CN204841658U - Gas phase reaction prepares biodiesel's device in succession - Google Patents
Gas phase reaction prepares biodiesel's device in succession Download PDFInfo
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- CN204841658U CN204841658U CN201520265282.8U CN201520265282U CN204841658U CN 204841658 U CN204841658 U CN 204841658U CN 201520265282 U CN201520265282 U CN 201520265282U CN 204841658 U CN204841658 U CN 204841658U
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The utility model discloses a gas phase reaction prepares biodiesel's device in succession. The device is including the cauldron that comes unstuck, a reation kettle, the 2nd reation kettle, the 3rd reation kettle, methyl alcohol vaporizer, first flash distillation dealcoholize unit, settling cask, commentaries on classics esterifying kettle, second flash distillation dealcoholize unit and the underpressure distillation tower once connected, a reation kettle is added with the oil through coming unstuck to this method, and gaseous phase methyl alcohol is got into by the 3rd reation kettle, the grease gets into the 2nd reation kettle three reentrant reation kettle by a reation kettle, and the grease that reaction at last is good is discharged by the 3rd reation kettle, gaseous phase methyl alcohol reverse by the third to the second to first, excessive gaseous phase methyl alcohol is discharged by a reation kettle and is got into methanol column purifying and separating by distillation. Reaction grease well obtains finished product biodiesel again through changeing esterification reaction, vacuum distillation at last, and vacuum distillation's residue is plant pitch. The utility model discloses can solve current technology length consuming time, methyl alcohol circulation volume is big, manufacturing cost is high, can not the continuous production scheduling problem.
Description
Technical field
The utility model relates to a kind of preparation of biodiesel, and particularly one utilizes palm acid-soluble oil (PalmAcidOil) continuous gas-phase reaction to prepare the device of biodiesel.
Background technology
Biodiesel also known as fatty acid methyl ester, it be waste animal and vegetable oil, microbial grease etc. as raw material, obtain through esterification, ester exchange reaction with low-carbon alcohols such as methyl alcohol (or ethanol).Biodiesel, with the recyclability of its uniqueness and green, becomes a kind of petroleum diesel substitute of high-quality, is considered to solve global energy crisis, environmental pressure of releiving, and controls one of optimal approach of atmosphere pollution.
At present, the technique that China's suitability for industrialized production biodiesel is comparatively ripe mainly contains " sour one-step method " and " acid-alkali two-step method " two kinds of methods." sour one-step method " technique is generally applicable to the higher acidification oil raw material of acid number, and general northerly production of biodiesel enterprise is comparatively common, but the requirement of the method to equipment is higher, and the reaction time is longer, and can produce a large amount of waste acid water." acid-alkali two-step method " technique is generally applicable to acid number at greases such as the waste oil of below 100mgKOH/g or frying oils, but traditional " acid-alkali two-step method " technique exists that production process is tediously long, production cost is high and to shortcomings such as ester exchange reaction conditional request are high.
Chinese invention patent application 201210165367X discloses a kind of equipment of waste oil conversion biodiesel.Comprise waste oil storage tank, waste oil storage tank connects waste oil glue kettle, waste oil glue kettle connects pans, pans coupled reaction still, inside reactor, agitating device is installed, install chemicals dosing plant above reactor, mounting heater and temperature sensor inside reactor, heater is all connected with controller with described temperature sensor.This utility model is a kind of typical equipment waste oil being processed into biodiesel, but because the waste oil of raw oil material is complicated, moisture impure change is large, single glue kettle process is difficult to ensure reactor continuous seepage, is also difficult to ensure product quality.Someone also adopts hydration degum PROCESS FOR TREATMENT raw material in fats and oils processing, but because producing a large amount of waste water in actual production, is all closed down.
Chinese invention patent application 2010105586393 discloses a kind of process preparing biodiesel, comprises the following steps: grease and monohydric alcohol are supplied to reactor by (A), carries out ester exchange reaction; (B) steam monohydric alcohol from reacted crude product, product is divided into mixed ester phase and glycerine phase or aqueous phase; (C) by mixed ester phase and glycerine phase or aqueous phase separation; (D) part mixed ester is back to after reactor inlet mixes with raw oil material enters reactor; (E) remain mixed ester and glycerine phase or aqueous phase to distill respectively, obtain high purity fatty acid ester and glycerine.The utility model method can obtain the lower biodiesel of acid number by high yield.But the method does not have degumming process, also continuous seepage cannot be ensured.
Utility model content
The utility model object be to overcome prior art can not be suitable for exist in complicated raw material continuous seepage and production process technique length consuming time, methanol loop amount is large, manufacturing cost is high, can not continuous seepage problem, provide a kind of consuming time short, methanol loop amount is little, can contact the device that the continuous gas-phase reaction of production prepares biodiesel.
Palm acid-soluble oil (PalmAcidOil) is the one of common waste cooking oils, is characterized in the scope of acid number at 60mgKOH/g-120mgKOH/g.Of this sort raw material is not suitable for sour one-step method.And because biodiesel raw material used is at present complicated, moisture impure change is large, so adopt continuous processing to be difficult to reach ideal effect.Someone also adopts hydration degum PROCESS FOR TREATMENT raw material in fats and oils processing to remove excessive impurity, but because producing a large amount of waste water in actual production, nearly all forces to close down.The waste acid water process feedstock oil that the utility model adopts course of reaction to produce, remove the impurity in raw material, make material quality unified, apply multiple reactor step-reaction simultaneously, and adopt the method for methyl alcohol and grease backward feed, not only solve the too much problem of raw material impurity but also consume the discharge capacity that sour water decreases sour water.
