CN104031747A - Production device and method of biodiesel - Google Patents
Production device and method of biodiesel Download PDFInfo
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- CN104031747A CN104031747A CN201410261146.1A CN201410261146A CN104031747A CN 104031747 A CN104031747 A CN 104031747A CN 201410261146 A CN201410261146 A CN 201410261146A CN 104031747 A CN104031747 A CN 104031747A
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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 invention discloses a production device and method of biodiesel and belongs to the technical field of preparation of biodiesel. The production device comprises a tower-kettle integrated device, a rectifying tower, a flash tower and a separation tower. The production method comprises the following steps: carrying out a countercurrent contact reaction on grease which flows downward through a catalyst reaction layer and gas phase methanol; recovering unreacted methanol; introducing reaction products through a temperature raising layer to a layering kettle to further separate polar products and coarse oil products; and rectifying or separating and purifying to obtain multifunctional biodiesel. According to the production device and method disclosed by the invention, solid-liquid-gas phase catalytic reactions are carried out in the catalytic reaction layer of a reaction tower, so that the reactants and the catalyst fully contact for efficient reaction, and the conversion ratio is increased by 10-25% than that in the prior art. The production device is reasonable in design, high in product purity and complete in cyclic utilization and suitable for market promotion and has a very good application prospect.
Description
Technical field
The present invention relates to a kind of production equipment and production method of biofuel, be specifically related to a kind of method of tower reactor integrated production equipment and production multifunctional bio diesel oil thereof, belong to the preparing technical field of biofuel.
Background technology
Biofuel is a kind of green, environmental protection, reproducible secondary energy, compare with primary energy source petroleum diesel, there is flash-point high, store transportation safety, self is biodegradable, the advantage such as environmentally friendly, and in its fire emission, the harmful substance contents such as sulfurous gas, sulfide, carbonic acid gas is low.Biofuel replaces petroleum diesel can alleviate the present situation of diesel oil supply shortage, and then alleviates oil supply crisis.
The preparation of biofuel is to take animal-plant oil as raw material, with methyl alcohol or ethanol, under catalyst action, through transesterify, makes, and its method has acid-base catalysis method, catalyzed by biological enzyme and supercritical methanol technology.Biofuel scale operation both at home and abroad all be take traditional homogeneous catalysis method as main, take grease and methyl alcohol as reactant, with liquid acid (HCl, H
2sO
4, HNO
3deng) and liquid base (NaOH, KOH etc.) carry out esterification and transesterification reaction production biofuel for catalyzer.And adopt homogeneous acid or base catalysis biofuel processed (as CN1473907A, DE3444893 etc.) to remove catalyzer by neutralization and washing.Caused thus the acid of research multiphase solid or alkaline catalysts (CN101338215A, CN101289629A, CN101294096A etc.), but be only the research in laboratory, it is limited to the improvement of reaction process and the innovation of production equipment.
The production technique of overwhelming majority biofuel is all carried out with tank reactor, the methyl alcohol of polarity and nonpolar grease are immiscible mutually, and reactor stir speed (S.S.) is low, as mentioned revolution in CN101245253A, be 30～50r/min, alcohol oil two-phase can not fully contact and react like this, causes reaction conversion ratio low.Different reaction process, temperature of reaction and pressure are also different, generally at 65 ℃～280 ℃, (application number is 200610165102.4 to temperature, 200710037601.X patent), from normal pressure to overcritical, (application number is 201010161581.9 to pressure, 200810017849.4,200610010882.5 patent).Insoluble practical problems is that the methyl alcohol (or ethanol) of polarity and nonpolar animal-plant oil do not dissolve each other and make itself and catalyzer contact area little and cause sluggish or low conversion rate etc. always.
In addition, biofuel is applied in engine, having obvious attribute problem is that its viscosity (1.9-6.0) is greater than petroleum diesel (1.3-4.1) [Renewable and Sustainable Energy Reviews 35 (2014) 136 – 153], large mainly due to its raw material sources complexity and molecular weight, so can be isolated out according to the boiling point of product in process of production light constituent and the large heavy constituent of viscosity that viscosity is little, to its utilization, be very with practical value and social effect respectively.
Summary of the invention
The present invention aims to provide a kind of production equipment and production method of biofuel, has solved the problem that grease is immiscible with methyl alcohol in transesterification reaction, catalyzer can not fully contact with reactant.The invention provides a kind of tower reactor integrated apparatus, the methyl alcohol of liquid grease, gaseous state and the mode that solid catalyst three contacts have been realized, carry out catalyzed reaction and prepare the biofuel of different boiling, thereby realize High-efficient Production and the multifunctional usage of biofuel.
The present invention is achieved by the following technical solutions:
A production equipment for biofuel, comprises tower reactor integrated apparatus and rectifying tower, flashing tower, knockout tower; Described tower reactor integrated apparatus is comprised of reaction tower and stratification still, and reaction tower is tube structure, and reaction tower upper strata is catalytic reaction layer, and lower floor is methyl alcohol temperature raising layer, and the bottom of methyl alcohol temperature raising layer connects stratification still; The top of catalytic reaction layer is provided with grease entrance, and reaction tower middle part is provided with gas-phase methanol entrance, and reaction tower top is provided with methanol eddy device; The bottom of stratification still connects polarity storage tank, and middle part connects thick oily product storage tank; Described thick oily product storage tank connects one-level rectifying tower, two-stage rectification tower, three grades of rectifying tower successively, finally leads to grease storage tank; Described polarity storage tank connects methyl alcohol flashing tower and glycerine knockout tower successively.
