CN101586041A - Device and method for continuously preparing biodiesel - Google Patents
Device and method for continuously preparing biodiesel Download PDFInfo
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- CN101586041A CN101586041A CNA2009100537275A CN200910053727A CN101586041A CN 101586041 A CN101586041 A CN 101586041A CN A2009100537275 A CNA2009100537275 A CN A2009100537275A CN 200910053727 A CN200910053727 A CN 200910053727A CN 101586041 A CN101586041 A CN 101586041A
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Abstract
The invention relates to a device and method for continuously preparing biodiesel with foamed metal filling reactor. The invention includes firstly injecting lipid and low carbon alcoholic solution with dissolved basic catalyst into a passive mixer 4 according to a setting ratio continuously and respectively, forming a chaotic stream intensified mixture inside, emulsifying and dispersing; and then continuously injecting the emulsified mixture into a reactor 5 for filling foamed metal 6, furthermore intensifying and mixing, and guaranteeing the reaction temperature through a heating mechanism 7 outside the reactor; at last, obtaining biodiesel through separation and purification from the reaction product. The apparatus and method for preparing biodiesel according to the invention have the advantages of simple technique, low energy consumption, high efficiency, continuous operation, mass production convenience or the like.
Description
Technical field
The present invention relates to a kind of device and method of continuous preparation biofuel, especially relate to a kind of apparatus and method that adopt foam metal filled reactor biodiesel synthesis, belong to technical field of biodiesel preparation.
Background technology
Biofuel is to be raw material with animal-plant oil etc., compare with conventional diesel oil, it has the favor that good environmental protection characteristic, good low-temperature engine starting performance, lubricity, safety performance and regenerative nature etc. obtain people, cleaning liq biofuel as alternative petrifaction diesel has great potential and vast market prospect.
Ester-interchange method is the main method of present biofuel suitability for industrialized production.It utilizes alcohols materials such as methyl alcohol, ethanol, under katalysis, the glycerine in the tri-glyceride in the vegetables oil is replaced to get off, and forms the fatty acid methyl ester of long-chain.Reaction in intermittence or continuous stirred tank reactor (CSTR), under 20-80 ℃, is passed through a few hours and is finished usually.Because the immiscible system blending dispersion of oleyl alcohol difficulty in conventional stirred reactor, so long reaction time, transformation efficiency is low, energy consumption is big.In addition, adopt the batch reactor reaction longer non-cutting time, production efficiency is low.
Under super critical condition, obtained in the recent period paying close attention to widely by the transesterification reaction biodiesel synthesis.CN15944504 has disclosed and has a kind ofly obtained the high conversion method of bio-diesel oil with supercritical process in 2-15min.Its reaction yield is higher, need not catalyzer, and product separates simple.But its molar ratio of methanol to oil is 40 to 100, a large amount of excessive risings that cause pure cost recovery of alcohol.In addition, because overcritical process relates to high temperature (320 ℃), high pressure (25MPa), the unit required energy consumption of biofuel output is higher, and conversion unit and operational safety have been proposed very high request.
At above problem, many high-efficiency biological diesel oil reactors have appearred in the recent period.CN1919973A proposes to utilize the loop turbulent flow reactor to form the device that a cover continous way prepares biofuel, temperature of reaction is 150-230 ℃, and pressure is 1-7MPa, and the residence time is 5-30min, the biofuel transformation efficiency can reach more than 99%, but its temperature and pressure is all higher.CN100999679A proposes to add solubility promoter and promotes pure oily two-phase to mix, mixed solution enters continuously and carries out transesterification reaction in the pipeline reactor, temperature of reaction is 60-65 ℃, alcohol oil rate is 10-27, reaction times is 30-120min, and biodiesel production rate is 97.0-99.9%, but its alcohol oil rate height, long reaction time is introduced solubility promoter and will be made troubles and increase the cost of raw material to subsequent disposal.CN1810930A is on traditional biological diesel production technical foundation, add emulsifying mixer (0.2-1.0MPa), make immiscible methyl alcohol and grease mix the drop that is dispersed into the 1-10 micron, the surface in contact that increases two phase reaction greatly is long-pending, enters the blistering reaction tower through the interchanger heating, step-down, methanol gasifying forms a large amount of tiny bubbles, strengthens contact interface, thereby accelerates transesterification reaction speed, but need by force (forcing) pump before entering emulsifying mixer, working condition is complicated.Stavarache people such as (Ultrasonic Sonochemistry, 2005,12,367) uses intensified by ultrasonic wave reactor biodiesel synthesis, is issued to 20 minutes residence time to surpass 90% productive rate.Azcan people such as (Fuel, 2008,87,1781) uses microwave reactor, is under the 5min in the residence time, and transformation efficiency reaches 93%, but hyperacoustic introducing has increased the complicacy of reaction unit, has strengthened production cost.