The utility model course of reaction adopts methyl alcohol and grease backward feed, fresh methanol first with is reacted close to the grease reacted completely, gasify together with the water that excessive methyl alcohol and reaction generate, enter next reactor and grease continues to react, until excessive methyl alcohol and the up-to-date grease reaction entered.Take full advantage of methyl alcohol like this, decrease the ratio that methyl alcohol is excessive, the water taking away again reaction generation makes more easily to carry out.All the utility model electric energy, heat energy, the consumption of methyl alcohol is less, and the structure of device is relatively simple, can continuous seepage production efficiency higher.
The utility model object is achieved through the following technical solutions:
A kind of continuous gas-phase reaction prepares the device of biodiesel, comprise at least three reactors, the still that comes unstuck, the first reactor, the second reactor, the 3rd reactor, methyl alcohol vaporizing device, the first flash distillation dealcoholysis unit, settling tank, transesterification still, the second flash distillation dealcoholysis unit are connected successively with vacuum distillation tower;
Described still upper end of coming unstuck is respectively equipped with charging aperture and acid sludge import, and lower end discharging opening is connected with feedstock oil charging aperture;
The upper end of described first reactor is respectively equipped with feedstock oil charging aperture, catalyst inlet, gaseous phase outlet, and bottom is provided with opening, and gaseous phase outlet is connected with methanol distillation column; Feedstock oil charging aperture is connected with feed pipe;
The upper end of described second reactor is provided with charging aperture and gaseous phase outlet, and bottom is provided with opening; Open communication bottom charging aperture and gaseous phase outlet and the first reactor;
The upper end of described 3rd reactor is provided with charging aperture and gaseous phase outlet, and bottom is provided with opening; Gas-phase methanol import is connected with methyl alcohol vaporizing device, adds fresh gas-phase methanol; Bottom opening is connected with discharge pipe; Gaseous phase outlet is connected with the second reactor bottom opening;
Described discharge pipe is connected with the first flash distillation dealcoholysis unit, first flash distillation dealcoholysis unit is connected with settling tank, settling tank is connected with transesterification still, transesterification still is connected with settling tank or centrifuge, settling tank or centrifuge and the second flash distillation dealcoholysis unit, second flash distillation dealcoholysis unit is connected with vacuum distillation tower, and vacuum distillation tower is respectively equipped with pitch floss hole and product oil floss hole.
For realizing the utility model object further, preferably, the pipeline that described discharge pipe is connected with the first flash distillation dealcoholysis unit is provided with valve.
The pipeline that described first reactor and the second reactor bottom opening are connected with charging aperture and the gaseous phase outlet of the second reactor and the 3rd reactor upper end is respectively provided with valve.
The quantity of described reactor is 4-6; 4th reactor is identical with the connected mode of the 3rd reactor with the second reactor to the connected mode of the 6th reactor.
Described first reactor, the second reactor, the 3rd reactor adopt stainless steel still or glass-lined kettle; Described transesterification still adopts stainless steel still or glass-lined kettle.
Described methyl alcohol vaporizing device adopts tubular heat exchanger or spiral heat exchanger; Described vacuum distillation tower adopts packed tower or plate column.
A method for biodiesel is prepared in the continuous gas phase catalysis esterification of applying described device, comprises the steps:
Step 1: raw oil material is added by charging aperture and comes unstuck in still; Start agitating heating and be warmed up to 60 DEG C-90 DEG C, insulation reaction 1 ± 0.5 hour; Stop stirring, quiescent settling, discharge colloid and the sour water of bottom;
Step 2: the grease through coming unstuck is added the first reactor by feedstock pump by by feedstock oil import, fresh methanol adds the 3rd reactor by the speed of the 15%-30% of feedstock oil after the gasification of methyl alcohol vaporizing device, and catalyst adds in the first reactor by the speed of the 0.1%-5% of feedstock oil by catalyst inlet; Control reactor temperature 100 DEG C-185 DEG C, pressure 0-3Mpa;
Step 3: by controlling the switch size of the blow-off valve of each reactor, adjust the first reactor, the second reactor, the liquid level of the 3rd reactor, liquid level controls between the 1/2-2/3 of reactor height; Detect the acid number of the 3rd reactor grease; When acid number is lower than 2mgKOH/g, open the blow-off valve of the 3rd reactor, start discharging; If acid number is higher than 2mgKOH/g, then improve the liquid level of the first to the three reactor, liquid level is up to 2/3 of all reactors;
Step 4: react with grease after gas-phase methanol enters the 3rd reactor, the water that unreacted excessive methanol and reaction generate enters the bottom of the second reactor from the gaseous phase outlet of the 3rd reactor with the form of gas phase; Gas-phase methanol and grease react further, the water that excessive methyl alcohol and reaction produce is entered the bottom of the first reactor by the gaseous phase outlet of the second reactor with the form of gas phase, methyl alcohol and grease vigorous reaction in the first reactor, have methanol outlet to discharge by the gas phase of the first reactor together with the water that the water that excessive methyl alcohol and reaction generate, raw material are brought into; The pressure controlled in the first reactor is 0-3Mpa;
Step 5: the material that the 3rd reactor is discharged enters the first flash distillation dealcoholysis unit by discharge pipe, deviates from excessive methanol;
Step 6: the grease after dealcoholysis enters settling tank, acid sludge is discharged in sedimentation separation;
Step 7: the grease after deslagging enters transesterification still, adds the methyl alcohol of oil quality 25% ± 10% and the catalyst solution of oil quality 0.1-1.5%; At 65 DEG C ± 5 DEG C reaction 30-60 minute, deviate from excessive methanol; Described catalyst be sulfuric acid, phosphoric acid, p-methyl benzenesulfonic acid, aluminium chloride, iron chloride, boron trifluoride and tin tetrafluoride one or more
Step 8: the glycerine of generation isolated by the transesterification grease completed through natural subsidence or centrifuge.
