CN103666774A - Method and device for producing biodiesel according to coal-based methanol and palm oil supercritical method - Google Patents
Method and device for producing biodiesel according to coal-based methanol and palm oil supercritical method Download PDFInfo
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Abstract
The invention discloses a method and device for producing biodiesel according to the coal-based methanol and palm oil supercritical method, and belongs to the technical field of renewable energy resources. The coal-based methanol and palm oil are sent into a preheater continuously for mixing and preheating, then sent into a tube-type reactor to ensure that transesterification reaction of coal-based methanol is carried out under a supercritical condition; reaction products enter a gas-liquid separator after being decompressed through a reducing valve, so as to generate crude biodiesel and crude methanol; the crude biodiesel is sent into a decompression rectifying tower for rectification to obtain biodiesel and resid; the crude methanol enters a methanol rectifying tower to obtain methanol of which the purity is 99 percent. The method and device have the advantages that the raw materials are easy to obtain and low in price; no catalyst is added; high-quality biodiesel can be obtained through decompression rectifying of the crude biodiesel; the problems, such as corrosion of acid-base catalyst on equipment and difficulty in separating a catalyst, of the conventional catalysis supercritical method are solved; environmental pollution is avoided; the biodiesel is good in quality; the methyl ester conversion is high.
Description
Technical field
The invention belongs to technical field of green regenerative energy sources, particularly the method and apparatus of a kind of coal-based methanol and plam oil Preparation of Biodiesel by Supercritical Method.
Background technology
Biofuel is usingd animal and plant grease etc. and is prepared, can be used for alternative ore diesel oil as the clean fuel oil of self-igniton engine as raw material.For mineral oil, biofuel is a kind of clean renewable energy source.Because petroleum resources on the earth are limited, according to the exploitation of current oil and operating speed, world petroleum resource will exhaust in 50 years.Along with the aggravation of energy dilemma, the mineral substance energy (oil, coal) worsening shortages, searching aboundresources, environmental friendliness, economically viable fuel substitute become mankind's significant problem urgently to be resolved hurrily.Therefore, the technology of preparing of biofuel is also with regard to Cheng Liao various countries scholar's study hotspot.
Biofuel is a series of longer chain fatty acid mono alkyl esters.Traditional biofuel preparation is under the condition existing at catalyzer (acid, alkali or biological enzyme, also someone adopts ionic liquid recently), by animal and plant grease and low-carbon alcohol generation transesterification reaction, realizes.
Acid catalyzed process, under the condition existing, by animal and plant greases (triglyceride) and methyl alcohol or ethanol generation transesterification reaction (temperature control is at 60-250 ℃), generates corresponding fatty acid methyl ester or ethyl ester at acid catalyst.This method exists speed of response slow, often needs several hours, and acid can corrosion reaction device.
Base catalysis method, under the condition existing, by animal and plant grease and methyl alcohol or ethanol generation transesterification reaction (temperature control is at 60-250 ℃), generates corresponding fatty acid methyl ester or ethyl ester at alkaline catalysts.Require in raw material moisture and free fatty acid content quite low, otherwise the saponification reaction that fat hydrolysis occurs and cause with alkali effect, and biofuel product must wash with water and remove alkaline catalysts.For alkali heterogeneous catalyst, also there is the problem of catalyzer stripping.
Solid inorganic salt catalysis method, under solid inorganic salt catalyst, makes animal and plant grease and low-carbon alcohol generation transesterification reaction generate biofuel., without obvious toxicity and corrodibility, but there is the problem that separating catalyst flow process is complicated, cost is high in inorganic salt low price.
Composite catalyst method, makes catalyzer with tosic acid, tin tetrachloride and the vitriol oil (1:1:1), at 58-63 ℃, reacts 3.5-4 hour, and waste grease is converted into biofuel.Biofuel yield is high, good product quality, but the same with acid catalyzed process, exist catalyzer to equipment heavy corrosion problem, be not suitable for large-scale industrial production.
Catalyzed by biological enzyme, carries out transesterification by animal and plant grease and low-carbon alcohol by lipase, prepares fatty acid methyl ester or ethyl ester.This method mild condition, alcohol consumption is little, pollution-free.But catalyzer cost is high, speed of response is also slow.And lipase is effective for the transesterificationization of long chain aliphatic alcohol, as lower in the transformation efficiency of methyl alcohol and ethanol to short chain fatty alcohol, generally only have 40-60%, i.e. the easy poisoning and deactivation of enzyme.These problems have restricted the realization of industrialization of this method.