Little reaction technology is one of technology of the tool innovation of of current fine chemistry industry, pharmacy, health care industry, has extremely good mixing fast, efficient heat transfer, raising productive rate, the characteristics of the narrow distribution of reactant residence time.CN101148409A utilizes micro passage reaction, and under the temperature of reaction of normal pressure and 90-170 ℃, the control reaction mass stops 5-60min in micro passage reaction, can prepare biofuel, and productive rate is higher, but the output of microreactor is too little.CN1861751C disclosed a kind of in micro passage reaction the method with base catalysis method biodiesel synthesis, this method can be again under 60 ℃, makes the biofuel transformation efficiency reach 95% in the 5min.But this method need be pre-mixed, and reaction efficiency is low.CN101333451A has disclosed a kind of little reactive system of biofuel that little interchanger, micro mixer and microreactor are integrated in one, 70 ℃, 1min, soybean oil methyl esters yield is 95.5%, but it needs preheating, and system is comparatively complicated, and yield of biodiesel is less than 10mLmin
-1
At present, the problem of microreactor technology maximum is that the output of biofuel is very low, and separate unit microreactor output is less than 0.6kgh
-1Though above invention all declares to improve by the increase of simple quantity the output of biofuel.Even but, minimumly needing 2200 microreactors in parallel for the industrial scale (10,000 tons/year) of small-scale biofuel, this is very difficult.
Therefore, need exploitation a kind of less energy-consumption, high-level efficiency, operate continuously, be convenient to the method for synthesizing biologic diesel oil of volume production.
Summary of the invention
At the defective of prior art, the invention provides a kind of preparation facilities and method of biofuel, have that technology is simple, energy consumption is low, efficient is high, operate continuously, be convenient to the characteristics of volume production.
The present invention is achieved by the following technical solutions:
A kind of device of continuous preparation biofuel, it is characterized in that, described device comprises: an oil tank 1 links to each other with volume pump 3, a low-carbon alcohol container 2 links to each other with volume pump 9, after converging, the outlet line of volume pump 3 and volume pump 9 is connected in the import of reactor 5, tight 6, one electrically heated of filled and process metal and control device 7 in the reactor 5 by a passive type mixing tank 4, be installed on the outside surface of foam metal filled reactor, a collector 8 is connected the outlet of reactor 5.
The bore of described tubular reactor is 10～100mm, and concrete size is determined by the foamed metal external diameter.Length is 0.2～1.8m, preferred 0.5～1.2m.
The shape of described foamed metal 6 is carved mutually with reactor 5 and is closed, the external diameter of foamed metal is 10～100mm, preferred 15～25mm, length is 10～80mm, preferred 20～40mm, and material is preferably stainless steel, porosity is 0.80～0.98%, preferred 0.93～0.96%, PPI (hole count of per inch line length) is 5-150, preferred 20-50.
Described passive type mixing tank 4 is small-sized passive type mixing tanks, adopts Y type inlet, Zigzag type runner, and the runner interface shape is a square or circular, equivalent diameter is 1.0～5mm, preferred 1.2～3mm, length is 0.3～0.8m, preferred 0.5～0.7m.
The present invention also provides a kind of continuous preparation method of bio-diesel oil based on said apparatus, comprises the steps:
1) grease is injected in the passive type mixing tank 4 through volume pump 9 through volume pump 3, the low-carbon alcohol solution that is dissolved with basic catalyst mixes; Wherein, be dissolved with in the low-carbon alcohol solution of basic catalyst, low-carbon alcohol and greasy mol ratio are (3～15): 1, and preferred low-carbon alcohol and grease mol ratio are (3～8): 1, the consumption of basic catalyst is 0.5～2% of a grease weight, preferred 0.8～1.2%;
2) mixed solution in the step 1) mixing tank 4 is injected in the reactor 5 that is filled with foamed metal 6, reaction times 0.5-5min, preferred 1-3min regulates and keeps 20～130 ℃ of temperature of reaction, preferred 50～63 ℃ by reactor indirect heating device 7; Reactant enters collector 8 through reactor 5 outlets;
3) reactant in the collector 8 is collected, separated, obtain biofuel after the purification; Described basic catalyst is to be selected from a kind of in sodium hydroxide, potassium hydroxide and the sodium methylate.
