease to prepare biological bavinThe continuous esterification method of oil.
Background technology
Biodiesel refers to the compression ignition engine that can be used for of producing with the renewable biological source such as plant, animal fatClean alternative fuel. From chemical composition, biodiesel is a series of LCFA methyl esters or ethyl ester, isThe petrifaction diesel substitute of high-quality, have the title of " green diesel ". In recent years, due to the rising of oil price, petrochemical industryThe series of environmental problems of the non-renewable and generation of the energy, biodiesel becomes the main alternative energy source of researchOne of.
Preparation biodiesel mainly adopt chemical method produce, animal and plant grease reacts with methyl alcohol, acidity orUnder the effect of person's base catalyst, there is esterification, generate corresponding fatty acid methyl ester, then through techniques such as washingsObtain biodiesel. Affected by many factors, be engaged at present the enterprise of production of biodiesel aspect technology inputShortcoming to some extent, mostly manufacturing enterprise's technical merit is comparatively low, product yield all the time below 85%, energy consumptionThe disposable quality of height and biodiesel cannot ensure to reach up-to-date GB. Part producing enterprise is for meeting GB and useFamily requirement, in esterification technique, adopt improve reaction pressure (> 0.4MPa), segmentation acid discharge slag add again methyl alcohol andThe measures such as catalyst are to reduce the acid number after esterification, but this kind of technique also can only be by esterification endpoint acid numberDrop to 2.0mgKOH/g left and right. Because most producer is used sulphur acid as catalyst, therefore must adopt enamel simultaneouslyReactor is as supporting reactor, and the operating pressure of general enamel reaction still is 0.25MPa, and compressive reaction existsLarger potential safety hazard, and waste heat recovery is not done in this workshop section by each producer.
Summary of the invention
Technical problem to be solved by this invention is to overcome esterification in existing biodiesel preparation technology and existsShortcoming, provide that a kind of production cost is low, energy consumption is low, production efficiency is high, utilize waste grease to prepare biodieselContinuous esterification method.
Solving the problems of the technologies described above adopted technical scheme is: by the oil pump pump of the waste grease in feedstock oil storage tankEnter in feedstock oil heat exchanger and be preheated to 50～60 DEG C, the waste grease after preheating is heated to through feedstock oil steam heaterAfter 70～80 DEG C, enter in oil-water mixer and mix with the hot water of its quality 5%～10%, then enter washing agitator tankFully washing, removes water by centrifugation in washing agitator tank bottom suction butterfly centrifugal machine after washing; RemainingOil enters falling liquid film dehydrating tower after washing oil vapour heater is heated to 100～110 DEG C, deviates from after residual moisture by pumpIn suction Hi-mixer, after mixing with esterification catalyst, enter in pre-esterification reactor device; Refined methanol is through heat exchange of methanolAfter device preheating, enter and in methyl alcohol heater, be heated to gasification, a part of gasification of methanol is from pre-esterification reactor device bottomGas-phase methanol pipe enters in pre-esterification reactor device, another part gasification of methanol is from the every Jie Tajie's of continuous esterification towerMethyl alcohol jet pipe sprays in continuous esterification tower; Heating steam coil pipe control pre-esterification reactor in pre-esterification reactor deviceTemperature in device is 100～110 DEG C, and oil is extracted out and entered continuous esterification tower continuously from pre-esterification reactor device bottom,Oil overflows to next Jie Tajie by the overflow pipe of a upper Jie Tajie of continuous esterification tower, until overflow to continuous esterAt the bottom of changing the tower of reaction tower, the temperature in the heating steam coil pipe control continuous esterification tower in continuous esterification towerBe 100～110 DEG C, the thick methyl esters that reaction generates pumps into spinning liquid by the discharging opening of continuous esterification tower bottom by oil pumpSeparator is isolated after esterification catalyst, enters feedstock oil heat exchanger and waste grease heat exchange, the thick methyl esters after heat exchangeEnter ester exchange reaction; The steam generating in pre-esterification reactor device and continuous esterification tower course of reaction and not anti-The gasification of methanol of answering enters heat exchange of methanol device after the demister oil removing of pre-esterification reactor device and continuous esterification towerWith refined methanol heat exchange, the steam after heat exchange and unreacted gasification of methanol enter methanol fractionation system and purify.