Step 9: the grease after separation of glycerin, by the second flash distillation dealcoholysis unit, removes remaining Trace Methanol;
Step 10: the grease after dealcoholysis enters vacuum distillation tower and purifies out refined biometric diesel oil from the collection of product oil floss hole, and the residue of vacuum distillation is plant asphalt, discharges from pitch floss hole.
Preferably, raw oil material be waste oil, hogwash fat, palm acid-soluble oil and vegetable oil mill containing one or more in greasyfoot.
Preferably, the time of described quiescent settling is 3-6 hour; The described pressure Wei removing remaining Trace Methanol ?0.08Mpa ± 0.01Mpa, temperature is 110 DEG C ± 10 DEG C.
Relative to prior art, the utility model tool has the following advantages:
1) for the feedstock oil of complexity, the utility model utilizes the acid sludge process feedstock oil of discharging, deviate from most water and impurity, remove the impurity in raw material, make material quality unified, apply multiple reactor step-reaction simultaneously, and adopt the method for methyl alcohol and grease backward feed, not only solve the too much problem of raw material impurity but also consume the discharge capacity that sour water decreases sour water, make that raw material is pure can be suitable for continuous processing.
2) the utility model saves energy consumption, decreases the internal circulating load of methyl alcohol: the utility model methyl alcohol and grease backward feed, and fresh methanol grease that is first and low acid number reacts, the grease reaction of the methyl alcohol that concentration is low and high acid value.This process takes full advantage of methyl alcohol, improves the problem that when single still reacts, methanol loop amount is large.
3) continuous seepage, stable, operative is simple, and labour intensity is low: the utility model continuous feed continuous discharge is simple to operate, stable, and labor strength is low.
4) equipment manufacturing cost low, easily realize automation: the utility model continuous feed continuous discharge, reaction speed is fast, constant product quality.Much larger than output during intermittent reaction of onesize reactor.Methyl alcohol and grease enter reaction system in proportion and are easy to realize automation.
5) methanol loss is low: the utility model excessive methanol is few, and methyl alcohol evaporation capacity and yield all reduce, so methanol loss reduces.
Accompanying drawing explanation
Fig. 1 is the structural representation that continuous gas-phase reaction prepares the device of biodiesel.
Shown in figure: charging aperture 1, acid sludge import 2, the still 3 that comes unstuck, feedstock oil charging aperture 4, catalyst inlet 5, gaseous phase outlet 6, first reactor 7, second reactor 8, the 3rd reactor 9, discharge pipe 10, methyl alcohol vaporizing device 11, first flash distillation dealcoholysis unit 12, settling tank 13, transesterification device 14, second flash distillation dealcoholysis unit 15, vacuum distillation tower 16, pitch floss hole 17, product oil floss hole 18.
Detailed description of the invention
For understanding the utility model better, below in conjunction with drawings and Examples, the utility model is further described, but embodiment of the present utility model is not limit so.
As shown in Figure 1, a kind of continuous gas-phase reaction prepares the device of biodiesel, comprises still 3, first reactor 7, second reactor 8 that comes unstuck, the 3rd reactor 9, methyl alcohol vaporizing device 11, first flash distillation dealcoholysis unit 12, settling tank 13, transesterification still 14, second flash distillation dealcoholysis unit 15 and vacuum distillation tower 16;
Still 3 upper end of coming unstuck is respectively equipped with charging aperture 1 and acid sludge import 2, and lower end discharging opening is connected with feedstock oil charging aperture 4;
The upper end of the first reactor 7 is respectively equipped with feedstock oil charging aperture 4, catalyst inlet 5, gaseous phase outlet 6, and bottom is provided with opening, enters for discharging and methyl alcohol; Gaseous phase outlet 6 is connected with methanol distillation column; Feedstock oil charging aperture 4 is connected with feed pipe;
The upper end of the second reactor 8 is provided with charging aperture and gaseous phase outlet, and bottom is provided with opening; Open communication bottom charging aperture and gaseous phase outlet and the first reactor 7;
The upper end of the 3rd reactor 9 is provided with charging aperture and gaseous phase outlet, and bottom is provided with opening; Gas-phase methanol import is connected with methyl alcohol vaporizing device 11, adds fresh gas-phase methanol; Bottom opening is connected with discharge pipe 10; Gaseous phase outlet is connected with the second reactor 8 bottom opening;
The pipeline that first reactor 7 and the second reactor 8 bottom opening are connected with charging aperture and the gaseous phase outlet of the second reactor 8 and the 3rd reactor 9 upper end is respectively provided with valve.
Discharge pipe 10 is connected with the first flash distillation dealcoholysis unit 12, first flash distillation dealcoholysis unit 12 is connected with settling tank 13, settling tank 13 is connected with transesterification still 14, transesterification still 14 is connected with settling tank or centrifuge, settling tank or centrifuge and the second flash distillation dealcoholysis unit 15, second flash distillation dealcoholysis unit 15 is connected with vacuum distillation tower 16, and vacuum distillation tower 16 is respectively equipped with pitch floss hole 17 and product oil floss hole 18.
The pipeline that discharge pipe 10 is connected with the first flash distillation dealcoholysis unit 12 is provided with valve.