Described grease can be a vegetables oil, as low erucic acid mustard caul-fat, rapeseed oil, soybean oil, peanut oil, Oleum Gossypii semen, Semen Maydis oil, plam oil, Oleum Cocois, Viscotrol C and sunflower wet goods, also can be animal grease, for example lard, sheep oil and butter etc. also can be above-mentioned greasy mixtures.
Described low-carbon alcohol particular methanol and ethanol.
The present invention also discloses a kind of improvement project of device of above-mentioned continuous preparation biofuel:
In the device of described a kind of continuous preparation biofuel, the outlet line of volume pump 3 and volume pump 9 converges the back and is connected respectively with the passive type mixing tank 4 of parallel connection more than two, the outlet of each passive type mixing tank 4 links to each other with the import of the reactor 5 of a tight filled and process metal 6, and the outlet line of reactor 5 compiles the back connection and is connected with collector 8.
Beneficial effect
The present invention adopts small-sized passive type mixing tank, by Zigzag type runner the immiscible two kinds of liquid of alcohol oil is carried out premix, forms chaotic flow by the Zigzag structure, promotes to mix.The equivalent diameter of runner is preferably 1.2～3mm, and length is preferably 0.5～0.7m, avoids bigger pressure to fall on the basis that guarantees mixed effect.Because foamed metal has loose porous characteristics, porosity preferred 0.93～0.96%, pure oily mixed solution behind the premix in foamed metal will be further by forming the chaotic flow enhancing mixed, having formed median size is the emulsion droplet of 1～2 μ m, increased the contact area of oleyl alcohol two phase reaction greatly, strengthen mass transfer, improved reaction efficiency.Because foamed metal has heat conductivility preferably, foamed metal closely is filled in and will makes reacting appliance that the ideal heat-conducting effect is arranged in the reactor, has reduced energy consumption.With intermittently or continuous stirred tank reactor (CSTR) need a few hours reach high biofuel transformation efficiency to compare, the time required for the present invention is 1-3min, has significantly improved reaction efficiency.Compare with microreactor, the present invention adopts small-sized passive type mixing tank and foam metal filled mixed intensified method of two step of reactor, foam metal filled reactor equivalent diameter is much larger than microreactor, and reaction times and microreactor are suitable, and the output of biofuel can reach 3kgh
-1, the output of separate unit reactor has improved 50 times with respect to microreactor, has guaranteed higher biodiesel production rate simultaneously, has avoided microreactor to need a large amount of problems in parallel when the biofuel volume production, greatly reduces cost.
The apparatus and method of continuous preparation biofuel of the present invention, utilize chaotic flow forced fluid liquid immiscible liquid blended principle, adopt small-sized passive type mixing tank, especially first adopt foam metal filled reactor as the high-efficiency biological diesel oil reactor, have that technology is simple, energy consumption is low, efficient is high, operate continuously, be convenient to the characteristics of volume production with respect to prior art.
Description of drawings
Fig. 1 is the device and the process flow diagram of continuous preparation biofuel of the present invention.
In Fig. 1,1: oil tank, 2: low-carbon alcohol container, 3,9: volume pump, 4: passive type mixing tank, 5: reactor, 6: the foamed metal of filling, 7: electrically heated and temperature-control device, 8: collector
Fig. 2 is the parallel system synoptic diagram of continuous preparation biofuel device of the present invention's embodiment 3.
In Fig. 2,1: oil tank, 2: low-carbon alcohol container, 3,9: volume pump, 4: passive type mixing tank, 5: reactor, 6: the foamed metal of filling, 7: electrically heated and temperature-control device, 8: collector.
Embodiment
Respectively the low-carbon alcohol that is dissolved with basic catalyst in grease in the grease jar 1 and the low-carbon alcohol container 2 is injected small-sized passive type mixing tank 4 continuously with volume pump 3 and volume pump 9, behind the emulsification premix, enter foam metal filled reactor 5, keep and the stopping reaction temperature by electrically heated and the temperature-control device 7 that is installed on foam metal filled reactor 5 outside surfaces, reaction mass stops 1-3min in the foamed metal reactor.Product is collected in outlet, obtains biofuel after separating, purifying.