Above-mentioned continuous esterification tower is preferably made up of 8～15 Jie Tajie, and every Jie Tajie is an independently reactionUnit.
The mixture that above-mentioned esterification catalyst preferred acid and the mass ratio of erosion resistant agent are 1:0.01～0.15, described inAcid be pyrovinic acid, ethylsulfonic acid or chlorosulfonic acid, erosion resistant agent is phosphate monoester, polyethers phosphate ester acid or alkynes thirdBase alcohol, the addition of esterification catalyst preferably waste grease quality 0.1%～0.5%.
Above-mentioned waste grease is that acid number is waste oil, hogwash fat or the acidification oil of 15～180mgKOH/g.
Beneficial effect of the present invention mainly contains the following aspects:
1, raw material acid number is extensive, is applicable to the animals and plants waste grease production biodiesel of different acid numbers; Reaction isSynthesis under normal pressure, requires low to equipment material; Catalyst amount is few, is only 1/10 left and right of sulfuric acid, catalyst pairThe corrosivity of equipment is little, does not have other side reaction products to generate, almost without acid sludge processing, without environmental protection in course of reactionPressure, the yield of biodiesel can exceed 2%～5% while making catalyst than use sulfuric acid, and reaction finishes rear isolatedEsterification catalyst is reusable.
2, the water that in esterification process, excessive gas-phase methanol generates reaction is taken reaction system out of, accelerates positive reaction and entersOK, effectively Reaction time shorten, has saved energy consumption; The water that reaction generates and unreacted gas-phase methanol are passed through to reclaim,Can recycle, save methanol usage; The water that unreacted gas-phase methanol and reaction generate transfers heat toRefined methanol, has greatly reduced steam consumption, has saved cost.
3,, compared with conventional liquid phase reactor, gas-phase methanol pipe and the continuous esterification tower of pre-reactor bottom are eachThe methyl alcohol jet pipe of tower joint makes methyl alcohol good dispersion, has increased the mixability of gas-phase methanol and waste grease, liquid phaseContact interface is large, has improved esterification efficiency.
4, the present invention can become the disposable esterification of high acid value (15～180mgKOH/g) animal and plant waste greaseAcid number is less than 1mgKOH/g, without further deacidification value, for post-order process provides the semi-finished product of high-quality and productYield has improved 0.5%～1%.
5, the present invention is taking continuous esterification tower as main reaction unit, broken through waste grease continuous esterificationA production difficult problem, makes the production of biodiesel can realize serialization completely, automation, has greatly improved biodieselProduction efficiency, reduced energy consumption.
Brief description of the drawings
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in more detail, but protection scope of the present invention not only forIn these embodiment.
Embodiment 1
As shown in Figure 1, the waste oil that is 120mgKOH/g by 100 tons of acid numbers adds in feedstock oil storage tank 1,Utilize oil pump with the flow of 10 tons of/hour, waste oil to be pumped in feedstock oil heat exchanger 3 and is preheated to 50～60 DEG C, thenAfter feedstock oil steam heater 2 is heated to 75 DEG C, enter in oil-water mixer 4, the hot water of 75 DEG C with 0.5 ton/Hour flow enter oil-water mixer 4 and waste oil fully mixes, then flow into washing agitator tank 5 and fully wash,After washing continuously by washing agitator tank 5 bottoms by pump with in the flow suction butterfly centrifugal machine 6 of 10.5 tons/hour fromThe heart separates except anhydrating and impurity, and it is de-that remaining oil enters falling liquid film after washing oil vapour heater 7 is heated to 100 DEG CWater tower 14, deviates from after residual moisture by pump suction Hi-mixer 8, and esterification catalyst was with the stream of 30kg/ hourAmount enters after Hi-mixer 8 and the abundant mixing of oil, enters in pre-esterification reactor device 11 wherein esterification catalystIt is the mixture that pyrovinic acid and phosphate monoester mass ratio are 1:0.1. Open the stirring dress of pre-esterification reactor