Ionic liquid-catalyzed method, at alcohol oil rate 24:1,170 ℃ of temperature of reaction, pressure 1MPa and ionic liquid-catalyzed under, make animal-plant oil and low-carbon alcohol generation transesterification reaction generate biofuel.Ionic liquid is a kind of eco-friendly catalyzer, and equipment is not had to corrodibility, and is easy to and product separation, reusable edible, but there is the problem that catalyzer cost is high.
Catalytic intensification Supercritical methanol: patent CN101818102A, adds autoclave by methyl alcohol and soybean oil with 12:1-42:1, adds the 0.1-5.0%(wt that oil is heavy) solid catalyst (K
3pO
4, magnesium aluminum-hydrotalcite or calcining sodium silicate), at temperature 150-300 ℃, reaction 2-7Mpa, realizes transesterification reaction under the condition of time 5-60 minute, and result methyl ester conversion rate reaches 90-97%.Patent CN101362958A, makes the Supercritical methanol of catalyzer with alkali (KOH), obtain methyl ester conversion rate 90-99%.The shortcoming of catalytic intensification supercritical methanol technology is to have catalyst acid or the recovery problem of alkali to the etching problem of high-tension apparatus and catalyzer.
Supercritical methanol (CN101935593B), methyl alcohol and Oleum Gossypii semen or soybean oil or rapeseed oil or sunflower seed oil or shinyleaf yellowhorn oil are added to tubular reactor with 24:1-42:1, at temperature 240-320 ℃, reaction 15-20Mpa, under the condition of time 4-15 minute, realize transesterification reaction, result methyl ester conversion rate reaches 96%.This method does not need to add catalyzer, does not have the acid base catalysator problem difficult separated with product with catalyzer to equipment corrosion problem.But have no bibliographical information for the cheap coal-based methanol of wide material sources and palmitic Preparation of Biodiesel by Supercritical Method.
Summary of the invention
Object of the present invention utilizes wide material sources, low-cost coal-based methanol and plam oil as raw material for solving exactly, is not adding methodology and the device of inventing with methyl alcohol Preparation of Biodiesel by Supercritical Method under catalyzer condition.
Coal-based methanol main component is still methyl alcohol, but the biofuel quality that its a small amount of impurity is prepared supercritical methanol technology has a certain impact.For addressing the above problem, the coarse biodiesel that the present invention prepares coal-based methanol supercritical methanol technology carries out rectification under vacuum, has obtained the measured biofuel of matter.The mechanism of methyl alcohol Preparation of Biodiesel by Supercritical Method is: grease (triglyceride) is placed in methyl alcohol the tubular reactor that stainless steel is made, and is heated to methyl alcohol supercritical state under the condition that does not add catalyzer, and meeting transesterification reaction, generates biofuel.Because methyl alcohol can dissociate into CH under super critical condition under the katalysis of reactor metal wall
3o
-+ H
+.CH
3o
-in Sauerstoffatom can attack carbonylic carbon atom on triglyceride, there is nucleophilic reaction, through generating intermediate, finally generate target product methyl esters.Here the oxygen on methyl alcohol has electronegativity, is therefore a kind of alkali.So methyl alcohol is reaction medium, be also reactant, or the alkaline catalysts of transesterification reaction.
The technical scheme that technical solution problem of the present invention adopts is:
A kind of method of coal-based methanol and plam oil Preparation of Biodiesel by Supercritical Method, coal-based methanol and plam oil are sent into preheater continuously with the ratio of 30:1-40:1, mix and be preheating to temperature 300-350 ℃, then send into tubular reactor, do not adding under the condition of catalyzer, make methyl alcohol under supercritical state, carry out the transesterification reaction of grease, generate biofuel and glycerine; In tubular reactor, control temperature of reaction is 300-350 ℃, and reaction pressure is at 15-20Mpa, and the reaction times is 5-15 minute; Reaction product obtains coarse biodiesel and thick methyl alcohol through decompression, phase-splitting; Coarse biodiesel is carried out to rectifying, to eliminate the impact on product biofuel quality of impurity in coal-based methanol, obtain biofuel and residual oil that purity is higher; Thick methanol gas is carried out to rectifying, obtain the methyl alcohol that purity is higher, then return and plam oil batching, recycle.
Described plam oil replaces with palm oil foot or plam oil Chinese honey locust.