13g NaOH is dissolved in formation homogeneous phase mixed solution in the 287.5g methyl alcohol.This mixed solution and soya-bean oil are respectively with 20mlmin
-1And 80mlmin
-1Flow be injected into small-sized passive type mixing tank continuously through volume pump, this mixing tank has Y type inlet, Zigzag type runner, equivalent diameter is 1.2mm, length is 0.5m.This moment, the mol ratio of methyl alcohol and soya-bean oil was 6: 1, and the concentration of NaOH is 1% (with the Mass Calculation of soya-bean oil).It is 20mm that mixed solution behind premix enters internal diameter, and length is in the foam metal filled reactor of 0.5m.Foamed metal is that cylindrical, material is that stainless steel, external diameter are 20mm, and length is 20mm, and PPI (hole count of per inch line length) is 20, and porosity is 95%.Electrically heated by being installed on foamed metal reactor outside surface and control device keep and the stopping reaction temperature is 60 ℃, and the residence time of material in reactor is 1.57min.Outlet liquid obtains reaction product through standing separation, supernatant liquid through neutralization, washing, drying.The biofuel transformation efficiency that utilizes gas chromatographic analysis to obtain is 95.0%.
13g NaOH is dissolved in formation homogeneous phase mixed solution in the 287.5g methyl alcohol.This mixed solution and soya-bean oil are injected into small-sized passive type mixing tank with the flow of 20ml/min and 80ml/min through volume pump respectively continuously, and this mixing tank has Y type inlet, Zigzag type runner, and equivalent diameter is 1.2mm, length is 0.5m.This moment, the mol ratio of methyl alcohol and soya-bean oil was 6: 1, and the concentration of NaOH is 1% (with the Mass Calculation of soya-bean oil).It is 20mm that mixed solution behind premix enters internal diameter, and length is in the foam metal filled reactor of 0.5m.Foamed metal is that cylindrical, material is that stainless steel, external diameter are 20mm, and length is 20mm, and PPI (hole count of per inch line length) is 30, and porosity is 95.3%.Electrically heated by being installed on foamed metal reactor outside surface and control device keep and the stopping reaction temperature is 60 ℃, and the residence time of material in reactor is 1.57min.Outlet liquid obtains reaction product through standing separation, supernatant liquid through neutralization, washing, drying.The biofuel transformation efficiency that utilizes gas chromatographic analysis to obtain is 95.8%.
850gNaOH is dissolved in formation homogeneous phase mixed solution in the 14375g methyl alcohol.As shown in Figure 2.Through pump delivery, this mixed solution and soya-bean oil are respectively with 200mlmin
-1And 800mlmin
-1Flow enter 10 small-sized passive type mixing tanks respectively and carry out premix by-Y-junction, this mixing tank has Y type inlet, Zigzag type runner, equivalent diameter is 3mm, length is 0.5m.This moment, the mol ratio of methyl alcohol and soya-bean oil was 6: 1, and the concentration of NaOH is 1% (with the Mass Calculation of soya-bean oil).Then, it is 50mm that the mixed solution behind premix enters 10 internal diameters respectively, and length is the foam metal filled reactor of 1m.Foamed metal is that cylindrical, material is that stainless steel, external diameter are 20mm, and length is 20mm, and PPI (hole count of per inch line length) is 20, and porosity is 95.1%.Electrically heated by being installed on foam metal filled reactor outside surface and control device keep and the stopping reaction temperature is 60 ℃, and the residence time of material in reactor is 1.96min.The outlet liquid of 10 foam metal filled reactors converges collection, obtains reaction product through standing separation, supernatant liquid through neutralization, washing, drying.The biofuel transformation efficiency that utilizes gas chromatographic analysis to obtain is 91.7%.
By 1 year 300 days, continuous production calculated in 24 hours in one day, and the production of biodiesel device that more than has 10 foamed metal reactors can be produced 0.2 ten thousand tons of biofuel per year.For the industrial scale (10,000 tons/year) of small-scale biofuel, only need production of biodiesel device 5 covers as above, promptly need 50 foamed metal reactors.If reach identical industrial scale, microreactor is then minimum to need 2200 in parallel, is difficult on the technology realize that cost also can be very high.Method that it is a kind of less energy-consumption, high-level efficiency, operate continuously that so foam metal filled reactor of the present invention prepares biofuel continuously, be convenient to volume production.
Claims (10)
1, a kind of device of continuous preparation biofuel, it is characterized in that, described device comprises: an oil tank 1 links to each other with volume pump 3, a low-carbon alcohol container 2 links to each other with volume pump 9, after converging, the outlet line of volume pump 3 and volume pump 9 is connected in the import of reactor 5, tight 6, one electrically heated of filled and process metal and control device 7 in the reactor 5 by a passive type mixing tank 4, be installed on the outside surface of foam metal filled reactor, a collector 8 is connected the outlet of reactor 5.
2, the device of continuous preparation biofuel as claimed in claim 1 is characterized in that, described reactor 5 is a tubular reactor, and the bore of reactor 5 is 10～100mm, and length is 0.2～1.8m.