device 11Put and attemperating unit the temperature in the heating steam coil pipe control pre-esterification reactor device 11 in pre-esterification reactor device 11It is 100～110 DEG C. Refined methanol enters in methyl alcohol heater 12 and is heated to gasify after 13 preheatings of heat exchange of methanol device,Part gasification of methanol is with 1m3It is anti-that the flow velocity of/h enters pre-esterification from the gas-phase methanol pipe of pre-esterification reactor device 11 bottomsAnswer in device 11, the gasification of methanol good dispersion that gas-phase methanol pipe flows out, large with oily contact area, make methyl alcohol energyEnough and oily fully haptoreaction, Reaction time shorten. After oil in pre-esterification reactor device 11 and methyl alcohol haptoreaction,From pre-esterification reactor device 11 bottoms with the flow of 10 tons/hour by pump suction continuous esterification tower 10, the company of unlatchingThe temperature regulating device of continuous esterification reaction tower 10, the heating steam coil pipe control continuous esterification in continuous esterification tower 10Temperature in reaction tower 10 is 100～110 DEG C. Continuous esterification tower 10 is made up of 10 Jie Tajie, every joint towerJoint is an independently reaction member, and the oil in suction continuous esterification tower 10 is by continuous esterification tower 10The overflow pipe of a upper Jie Tajie overflows to next Jie Tajie, until at the bottom of overflowing to the tower of continuous esterification tower 10.Another part gasification of methanol in methyl alcohol heater 12 is with 2m3The flow velocity of/h is from the every joint tower of continuous esterification tower 10The methyl alcohol jet pipe of joint sprays in continuous esterification tower 10, the gasification of methanol good dispersion of methyl alcohol jet pipe ejection, withOil contact area large, make methyl alcohol can with the abundant haptoreaction of oil, Reaction time shorten. Continuous esterification towerThe thick methyl esters generating after oil in 10 and methyl alcohol haptoreaction by the discharging opening of continuous esterification tower 10 bottoms by oilPump pumps in cyclone hydraulic separators 9 with the flow of 10 tons/hour, and isolated esterification catalyst is reused, thick firstEster is by the discharging opening at cyclone hydraulic separators 9 tops by pump suction feedstock oil heat exchanger 3 and waste grease heat exchange, and collection is changedThick methyl esters after heat enters ester exchange reaction. In pre-esterification reactor device 11 and continuous esterification tower 10 courses of reactionThe steam generating and unreacted gasification of methanol are through the foam removal of pre-esterification reactor device 11 and continuous esterification tower 10After device oil removing, enter heat exchange of methanol device 13 and refined methanol heat exchange, the steam after heat exchange and unreacted gasification of methanolEntering methanol fractionation system purifies.
The acid number of the thick methyl esters that the present embodiment is collected is less than 1mgKOH/g, and the conversion ratio of methyl esters is 98%.
Embodiment 2
As shown in Figure 1, the waste oil that is 120mgKOH/g by 100 tons of acid numbers adds in feedstock oil storage tank 1,Utilize oil pump with the flow of 10 tons of/hour, waste oil to be pumped in feedstock oil heat exchanger 3 and is preheated to 50～60 DEG C, thenAfter feedstock oil steam heater 2 is heated to 75 DEG C, enter in oil-water mixer 4, the hot water of 75 DEG C with 0.7 ton/Hour flow enter oil-water mixer 4 and waste oil fully mixes, then flow into washing agitator tank 5 and fully wash,After washing continuously by washing agitator tank 5 bottoms by pump with in the flow suction butterfly centrifugal machine 6 of 10.7 tons/hour fromThe heart separates except anhydrating and impurity, and it is de-that remaining oil enters falling liquid film after washing oil vapour heater 7 is heated to 100 DEG CWater tower 14, deviates from after residual moisture by pump suction Hi-mixer 8, and esterification catalyst was with the stream of 30kg/ hourAmount enters after Hi-mixer 8 and the abundant mixing of oil, enters in pre-esterification reactor device 11 wherein esterification catalystIt is the mixture that pyrovinic acid and phosphate