A device for coal-based methanol and plam oil Preparation of Biodiesel by Supercritical Method, comprises that methyl alcohol storage tank 1 is connected with preheater 5 by the first ram pump 2; Grease storage tank 3 is connected with preheater 5 by the second ram pump 4; Preheater 5 is connected with tubular reactor 6; Tubular reactor 6 is connected with gas-liquid separator 8, and tubular reactor 6 arranges reducing valve 7, and gas-liquid separator 8 is connected with rectification under vacuum tower 9 by pump 12, and gas-liquid separator 8 is connected with methanol rectifying tower 10; Methanol rectifying tower 10 tower tops are connected with methyl alcohol storage tank 1, at the bottom of methanol rectifying tower 10 towers, are connected again with gas-liquid separator 8; Rectification under vacuum tower 9 is connected with vacuum pump 11.
Described preheater 5 is static mixer, and the inner stainless steel cross-leaf of placing is outsidely wound around electric stove wire heating and by temp controlled meter A.T.C.
Described tubular reactor 6 is spiral tube, and material is stainless steel, and outside twines electric stove wire heating, by temp controlled meter, controls temperature of reaction, and setting pressure sensor is installed reducing valve to control the pressure of reaction process to measure pressure, to export.
Described gas-liquid separator 8 is cylindrical shell, and material is stainless steel.
Described rectification under vacuum tower 9 is Stainless Steel Helices tower; Described methanol rectifying tower 10 is Stainless Steel Helices tower.
Described all overcritical equipment is specific equipment, can bear the temperature of 500 ℃ and the internal pressure of 50MPa.
The present invention utilizes wide material sources, low-cost coal-based methanol and plam oil to make raw material, utilize the autocatalysis character of supercritical methanol itself, the transesterification that issues oil generation fat in the condition that does not add catalyzer is prepared coarse biodiesel, then rectification under vacuum obtains the measured biofuel of matter to coarse biodiesel.Both utilize cheap raw material, avoided again the conventional catalyst supercritical methanol technology acidand basecatalysts problem difficult separated with catalyzer with product to the corrosion of equipment.Have equipment corrosion little, without separating catalyst, environmental friendliness, biofuel quality is good and methyl esters transforms advantages such as high (92-97%), is suitable for serialization scale operation.
Accompanying drawing explanation
Fig. 1 is technical process of the present invention and apparatus structure schematic diagram; Wherein each label is:
1-methyl alcohol storage tank, 2-the first ram pump, 3-grease storage tank, 4-the second ram pump, 5-preheater, 6-tubular reactor, 7-reducing valve, 8-gas-liquid separator, 9-rectification under vacuum tower, 10-methanol rectifying tower, 11-vacuum pump, 12-pump.
Specific embodiments
Technical process of the present invention and apparatus structure schematic diagram are as shown in Figure 1, the right is first and second ram pump 2 and 4 that charging is used, respectively the feed liquid plam oil of the feed liquid coal-based methanol of methyl alcohol storage tank 1 and grease storage tank 3 being sent into continuously to upper right side preheater 5 mixes and preheating, feed liquid reaches the tubular reactor 6 that enters middle part after temperature required, make coal-based methanol under supercritical state, carry out the transesterification reaction of grease, generate coarse biodiesel and glycerine.Reaction product enters the gas-liquid separator 8 of bottom after reducing valve 7 decompressions, is divided into gas phase and two liquid phases: gas phase is thick methanol gas, and the upper strata of liquid phase is coarse biodiesel, and lower floor is raw glycerine.Coarse biodiesel is sent into 9 rectifying of rectification under vacuum tower with pump 12, and rectification under vacuum tower 9 is connected with vacuum pump 11.From rectifying tower 9 tower tops out be biofuel, at the bottom of tower out be oil fuel (residual oil).From gas-liquid separator 8 thick methanol gas out, enter methanol rectifying tower 10, from rectifying tower 10 tower tops out be methyl alcohol, send methyl alcohol storage tank 1 back to; At the bottom of tower, high boiling liquid is out sent gas-liquid separator 8 back to.By biofuel measure, sampling analysis, calculated yield.
The structure of described preheater 5 is: Φ 20 * 1000mm static mixer, the inner 304 stainless steel cross-leafs of placing, are outsidely wound around electric stove wire heating and by temp controlled meter A.T.C.
Described tubular reactor 6 structures are: Φ 20 * 5000mm spiral tube, and the flow-pattern that makes to manage interior medium is plug flow, material is 304 stainless steels.Outside twines electric stove wire heating, by temp controlled meter, automatically controls temperature of reaction, and setting pressure sensor is to measure pressure, by adjusting, exports the pressure that reducing valve is controlled reaction process.
Described phase splitter 8 structures are: Φ 300 * 600mm cylindrical shell, material is 304 stainless steels.
Described all overcritical equipment is specific equipment, can bear the temperature of 500 ℃ and the internal pressure of 50MPa.