First reactor 7, second reactor 8, the 3rd reactor 9 can adopt stainless steel still or glass-lined kettle.
Methyl alcohol vaporizing device 11 can adopt tubular heat exchanger or spiral heat exchanger; Settling tank 13 is taper settling tank; Transesterification still 14 can adopt stainless steel still or glass-lined kettle; Vacuum distillation tower 16 can adopt packed tower or plate column.
First flash distillation dealcoholysis unit 12 and the second flash distillation dealcoholysis unit 15 all adopt falling film heating device, can quick separating methyl alcohol and a small amount of water, avoid side reaction to produce.
Grease through coming unstuck is added the first reactor 7 by the method that biodiesel is prepared in the continuous gas phase catalysis esterification of the utility model, and gas-phase methanol is entered by the 3rd reactor 9.Grease enters the second reactor 8 by the first reactor 7 and enters the 3rd reactor 9 again, and the grease that final reaction is good is discharged by the 3rd reactor 9; Gas-phase methanol is reverse by the 3rd reactor 9, second reactor 8 to the first reactor 7, and excessive gas-phase methanol is discharged by the first reactor 7 and entered methanol column rectification and purification.Completely reacted grease is again through transesterification, vacuum distillation, and finally obtain refined biometric diesel oil, the residue of vacuum distillation is plant asphalt.Raw oil material of the present utility model can be waste oil, hogwash fat, palmitic acid carburetion and vegetable oil mill containing one or more in greasyfoot.
Embodiment 1
A method for biodiesel is prepared in continuous gas phase catalysis esterification, comprises the steps:
Step 1: get palmitic acid carburetion raw material 1000Kg (acid number 100mgKOH/g, water is assorted is less than 3%), added by charging aperture 1 and come unstuck in still 3; Get gas-phase reaction complete after the acid sludge top mobility good part 100Kg acid sludge import 2 of discharge add and come unstuck in still 3.Start agitating heating and be warmed up to 60 DEG C-90 DEG C, insulation reaction 1 hour.Stop stirring, quiescent settling 3-6 hour, discharge colloid and the sour water of bottom.Top grease enters subsequent processing.
Step 2: the grease through coming unstuck is added first reactor 7 by the speed of 150Kg/h by feedstock oil import 4 by feedstock pump, fresh methanol adds the 3rd reactor 9 by the speed of 35Kg/h after methyl alcohol vaporizing device 11 gasifies, and concentrated sulfuric acid catalyst is added in the first reactor 4 by catalyst inlet 5 by the speed of 0.3Kg/h.Control reactor temperature 105 DEG C-110 DEG C, pressure 0.3Mpa.
Step 3: along with constantly adding of glyceride stock, the material level of the first reactor 7 constantly raises, and opens the blow-off valve of the first reactor 7 to the second reactor 8 punishment in advance when material level reaches the half of reactor time.The material level of same control second reactor 8, to the 3rd reactor 9 punishment in advance.When the 3rd reactor 9 material level reaches a half, detect the acid number of the 3rd reactor 9.When acid number is lower than 2mgKOH/g, open the blow-off valve of the 3rd reactor 9, start discharging.If acid number is higher than 2mgKOH/g, then improve the liquid level of the first to the three reactor, liquid level is the highest can reach 2/3 of all reactors.By controlling the switch size of the blow-off valve of each reactor, adjust the liquid level of the first reactor 7, second reactor the 8, three reactor 9, liquid level is generally between the 1/2-2/3 of reactor height.The blow-off valve can driving each reactor large when the acid number of the 3rd reactor 9 is lower time reduces the material level of each reactor, and when the acid number of the 3rd reactor 9 is higher time, the blow-off valve that turn down each reactor improves the material level of each reactor.Inlet amount, quantity of methyl alcohol are through the general of calculating does not need adjustment, and only need to adjust the material stock in reactor, namely the reaction time just can control the acid number of product.
Step 4: gas-phase methanol enters after the 3rd reactor 9 react with grease, unreacted excessive methanol and the water reacting generation enter the bottom of the second reactor 8 from the gaseous phase outlet of the 3rd reactor 9 with the form of gas phase.Gas-phase methanol and grease react further, the water that excessive methyl alcohol and reaction produce is entered the bottom of the first reactor 7 by the gaseous phase outlet of the second reactor 8 with the form of gas phase, methyl alcohol and grease vigorous reaction in the first reactor 7, have methanol outlet 6 to discharge by the gas phase of the first reactor 7 together with the water that the water that excessive methyl alcohol and reaction generate, raw material are brought into.Control the valve size of gas-phase methanol outlet 6, control the pressure 0.3 ± 0.01Mpa in reactor.Gas-phase methanol directly enters methanol distillation column, adjustment recovery tower, ensures that rectifying methanol content reaches more than 99%.The methyl alcohol reclaimed continues to use.
Step 5: the material that the 3rd reactor 9 is discharged enters the first flash distillation dealcoholysis unit 12 by discharge pipe 10, deviates from excessive methanol.
Step 6: the grease after dealcoholysis enters settling tank 13, acid sludge is discharged in sedimentation separation.
Step 7: the grease after deslagging enters transesterification still 14, adds the methyl alcohol of oil quality 20% and the potassium hydroxide solution of oil quality 0.4%.65 DEG C ± 5 DEG C reactions 30 minutes, deviate from excessive methanol.
Step 8: the glycerine of generation isolated by the transesterification grease completed through natural subsidence or centrifuge.
Step 9: the grease after separation of glycerin, by the second flash distillation dealcoholysis unit 15, at-0.08Mpa, under 110 DEG C of conditions, removes remaining Trace Methanol.