monoester mass ratio are 1:0.05. Open the stirring dress of pre-esterification reactor device 11Put and attemperating unit the temperature in the heating steam coil pipe control pre-esterification reactor device 11 in pre-esterification reactor device 11It is 100～110 DEG C. Refined methanol enters in methyl alcohol heater 12 and is heated to gasify after 13 preheatings of heat exchange of methanol device,Part gasification of methanol is with 1.2m3The flow velocity of/h enters pre-esterification from the gas-phase methanol pipe of pre-esterification reactor device 11 bottomsIn reactor 11, the gasification of methanol good dispersion that gas-phase methanol pipe flows out, large with oily contact area, make methyl alcoholCan with the abundant haptoreaction of oil, Reaction time shorten. Oil in pre-esterification reactor device 11 and methyl alcohol haptoreactionAfter, from pre-esterification reactor device 11 bottoms with the flow of 10 tons/hour by pump suction continuous esterification tower 10, openOpen the temperature regulating device of continuous esterification tower 10, the heating steam coil pipe control in continuous esterification tower 10 is continuousTemperature in esterification reaction tower 10 is 100～110 DEG C. Continuous esterification tower 10 is made up of 8 Jie Tajie, every jointTower joint is an independently reaction member, and the oil in suction continuous esterification tower 10 is by continuous esterification tower 10The overflow pipe of a upper Jie Tajie overflow to next Jie Tajie, until at the bottom of overflowing to the tower of continuous esterification tower 10.Another part gasification of methanol in methyl alcohol heater 12 is with 2.5m3The flow velocity of/h is from the every joint of continuous esterification tower 10The methyl alcohol jet pipe of tower joint sprays in continuous esterification tower 10, the gasification of methanol good dispersion of methyl alcohol jet pipe ejection,Large with oily contact area, make methyl alcohol can with the abundant haptoreaction of oil, Reaction time shorten. Continuous esterificationThe thick methyl esters generating after oil in tower 10 and methyl alcohol haptoreaction by the discharging opening of continuous esterification tower 10 bottoms byOil pump pumps in cyclone hydraulic separators 9 with the flow of 10 tons/hour, and isolated esterification catalyst is reused, thickMethyl esters, is collected by pump suction feedstock oil heat exchanger 3 and waste grease heat exchange by the discharging opening at cyclone hydraulic separators 9 topsThick methyl esters after heat exchange enters ester exchange reaction. Pre-esterification reactor device 11 and continuous esterification tower 10 courses of reactionThe steam of middle generation and unreacted gasification of methanol remove through pre-esterification reactor device 11 and continuous esterification tower 10After the oil removing of foam device, enter heat exchange of methanol device 13 and refined methanol heat exchange, the steam after heat exchange and unreacted gasification firstAlcohol enters methanol fractionation system and purifies.
The acid number of the thick methyl esters that the present embodiment is collected is less than 1mgKOH/g, and the conversion ratio of methyl esters is 98.3%.
Embodiment 3
As shown in Figure 1, the waste oil that is 120mgKOH/g by 100 tons of acid numbers adds in feedstock oil storage tank 1,Utilize oil pump with the flow of 10 tons of/hour, waste oil to be pumped in feedstock oil heat exchanger 3 and is preheated to 50～60 DEG C, thenAfter feedstock oil steam heater 2 is heated to 75 DEG C, enter in oil-water mixer 4, the hot water of 75 DEG C with 1 ton/littleTime flow enter oil-water mixer 4 and waste oil fully mixes, then flow into washing agitator tank 5 and fully wash,After washing continuously by washing agitator tank 5 bottoms by pump with centrifugal in the flow suction butterfly centrifugal machine 6 of 11 tons/hourSeparate except anhydrating and impurity, remaining oil enters falling liquid film dehydration after washing oil vapour heater 7 is heated to 100 DEG CTower 14, deviates from after residual moisture by pump suction Hi-mixer 8, and esterification catalyst was with the flow of 50kg/ hourEnter after the abundant mixing of Hi-mixer 8 and oil, enter in pre-esterification reactor device 11, wherein esterification catalyst isThe mixture that pyrovinic