3, the device of continuous preparation biofuel as claimed in claim 2 is characterized in that, the length of described reactor 5 is 0.5～1.2m.
4, the device of continuous preparation biofuel as claimed in claim 1 is characterized in that, the external diameter of described foamed metal 6 is 10～100mm, and length is 10～80mm, and porosity is 0.80～0.98%, and the hole count of per inch line length is 5-150.
5, the device of continuous preparation biofuel as claimed in claim 4 is characterized in that, the external diameter of described foamed metal is 15～25mm, length is 20～40mm, porosity is 0.93～0.96%, and the hole count of per inch line length is 20-50, and material is a stainless steel.
6, the device of continuous preparation biofuel as claimed in claim 1 is characterized in that, the equivalent diameter of described passive type mixing tank 4 is 1.0～5mm, and length is 0.3～0.8m.
7, the device of continuous preparation biofuel as claimed in claim 6 is characterized in that, the equivalent diameter of described passive type mixing tank 4 is 1.2～3mm, and length is 0.5～0.7m.
8, a kind of employing device as claimed in claim 1 prepares method of bio-diesel oil continuously, it is characterized in that described method comprises the steps:
1) grease is injected in the passive type mixing tank 4 through volume pump 9 through volume pump 3, the low-carbon alcohol solution that is dissolved with basic catalyst mixes; Wherein, be dissolved with in the low-carbon alcohol solution of basic catalyst, low-carbon alcohol and greasy mol ratio are (3～15): 1, and the consumption of basic catalyst is 0.5～2% of a grease weight;
2) mixed solution in the step 1) mixing tank 4 is injected in the reactor 5 that is filled with foamed metal 6, reaction times 0.5-5min regulates and keeps 20～130 ℃ of temperature of reaction by reactor indirect heating device 7; Reactant enters collector 8 through reactor 5 outlets;
3) reactant in the collector 8 is collected, separated, obtain biofuel after the purification;
Wherein, described basic catalyst is to be selected from a kind of in sodium hydroxide, potassium hydroxide and the sodium methylate, and described grease is vegetables oil or animal oil.
9, continuous preparation method of bio-diesel oil as claimed in claim 8 is characterized in that, described low-carbon alcohol particular methanol and ethanol, and the described reaction times is 1-3min, temperature of reaction is 50～63 ℃.
10, the device of continuous preparation biofuel as claimed in claim 1, it is characterized in that, the outlet line of described volume pump 3 and volume pump 9 converges the back and is connected respectively with the passive type mixing tank 4 of parallel connection more than two, the outlet of each passive type mixing tank 4 links to each other with the import of the reactor 5 of a tight filled and process metal 6, and the outlet line of reactor 5 compiles the back connection and is connected with collector 8.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106132530A (en) * | 2014-03-18 | 2016-11-16 | 瓦克化学股份公司 | Prepare reactor and the method for granular polycrystalline silicon |
| CN108395938A (en) * | 2017-02-07 | 2018-08-14 | 中国石油化工股份有限公司 | A kind of preparation method and system of biodiesel |
| CN108395936A (en) * | 2017-02-07 | 2018-08-14 | 中国石油化工股份有限公司 | A kind of method and system preparing biodiesel |
| CN115820314A (en) * | 2022-11-16 | 2023-03-21 | 重庆大学 | Method and device for improving coal quality by coupling effect of memristive lorentz chaotic electric field and pyrolusite |
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- 2009-06-25 CN CNA2009100537275A patent/CN101586041A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106132530A (en) * | 2014-03-18 | 2016-11-16 | 瓦克化学股份公司 | Prepare reactor and the method for granular polycrystalline silicon |
| CN106132530B (en) * | 2014-03-18 | 2019-12-20 | 瓦克化学股份公司 | Reactor and method for preparing granular polycrystalline silicon |
| CN108395938A (en) * | 2017-02-07 | 2018-08-14 | 中国石油化工股份有限公司 | A kind of preparation method and system of biodiesel |
| CN108395936A (en) * | 2017-02-07 | 2018-08-14 | 中国石油化工股份有限公司 | A kind of method and system preparing biodiesel |
| CN108395938B (en) * | 2017-02-07 | 2021-07-09 | 中国石油化工股份有限公司 | Preparation method and system of biodiesel |
| CN115820314A (en) * | 2022-11-16 | 2023-03-21 | 重庆大学 | Method and device for improving coal quality by coupling effect of memristive lorentz chaotic electric field and pyrolusite |
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Application publication date: 20091125 |