Step 10: the grease after dealcoholysis enters vacuum distillation tower 16 refined biometric diesel oil of purifying out and collects from product oil floss hole 18, and the residue of vacuum distillation is plant asphalt, discharges from pitch floss hole 17.Product oil yield is about 86% of raw oil material quality, and quality can reach the standard of diesel fuel mediation biodiesel (BD100) GB/T20828-2014.
Embodiment 2
A method for biodiesel is prepared in continuous gas phase catalysis esterification, comprises the steps:
Step 1: get waste oil raw material 1000Kg (acid number 70mgKOH/g, water is assorted is less than 3%), added by charging aperture 1 and come unstuck in still 3; Get gas-phase reaction complete after the acid sludge top mobility good part 150Kg acid sludge import 2 of discharge add and come unstuck in still 3.Start agitating heating and be warmed up to 60 DEG C-90 DEG C, insulation reaction 1 hour.Stop stirring, quiescent settling 3-6 hours, discharge colloid and the sour water of bottom.Top grease enters subsequent processing.
Step 2: the grease through coming unstuck is added first reactor 7 by the speed of 150Kg/h by feedstock oil import 4 by feedstock pump, fresh methanol adds the 3rd reactor 9 by the speed of 45Kg/h after methyl alcohol vaporizing device 11 gasifies, and concentrated sulfuric acid catalyst is added in the first reactor 4 by catalyst inlet 5 by the speed of 0.5Kg/h.Control reactor temperature 100 DEG C-105 DEG C, pressure 0.2Mpa.
Step 3: along with constantly adding of glyceride stock, the material level of the first reactor 7 constantly raises, and opens the blow-off valve of the first reactor 7 to the second reactor 8 punishment in advance when material level reaches the half of reactor time.The material level of same control second reactor 8, to the 3rd reactor 9 punishment in advance.When the 3rd reactor 9 material level reaches a half, detect the acid number of the 3rd reactor 9.When acid number is lower than 2mgKOH/g, open the blow-off valve of the 3rd reactor 9, start discharging.If acid number is higher than 2mgKOH/g, then improve the liquid level of the first to the three reactor, liquid level is the highest can reach 2/3 of all reactors.By controlling the switch size of the blow-off valve of each reactor, adjust the liquid level of the first reactor 7, second reactor the 8, three reactor 9, liquid level is generally between 1/2 to 2/3 of reactor height.The blow-off valve can driving each reactor large when the acid number of the 3rd reactor 9 is lower time reduces the material level of each reactor, and when the acid number of the 3rd reactor 9 is higher time, the blow-off valve that turn down each reactor improves the material level of each reactor.Inlet amount, quantity of methyl alcohol are through to calculate generally does not need adjustment, and only need to adjust the material stock in reactor, namely the reaction time just can control the acid number of product.
Step 4: gas-phase methanol enters after the 3rd reactor 9 react with grease, unreacted excessive methanol and the water reacting generation enter the bottom of the second reactor 8 from the gaseous phase outlet of the 3rd reactor 9 with the form of gas phase.Gas-phase methanol and grease react further, the water that excessive methyl alcohol and reaction produce is entered the bottom of the first reactor 7 by the gaseous phase outlet of the second reactor 8 with the form of gas phase, methyl alcohol and grease vigorous reaction in the first reactor 7, have methanol outlet 6 to discharge by the gas phase of the first reactor 7 together with the water that the water that excessive methyl alcohol and reaction generate, raw material are brought into.By controlling the valve size of gas-phase methanol outlet 6, control the pressure 0.2 ± 0.01Mpa in reactor.Gas-phase methanol directly enters methanol distillation column, adjustment recovery tower, ensures that rectifying methanol content reaches more than 99%.The methyl alcohol reclaimed continues to use.
Step 5: the material that the 3rd reactor 9 is discharged enters the first flash distillation dealcoholysis unit 12 by discharge pipe, deviates from excessive methanol.
Step 6: the grease after dealcoholysis enters settling tank 13, acid sludge is discharged in sedimentation separation.
Step 7: the grease after deslagging enters transesterification still 14, adds the methyl alcohol of oil quality 25% and the potassium hydroxide solution of oil quality 0.5%.65 DEG C ± 5 DEG C reactions 30 minutes, deviate from excessive methanol.
Step 8: the glycerine of generation isolated by the transesterification grease completed through natural subsidence or centrifuge.
Step 9: the grease after separation of glycerin, by the second flash distillation dealcoholysis unit 15, at-0.08Mpa, under 110 DEG C of conditions, removes remaining Trace Methanol.
Step 10: the grease after dealcoholysis enters vacuum distillation tower 16 refined biometric diesel oil of purifying out and collects from product oil floss hole 18, and the residue of vacuum distillation is plant asphalt, discharges from pitch floss hole 17.Product oil yield is about 84.5% of raw oil material quality, and quality can reach the standard of diesel fuel mediation biodiesel (BD100) GB/T20828-2014.
Embodiment 3
A method for biodiesel is prepared in continuous gas phase catalysis esterification, comprises the steps:
Step 1: get hogwash fat raw material 1000Kg (acid number 35mgKOH/g, water is assorted is less than 2%), added by charging aperture 1 and come unstuck in still 3; Get gas-phase reaction complete after the acid sludge top mobility good part 100Kg acid sludge import 2 of discharge add and come unstuck in still 3.Start agitating heating and be warmed up to 60 DEG C-90 DEG C, insulation reaction 1 hour.Stop stirring, quiescent settling 2-4 hours, discharge colloid and the sour water of bottom.In the grease of top, add the aluminium chloride of grease weight 1%, start reactor and stir, stir and within 0.5 hour, make catalyst and grease mix.