acid and phosphate monoester mass ratio are 1:0.05. Open the agitating device of pre-esterification reactor device 11And attemperating unit, the temperature in the heating steam coil pipe control pre-esterification reactor device 11 in pre-esterification reactor device 11 is100～110 DEG C. Refined methanol enters in methyl alcohol heater 12 and is heated to gasify after 13 preheatings of heat exchange of methanol device, and onePartial gasification methyl alcohol is with 1.2m3It is anti-that the flow velocity of/h enters pre-esterification from the gas-phase methanol pipe of pre-esterification reactor device 11 bottomsAnswer in device 11, the gasification of methanol good dispersion that gas-phase methanol pipe flows out, large with oily contact area, make methyl alcohol energyEnough and oily fully haptoreaction, Reaction time shorten. After oil in pre-esterification reactor device 11 and methyl alcohol haptoreaction,From pre-esterification reactor device 11 bottoms with the flow of 10 tons/hour by pump suction continuous esterification tower 10, the company of unlatchingThe temperature regulating device of continuous esterification reaction tower 10, the heating steam coil pipe control continuous esterification in continuous esterification tower 10Temperature in reaction tower 10 is 100～110 DEG C. Continuous esterification tower 10 is made up of 15 Jie Tajie, every joint towerJoint is an independently reaction member, and the oil in suction continuous esterification tower 10 is by continuous esterification tower 10The overflow pipe of a upper Jie Tajie overflows to next Jie Tajie, until at the bottom of overflowing to the tower of continuous esterification tower 10.Another part gasification of methanol in methyl alcohol heater 12 is with 2.5m3The flow velocity of/h is from the every joint of continuous esterification tower 10The methyl alcohol jet pipe of tower joint sprays in continuous esterification tower 10, the gasification of methanol good dispersion of methyl alcohol jet pipe ejection,Large with oily contact area, make methyl alcohol can with the abundant haptoreaction of oil, Reaction time shorten. Continuous esterificationThe thick methyl esters generating after oil in tower 10 and methyl alcohol haptoreaction by the discharging opening of continuous esterification tower 10 bottoms byOil pump pumps in cyclone hydraulic separators 9 with the flow of 10 tons/hour, and isolated esterification catalyst is reused, thickMethyl esters, is collected by pump suction feedstock oil heat exchanger 3 and waste grease heat exchange by the discharging opening at cyclone hydraulic separators 9 topsThick methyl esters after heat exchange enters ester exchange reaction. Pre-esterification reactor device 11 and continuous esterification tower 10 courses of reactionThe steam of middle generation and unreacted gasification of methanol remove through pre-esterification reactor device 11 and continuous esterification tower 10After the oil removing of foam device, enter heat exchange of methanol device 13 and refined methanol heat exchange, the steam after heat exchange and unreacted gasification firstAlcohol enters methanol fractionation system and purifies.
The acid number of the thick methyl esters that the present embodiment is collected is less than 1mgKOH/g, and the conversion ratio of methyl esters is 98.5%.
Embodiment 4
In embodiment 1, esterification catalyst used such as uses at the quality of quality ethylsulfonic acid and polyethers phosphate ester acidReplace than the mixture for 1:0.01, other steps are identical with embodiment 1, obtain acid number and are less than 1mgKOH/g'sThick methyl esters, the yield of methyl esters is 98%.
Embodiment 5
In embodiment 1, esterification catalyst used such as uses at the mass ratio of quality chlorosulfonic acid and polyethers phosphate ester acidReplace for the mixture of 1:0.05, other steps are identical with embodiment 1, obtain acid number and are less than the thick of 1mgKOH/gMethyl esters, the conversion ratio of methyl esters is 98.2%.
Embodiment 6
In embodiment 1, esterification catalyst used such as uses to be at the mass ratio of quality chlorosulfonic acid and propargyl ethanolThe mixture of 1:0.15 is replaced, and other steps are identical with embodiment 1, obtain the thick first that acid number is less than 1mgKOH/gEster, the conversion ratio of methyl esters is 97.8%.