Described rectification under vacuum tower 9 is the 304 Stainless Steel Helices towers of Φ 200 * 4000mm; Described methanol rectifying tower 10 is the 304 Stainless Steel Helices towers of Φ 300 * 5000mm.
Embodiment 1
With ram pump 2 and 4 by coal-based methanol: plam oil proportioning is 40:1, respectively the palm oil grease in the coal-based methanol in methyl alcohol storage tank 1 and grease storage tank 3 is sent into Φ 20 * 1000mm preheater 5 continuously, after mixing and being preheated to 350 ℃ of temperature, enter the tubular reactor 6 of Φ 20 * 5000mm spiral tube, make coal-based methanol under supercritical state, carry out the transesterification reaction of grease, generate coarse biodiesel and glycerine.The temperature of the power input control tubular reactor 6 by automatic control electrical heating is at 350 ℃, pressure at 20MPa, and by the aperture that control exports reducing valve 7, to regulate the residence time of reactant in tubular reactor 6 be 5 minutes.Reaction product enters Φ 300 * 600mm gas-liquid separator 8 and is divided into gas phase (thick methyl alcohol) and two liquid phases (upper strata is coarse biodiesel, and lower floor is raw glycerine) after decompression.Coarse biodiesel is carried out to rectifying with the filler decompression rectifying tower 9 that pump 12 is sent into Φ 200 * 4000mm, and in control tower, vacuum tightness is 0.08-0.05MPa.From rectifying tower 9 tower tops, obtain biofuel, at the bottom of tower out be oil fuel (residual oil).Biofuel is measured and sampled, by gas-chromatography, analyze, obtaining methyl ester conversion rate is 97%.Thick methanol gas enters the filler methanol rectifying tower 10 of Φ 300 * 5000mm, and from rectifying tower 10 tower tops, obtaining purity is 99% methyl alcohol, sends methyl alcohol storage tank 1 back to; At the bottom of tower, high boiling liquid is out sent recycling in gas-liquid separator 8 back to.
Embodiment 2
With ram pump 2 and 4 by coal-based methanol: palm oil foot proportioning is 30:1, respectively the palm oil foot in the coal-based methanol in methyl alcohol storage tank 1 and grease storage tank 3 is sent into Φ 20 * 1000mm preheater 5 continuously, after mixing and being preheated to 300 ℃ of temperature, enter the tubular reactor 6 of Φ 20 * 5000mm spiral tube, make methyl alcohol under supercritical state, carry out the transesterification reaction of grease, generate biofuel and glycerine.Power by automatic control electrical heating is inputted, and the temperature of controlling tubular reactor 6 is at 300 ℃, pressure at 15MPa, and by the aperture that control exports reducing valve 7, to regulate the residence time of reactant in tubular reactor 6 be 15 minutes.Reaction product enters Φ 300 * 600mm gas-liquid separator 8 and is divided into gas phase (thick methyl alcohol) and two liquid phases (upper strata is coarse biodiesel, and lower floor is raw glycerine) after decompression.Coarse biodiesel is carried out to rectifying with the filler decompression rectifying tower 9 that pump 12 is sent into Φ 200 * 4000mm, and in control tower, vacuum tightness is 0.08-0.05MPa.From rectifying tower 9 tower tops, obtain biofuel, at the bottom of tower out be oil fuel.Biofuel is measured and sampled, by gas-chromatography, analyze, obtaining methyl ester conversion rate is 92%.Thick methanol gas enters the filler methanol rectifying tower 10 of Φ 300 * 5000mm, and from rectifying tower 10 tower tops, obtaining purity is 99% methyl alcohol, sends methyl alcohol storage tank 1 back to; At the bottom of tower, high boiling liquid is out sent recycling in gas-liquid separator 8 back to.
Embodiment 3
With ram pump 2 and 4 by coal-based methanol: palm oil foot proportioning is 35:1, respectively the palm oil foot in the coal-based methanol in methyl alcohol storage tank 1 and grease storage tank 3 is sent into Φ 20 * 1000mm preheater 5 continuously, after mixing and being preheated to 320 ℃ of temperature, enter the tubular reactor 6 of Φ 20 * 5000mm spiral tube, make methyl alcohol under supercritical state, carry out the transesterification reaction of grease, generate biofuel and glycerine.Power by automatic control electrical heating is inputted, and the temperature of controlling tubular reactor 6 is at 300 ℃, pressure at 17MPa, and by the aperture that control exports reducing valve 7, to regulate the residence time of reactant in tubular reactor 6 be 10 minutes.Reaction product enters Φ 300 * 600mm gas-liquid separator 8 and is divided into gas phase (thick methyl alcohol) and two liquid phases (upper strata is coarse biodiesel, and lower floor is raw glycerine) after decompression.Coarse biodiesel is carried out to rectifying with the filler decompression rectifying tower 9 that pump 12 is sent into Φ 200 * 4000mm, and in control tower, vacuum tightness is 0.08-0.05MPa.From rectifying tower 9 tower tops, obtain biofuel, at the bottom of tower out be oil fuel.Biofuel is measured and sampled, by gas-chromatography, analyze, obtaining methyl ester conversion rate is 95%.Thick methanol gas enters the filler methanol rectifying tower 10 of Φ 300 * 5000mm, and from rectifying tower 10 tower tops, obtaining purity is 99% methyl alcohol, sends methyl alcohol storage tank 1 back to; At the bottom of tower, high boiling liquid is out sent recycling in gas-liquid separator 8 back to.