Step 2: the grease through coming unstuck is added first reactor 7 by the speed of 150Kg/h by feedstock oil import 4 by feedstock pump, fresh methanol adds the 3rd reactor 9 by the speed of 40Kg/h after methyl alcohol vaporizing device 11 gasifies.Control reactor temperature 105 DEG C-110 DEG C, pressure 0.3Mpa.
Step 3: along with constantly adding of glyceride stock, the material level of the first reactor 7 constantly raises, and opens the blow-off valve of the first reactor 7 to the second reactor 8 punishment in advance when material level reaches the half of reactor time.The material level of same control second reactor 8, to the 3rd reactor 9 punishment in advance.When the 3rd reactor 9 material level reaches a half, detect the acid number of the 3rd reactor 9.When acid number is lower than 2mgKOH/g, open the blow-off valve of the 3rd reactor 9, start discharging.If acid number is higher than 2mgKOH/g, then improve the liquid level of the first to the three reactor, liquid level is the highest can reach 2/3 of all reactors.By controlling the switch size of the blow-off valve of each reactor, adjust the liquid level of the first reactor 7, second reactor the 8, three reactor 9, liquid level is generally between 1/2 to 2/3 of reactor height.The blow-off valve can driving each reactor large when the acid number of the 3rd reactor 9 is lower time reduces the material level of each reactor, and when the acid number of the 3rd reactor 9 is higher time, the blow-off valve that turn down each reactor improves the material level of each reactor.Inlet amount, quantity of methyl alcohol are through to calculate generally does not need adjustment, and only need to adjust the material stock in reactor, namely the reaction time just can control the acid number of product.
Step 4: gas-phase methanol enters after the 3rd reactor 9 react with grease, unreacted excessive methanol and the water reacting generation enter the bottom of the second reactor 8 from the gaseous phase outlet of the 3rd reactor 9 with the form of gas phase.Gas-phase methanol and grease react further, the water that excessive methyl alcohol and reaction produce is entered the bottom of the first reactor 7 by the gaseous phase outlet of the second reactor 8 with the form of gas phase, methyl alcohol and grease vigorous reaction in the first reactor 7, have methanol outlet 6 to discharge by the gas phase of the first reactor 7 together with the water that the water that excessive methyl alcohol and reaction generate, raw material are brought into.By controlling the valve size of gas-phase methanol outlet 6, control the pressure 0.3 ± 0.01Mpa in reactor.Gas-phase methanol directly enters methanol distillation column, adjustment recovery tower, ensures that rectifying methanol content reaches more than 99%.The methyl alcohol reclaimed continues to use.
Step 5: the material that the 3rd reactor 9 is discharged enters the first flash distillation dealcoholysis unit 12 by discharge pipe, deviates from excessive methanol.
Step 6: the grease after dealcoholysis enters settling tank 13, acid sludge is discharged in sedimentation separation.
Step 7: the grease after deslagging enters transesterification still 14, adds the methyl alcohol of oil quality 30% and the potassium hydroxide solution of oil quality 0.6%.65 DEG C ± 5 DEG C reactions 30 minutes, deviate from excessive methanol.
Step 8: the glycerine of generation isolated by the transesterification grease completed through natural subsidence or centrifuge.
Step 9: the grease after separation of glycerin, by the second flash distillation dealcoholysis unit 15, at-0.09Mpa, under 105 DEG C of conditions, removes remaining Trace Methanol.
Step 10: the grease after dealcoholysis enters vacuum distillation tower 16 refined biometric diesel oil of purifying out and collects from product oil floss hole 18, and the residue of vacuum distillation is plant asphalt, discharges from pitch floss hole 17.Product oil yield is about 84% of raw oil material quality, and quality can reach the standard of diesel fuel mediation biodiesel (BD100) GB/T20828-2014.
Embodiment 4
A method for biodiesel is prepared in continuous gas phase catalysis esterification, comprises the steps:
Step 1: get soybean acidified oil raw material 1000Kg (acid number 90mgKOH/g, water is assorted is less than 3%), added by charging aperture 1 and come unstuck in still 3; Get gas-phase reaction complete after the acid sludge top mobility good part 150Kg acid sludge import 2 of discharge add and come unstuck in still 3.Start agitating heating and be warmed up to 60 DEG C-90 DEG C, insulation reaction 1 hour.Stop stirring, quiescent settling 3-6 hours, discharge colloid and the sour water of bottom.Top grease enters subsequent processing.
Step 2: add the one the first reactors 7 by the speed of 150Kg/h by feedstock oil import 4 by feedstock pump through the grease that comes unstuck, fresh methanol adds the 3rd reactor 9 by the speed of 45Kg/h after methyl alcohol vaporizing device 11 gasifies, and SPA catalyst is added in the first reactor 4 by catalyst inlet 5 by the speed of 1.5Kg/h.Control reactor temperature 105 DEG C-110 DEG C, pressure 0.3Mpa.