Claims (5)
1. utilize waste grease to prepare a continuous esterification method for biodiesel, it is characterized in that: by raw materialWaste grease in oil tank (1) pumps in feedstock oil heat exchanger (3) and is preheated to 50～60 DEG C with oil pump, pre-Waste grease after heat enters oil-water mixer (4) after feedstock oil steam heater (2) is heated to 70～80 DEG CIn mix with the hot water of its quality 5%～10%, then enter washing agitator tank (5) fully wash, after washing by waterWash centrifugation in agitator tank (5) bottom suction butterfly centrifugal machine (6) and remove water; Remaining oil is through washing oilAfter steam heater (7) is heated to 100～110 DEG C, enter falling liquid film dehydrating tower (14), deviate from after residual moisture by pumpIn suction Hi-mixer (8), after mixing with esterification catalyst, enter in pre-esterification reactor device (11); Essence firstAlcohol enters in methyl alcohol heater (12) and is heated to gasify after heat exchange of methanol device (13) preheating, part gasification firstAlcohol from the gas-phase methanol pipe in pre-esterification reactor device (11) bottom enter in pre-esterification reactor device (11), another portionDivide gasification of methanol to spray into continuous esterification tower (10) from the methyl alcohol jet pipe of the every Jie Tajie of continuous esterification tower (10)In; Temperature in heating steam coil pipe control pre-esterification reactor device (11) in pre-esterification reactor device (11) is100～110 DEG C, oil is extracted out and is entered continuous esterification tower (10) continuously from pre-esterification reactor device (11) bottom,Oil overflows to next Jie Tajie by the overflow pipe of a upper Jie Tajie of continuous esterification tower (10), until overflow toAt the bottom of the tower of continuous esterification tower (10), the heating steam coil pipe control in continuous esterification tower (10) is continuousTemperature in esterification reaction tower (10) is 100～110 DEG C, and the thick methyl esters that reaction generates is by continuous esterification tower (10)The discharging opening of bottom pumps into cyclone hydraulic separators (9) by oil pump and isolates after esterification catalyst, enters feedstock oil heat exchangeDevice (3) and waste grease heat exchange, the thick methyl esters after heat exchange enters ester exchange reaction; Pre-esterification reactor device (11)Anti-through pre-esterification with the steam generating in continuous esterification tower (10) course of reaction and unreacted gasification of methanolAfter answering the demister oil removing of device (11) and continuous esterification tower (10), enter heat exchange of methanol device (13) and smart firstAlcohol heat exchange, the steam after heat exchange and unreacted gasification of methanol enter methanol fractionation system and purify.
2. the continuous esterification method of utilizing waste grease to prepare biodiesel according to claim 1, its spyLevy and be: described continuous esterification tower (10) is made up of 8～15 Jie Tajie, every Jie Tajie is an independenceReaction member.
3. the continuous esterification method of utilizing waste grease to prepare biodiesel according to claim 1 and 2,It is characterized in that: described esterification catalyst is the mixture that the mass ratio of acid and erosion resistant agent is 1:0.01～0.15,Described acid is pyrovinic acid, ethylsulfonic acid or chlorosulfonic acid, erosion resistant agent be phosphate monoester, polyethers phosphate ester acid orPropargyl ethanol.
4. the continuous esterification method of utilizing waste grease to prepare biodiesel according to claim 3, its spyLevy and be: the addition of described esterification catalyst is 0.1%～0.5% of waste grease quality.
5. the continuous esterification method of utilizing waste grease to prepare biodiesel according to claim 1, its spyLevy and be: described waste grease is that acid number is waste oil, hogwash fat or the acidification oil of 15～180mgKOH/g.
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Cited By (6)
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| CN107860249A (en) * | 2017-12-15 | 2018-03-30 | 重庆方盛净化设备有限公司 | Waste oil regeneration rectifying catalysis system residual heat using device |
| CN108329207A (en) * | 2018-05-03 | 2018-07-27 | 凯瑞环保科技股份有限公司 | A kind of device and method producing fatty acid methyl ester using catalytic distillation technology |
| CN110093212A (en) * | 2019-04-23 | 2019-08-06 | 龙岩卓越新能源股份有限公司 | A kind of method of waste oil continuous esterification production |
| CN111234932A (en) * | 2020-02-12 | 2020-06-05 | 常州市金坛区维格生物科技有限公司 | Method for preparing biodiesel by continuous countercurrent esterification reaction |
| CN113549476A (en) * | 2021-07-21 | 2021-10-26 | 四川新源素科技有限公司 | Civil life fuel and preparation method thereof |
| CN113563976A (en) * | 2021-07-21 | 2021-10-29 | 湖北天基生物能源科技发展有限公司 | Gas-phase esterification system of waste grease and method for treating waste grease |
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