Claims (7)
1. the method for a coal-based methanol and plam oil Preparation of Biodiesel by Supercritical Method, it is characterized in that, coal-based methanol and plam oil are sent into preheater continuously with the ratio of 30:1-40:1, mix and be preheating to temperature 300-350 ℃, then send into tubular reactor, do not adding under the condition of catalyzer, making methyl alcohol under supercritical state, carry out the transesterification reaction of grease, generating biofuel and glycerine; In tubular reactor, control temperature of reaction is 300-350 ℃, and reaction pressure is at 15-20Mpa, and the reaction times is 5-15 minute; Reaction product obtains coarse biodiesel and thick methyl alcohol through decompression, phase-splitting; Coarse biodiesel is carried out to rectifying, obtain biofuel and residual oil that purity is higher; Thick methanol gas is carried out to rectifying, obtain the methyl alcohol that purity is higher, then return and plam oil batching, recycle.
2. method according to claim 1, is characterized in that, described plam oil replaces with palm oil foot or plam oil Chinese honey locust.
3. a device for coal-based methanol and plam oil Preparation of Biodiesel by Supercritical Method, is characterized in that, comprises that methyl alcohol storage tank (1) is connected with preheater (5) by the first ram pump (2); Grease storage tank (3) is connected with preheater (5) by the second ram pump (4); Preheater (5) is connected with tubular reactor (6); Tubular reactor (6) is connected with gas-liquid separator (8), and tubular reactor (6) arranges reducing valve (7), and gas-liquid separator (8) is connected with rectification under vacuum tower (9) by pump (12), and gas-liquid separator (8) is connected with methanol rectifying tower (10); Methanol rectifying tower (10) tower top is connected with methyl alcohol storage tank (1), at the bottom of methanol rectifying tower (10) tower, is connected again with gas-liquid separator (8); Rectification under vacuum tower (9) is connected with vacuum pump (11).
4. device according to claim 3, is characterized in that, described preheater (5) is static mixer, and the inner stainless steel cross-leaf of placing is outsidely wound around electric stove wire heating and by temp controlled meter A.T.C.
5. device according to claim 3, it is characterized in that, described tubular reactor (6) is spiral tube, the flow-pattern that makes to manage interior medium is plug flow, material is stainless steel, and outside twines electric stove wire heating, by temp controlled meter, controls temperature of reaction, and setting pressure sensor is installed reducing valve to control the pressure of reaction process to measure pressure, to export.
6. device according to claim 3, is characterized in that, described gas-liquid separator (8) is cylindrical shell, and material is stainless steel.
7. device according to claim 3, is characterized in that, described rectification under vacuum tower (9) is Stainless Steel Helices tower; Described methanol rectifying tower (10) is Stainless Steel Helices tower.
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Cited By (6)
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| CN104789367A (en) * | 2015-03-27 | 2015-07-22 | 江苏大学 | Biodiesel preparing device |
| CN105385506A (en) * | 2015-12-10 | 2016-03-09 | 华南理工大学 | Apparatus and method for producing biodiesel through solid base catalysis heterogeneous ester interchange technology |
| WO2016048233A1 (en) * | 2014-09-24 | 2016-03-31 | Power 8 Energy Pte Ltd | Method for producing liquid crude palm-coal oil |
| CN105505590A (en) * | 2016-01-13 | 2016-04-20 | 山东联星能源集团有限公司 | Method for preparing biodiesel through supercritical extraction method |
| CN108219979A (en) * | 2016-12-22 | 2018-06-29 | 内蒙古中细软技术开发有限公司 | Supercritical extraction biodiesel synthesis |
| 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016048233A1 (en) * | 2014-09-24 | 2016-03-31 | Power 8 Energy Pte Ltd | Method for producing liquid crude palm-coal oil |
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Application publication date: 20140326 |