Step 3: along with constantly adding of glyceride stock, the material level of the first reactor 7 constantly raises, and opens the blow-off valve of the first reactor 7 to the second reactor 8 punishment in advance when material level reaches the half of reactor time.The material level of same control second reactor 8, to the 3rd reactor 9 punishment in advance.When the 3rd reactor 9 material level reaches a half, detect the acid number of the 3rd reactor 9.When acid number is lower than 2mgKOH/g, open the blow-off valve of the 3rd reactor 9, start discharging.If acid number is higher than 2mgKOH/g, then improve the liquid level of the first to the three reactor, liquid level is the highest can reach 2/3 of all reactors.By controlling the switch size of the blow-off valve of each reactor, adjust the liquid level of the first reactor 7, second reactor the 8, three reactor 9, liquid level is generally between 1/2 to 2/3 of reactor height.The blow-off valve can driving each reactor large when the acid number of the 3rd reactor 9 is lower time reduces the material level of each reactor, and when the acid number of the 3rd reactor 9 is higher time, the blow-off valve that turn down each reactor improves the material level of each reactor.Inlet amount, quantity of methyl alcohol are through to calculate generally does not need adjustment, and only need to adjust the material stock in reactor, namely the reaction time just can control the acid number of product.
Step 4: gas-phase methanol enters after the 3rd reactor 9 react with grease, unreacted excessive methanol and the water reacting generation enter the bottom of the second reactor 8 from the gaseous phase outlet of the 3rd reactor 9 with the form of gas phase.Gas-phase methanol and grease react further, the water that excessive methyl alcohol and reaction produce is entered the bottom of the first reactor 7 by the gaseous phase outlet of the second reactor 8 with the form of gas phase, methyl alcohol and grease vigorous reaction in the first reactor 7, have methanol outlet 6 to discharge by the gas phase of the first reactor 7 together with the water that the water that excessive methyl alcohol and reaction generate, raw material are brought into.By controlling the valve size of gas-phase methanol outlet 6, control the pressure 0.3 ± 0.01Mpa in reactor.Gas-phase methanol directly enters methanol distillation column, adjustment recovery tower, ensures that rectifying methanol content reaches more than 99%.The methyl alcohol reclaimed continues to use.
Step 5: the material that the 3rd reactor 9 is discharged enters the first flash distillation dealcoholysis unit 12 by discharge pipe, deviates from excessive methanol.
Step 6: the grease after dealcoholysis enters settling tank 13, acid sludge is discharged in sedimentation separation.
Step 7: the grease after deslagging enters transesterification still 14, adds the methyl alcohol of oil quality 23% and the potassium hydroxide solution of oil quality 0.5%.65 DEG C ± 5 DEG C reactions 30 minutes, deviate from excessive methanol.
Step 8: the glycerine of generation isolated by the transesterification grease completed through natural subsidence or centrifuge.
Step 9: the grease after separation of glycerin, by the second flash distillation dealcoholysis unit 15, at-0.08Mpa, under 110 DEG C of conditions, removes remaining Trace Methanol.
Step 10: the grease after dealcoholysis enters vacuum distillation tower 16 refined biometric diesel oil of purifying out and collects from product oil floss hole 18, and the residue of vacuum distillation is plant asphalt, discharges from pitch floss hole 17.Product oil yield is about 85.5% of raw oil material quality, and quality can reach the standard of diesel fuel mediation biodiesel (BD100) GB/T20828-2014.
Embodiment 5
A method for biodiesel is prepared in continuous gas phase catalysis esterification, comprises the steps:
Step 1: get palmitic acid carburetion raw material 1000Kg (acid number 120mgKOH/g, water is assorted is less than 3%), added by charging aperture 1 and come unstuck in still 3; Get gas-phase reaction complete after the acid sludge top mobility good part 250Kg acid sludge import 2 of discharge add and come unstuck in still 3.Start agitating heating and be warmed up to 60 DEG C-90 DEG C, insulation reaction 1 hour.Stop stirring, quiescent settling 3-6 hours, discharge colloid and the sour water of bottom.Top grease enters subsequent processing.
Step 2: the grease through coming unstuck is added first reactor 7 by the speed of 150Kg/h by feedstock oil import 4 by feedstock pump, fresh methanol adds the 3rd reactor 9 by the speed of 45Kg/h after methyl alcohol vaporizing device 11 gasifies, and concentrated sulfuric acid catalyst is added in the first reactor 4 by catalyst inlet 5 by the speed of 0.5Kg/h.Control reactor temperature 120 DEG C-125 DEG C, pressure 0.5Mpa.
Step 3: along with constantly adding of glyceride stock, the material level of the first reactor 7 constantly raises, and opens the blow-off valve of the first reactor 7 to the second reactor 8 punishment in advance when material level reaches the half of reactor time.The material level of same control second reactor 8, to the 3rd reactor 9 punishment in advance.When the 3rd reactor 9 material level reaches a half, detect the acid number of the 3rd reactor 9.When acid number is lower than 2mgKOH/g, open the blow-off valve of the 3rd reactor 9, start discharging.If acid number is higher than 2mgKOH/g, then improve the liquid level of the first to the three reactor, liquid level is the highest can reach 2/3 of all reactors.By controlling the switch size of the blow-off valve of each reactor, adjust the liquid level of the first reactor 7, second reactor the 8, three reactor 9, liquid level is generally between 1/2 to 2/3 of reactor height.The blow-off valve can driving each reactor large when the acid number of the 3rd reactor 9 is lower time reduces the material level of each reactor, and when the acid number of the 3rd reactor 9 is higher time, the blow-off valve that turn down each reactor improves the material level of each reactor.Inlet amount, quantity of methyl alcohol are through to calculate generally does not need adjustment, and only need to adjust the material stock in reactor, namely the reaction time just can control the acid number of product.
Step 4: gas-phase methanol enters after the 3rd reactor 9 react with grease, unreacted excessive methanol and the water reacting generation enter the bottom of the second reactor 8 from the gaseous phase outlet of the 3rd reactor 9 with the form of gas phase.Gas-phase methanol and grease react further, the water that excessive methyl alcohol and reaction produce is entered the bottom of the first reactor 7 by the gaseous phase outlet of the second reactor 8 with the form of gas phase, methyl alcohol and grease vigorous reaction in the first reactor 7, have methanol outlet 6 to discharge by the gas phase of the first reactor 7 together with the water that the water that excessive methyl alcohol and reaction generate, raw material are brought into.By controlling the valve size of gas-phase methanol outlet 6, control the pressure 0.5 ± 0.01Mpa in reactor.Gas-phase methanol directly enters methanol distillation column, adjustment recovery tower, ensures that rectifying methanol content reaches more than 99%.The methyl alcohol reclaimed continues to use.
Step 5: the material that the 3rd reactor 9 is discharged enters the first flash distillation dealcoholysis unit 12 by discharge pipe, deviates from excessive methanol.
Step 6: the grease after dealcoholysis enters settling tank 13, acid sludge is discharged in sedimentation separation.
Step 7: the grease after deslagging enters transesterification still 14, adds the methyl alcohol of oil quality 18% and the potassium hydroxide solution of oil quality 0.4%.65 DEG C ± 5 DEG C reactions 30 minutes, deviate from excessive methanol.
Step 8: the glycerine of generation isolated by the transesterification grease completed through natural subsidence or centrifuge.
Step 9: the grease after separation of glycerin, by the second flash distillation dealcoholysis unit 15, at-0.08Mpa, under 110 DEG C of conditions, removes remaining Trace Methanol.
Step 10: the grease after dealcoholysis enters vacuum distillation tower 16 refined biometric diesel oil of purifying out and collects from product oil floss hole 18, and the residue of vacuum distillation is plant asphalt, discharges from pitch floss hole 17.Product oil yield is about 86.5% of raw oil material quality, and quality can reach the standard of diesel fuel mediation biodiesel (BD100) GB/T20828-2014.
Claims (6)
1. a continuous gas-phase reaction prepares the device of biodiesel, it is characterized in that comprising at least three reactors, the still that comes unstuck, the first reactor, the second reactor, the 3rd reactor, methyl alcohol vaporizing device, the first flash distillation dealcoholysis unit, settling tank, transesterification still, the second flash distillation dealcoholysis unit are connected successively with vacuum distillation tower;
Described still upper end of coming unstuck is respectively equipped with charging aperture and acid sludge import, and lower end discharging opening is connected with feedstock oil charging aperture;
The upper end of described first reactor is respectively equipped with feedstock oil charging aperture, catalyst inlet, gaseous phase outlet, and bottom is provided with opening, and gaseous phase outlet is connected with methanol distillation column; Feedstock oil charging aperture is connected with feed pipe;
The upper end of described second reactor is provided with charging aperture and gaseous phase outlet, and bottom is provided with opening; Open communication bottom charging aperture and gaseous phase outlet and the first reactor;
The upper end of described 3rd reactor is provided with charging aperture and gaseous phase outlet, and bottom is provided with opening; Gas-phase methanol import is connected with methyl alcohol vaporizing device, adds fresh gas-phase methanol; Bottom opening is connected with discharge pipe; Gaseous phase outlet is connected with the second reactor bottom opening;
Described discharge pipe is connected with the first flash distillation dealcoholysis unit, first flash distillation dealcoholysis unit is connected with settling tank, settling tank is connected with transesterification still, transesterification still is connected with settling tank or centrifuge, settling tank or centrifuge and the second flash distillation dealcoholysis unit, second flash distillation dealcoholysis unit is connected with vacuum distillation tower, and vacuum distillation tower is respectively equipped with pitch floss hole and product oil floss hole.
2. continuous gas-phase reaction according to claim 1 prepares the device of biodiesel, it is characterized in that, the pipeline that described discharge pipe is connected with the first flash distillation dealcoholysis unit is provided with valve.
3. continuous gas-phase reaction according to claim 1 prepares the device of biodiesel, it is characterized in that, the pipeline that described first reactor and the second reactor bottom opening are connected with charging aperture and the gaseous phase outlet of the second reactor and the 3rd reactor upper end is respectively provided with valve.
4. continuous gas-phase reaction according to claim 1 prepares the device of biodiesel, it is characterized in that, the quantity of described reactor is 4-6; 4th reactor is identical with the connected mode of the 3rd reactor with the second reactor to the connected mode of the 6th reactor.
5. continuous gas-phase reaction according to claim 1 prepares the device of biodiesel, it is characterized in that, described first reactor, the second reactor, the 3rd reactor adopt stainless steel still or glass-lined kettle; Described transesterification still adopts stainless steel still or glass-lined kettle.
6. continuous gas-phase reaction according to claim 1 prepares the device of biodiesel, it is characterized in that, described methyl alcohol vaporizing device adopts tubular heat exchanger or spiral heat exchanger; Described vacuum distillation tower adopts packed tower or plate column.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830543A (en) * | 2015-04-28 | 2015-08-12 | 广东河山环保有限公司 | Device and method for preparing biodiesel through continuous gas-phase catalytic esterification |
| CN110029024A (en) * | 2019-04-23 | 2019-07-19 | 龙岩卓越新能源股份有限公司 | A kind of waste oil continuous esterification process units |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830543A (en) * | 2015-04-28 | 2015-08-12 | 广东河山环保有限公司 | Device and method for preparing biodiesel through continuous gas-phase catalytic esterification |
| CN110029024A (en) * | 2019-04-23 | 2019-07-19 | 龙岩卓越新能源股份有限公司 | A kind of waste oil continuous esterification process units |
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