In above-mentioned production equipment, described catalytic reaction layer is to be mixed by filler and solid catalyst, by filler, makes to support the bed forming.
In above-mentioned production equipment, described methyl alcohol temperature raising layer is to be formed by the symmetrical alternative arrangement of the column plate of heating of 10 ° of tilting; Or methyl alcohol temperature raising layer is comprised of the spiral plate body at 10 °, duplex inclination angle.
The aspect ratio of described catalytic reaction layer and methyl alcohol temperature raising layer is: 4 ~ 10:1.
A production method for biofuel, comprises the following steps:
(1) glyceride stock enters reaction tower from the grease entrance on reaction tower top, methyl alcohol enters reaction tower from the middle part of reaction tower, the methyl alcohol that enters reaction tower rises and enters catalyst reaction layer with gas phase state, grease reacts with gas-phase methanol counter current contact through catalyst reaction layer downwards, unreacted methyl alcohol rises to tower top and returns to reaction tower by methanol eddy device, and another part enters methyl alcohol storage tank;
(2) reaction product flows into temperature raising layer downwards along bed, and the methyl alcohol dissolving each other with product again gasifies and enters beds and react with grease at temperature raising layer, and other products continue to flow into stratification in stratification still downwards;
(3) after reaction product stratification, lower floor is polarity, enters polarity storage tank, and upper strata is thick oily product, enters thick oily product storage tank;
(4) thick oily product steams the methyl alcohol of dissolving by one-level rectifying tower, methyl alcohol enters methyl alcohol storage tank and recycles after methanol separator separation, the thick oily product that single flash goes out steams lower boiling light constituent biofuel by two-stage rectification tower again, finally by three grades of rectifying tower, steam high boiling heavy constituent biofuel, the unreacted high boiling point grease distilling out for three times returns to grease storage tank and recycles;
(5) polarity first flashes off methyl alcohol enter methanol separator through flashing tower, and isolated methyl alcohol enters methyl alcohol storage tank and recycles, and the product after flash distillation distills out the water of generation by glycerine knockout tower from tower top, obtain by-product glycerin at the bottom of tower.
In aforementioned production method, described grease comprises: one or more mixing of rapeseed oil, soybean oil, peanut oil or non-grain Vegetable oil lipoprotein or pretreated meal kitchen waste oil, sewer oil, acidification oil.
In aforementioned production method, described catalyzer is solid base catalyst or solid acid catalyst.Specifically, described catalyzer is solid alkali CaO, MgO, K
2o-Cao, NaY, KZSM-5, Ca-K/MCM41 or solid acid ZrO
2, Zr-SBA-15, SO
4 2-/ SBA-15, H
β, SO
4 2-a kind of in/C.
In aforementioned production method, the mol ratio of described catalyzed reaction methyl alcohol and grease is 20～100:1.
In aforementioned production method, described reaction bed temperature is 60 ℃～220 ℃; Described temperature raising layer temperature is 120 ℃～230 ℃.
In aforementioned production method, described reaction pressure is the spontaneous pressure of methyl alcohol under corresponding temperature of reaction, and pressure range is: 0.1～5.6MPa.Not another plus-pressure.
In aforementioned production method, described light constituent biofuel is the ester class product that is less than C18, and heavy constituent biofuel is the ester class product that is more than or equal to C18.
In aforementioned production method, described polarity comprises methyl alcohol, glycerine, water etc.
Of the present invention
beneficial effect:
(1) at reaction bed, carry out solid-liquid-gas three phase catalyzed reaction, thereby make reactant can contact fully highly effective reaction with catalyzer, than the method for production biofuel under existing the same terms, transformation efficiency improves 10-25%.
(2) production equipment is reasonable in design, and product purity is high, and realizes recycle to extinction utilization, is applicable to marketing.
(3) reaction product is produced the biofuel of different viscositys according to boiling point difference, is applicable to multifunctional usage, as automobile fuel, flotation reagent, lubricating oil, inert ingredient, original position mining separating agent etc., has extraordinary application prospect.
Accompanying drawing explanation
fig. 1 is biodiesel production apparatus schematic diagram.
1-responding layer in figure; 2-temperature raising layer; 3-stratification still; 4-polarity storage tank; 5-thick oily product storage tank; 6-one-level rectifying tower; 7-two-stage rectification tower; 8-three grades of rectifying tower; 9-methyl alcohol flashing tower; 10-glycerine knockout tower; 11-grease storage tank; 12-methanol separator; 13-methyl alcohol storage tank; E-1-stock oil sampling pump; E-2-methanol pump.
Embodiment
Below by embodiment, further illustrate the present invention, but be not limited to following examples.
Fig. 1 is the production equipment schematic diagram of biofuel of the present invention.A production equipment for biofuel, comprises tower reactor integrated apparatus and rectifying tower, flashing tower, knockout tower; Described tower reactor integrated apparatus is comprised of reaction tower and stratification still 3, and reaction tower is tube structure, and reaction tower upper strata is catalytic reaction layer 1, and lower floor is methyl alcohol temperature raising layer 2, and the bottom of methyl alcohol temperature raising layer 2 connects stratification still 3; The top of catalytic reaction layer 1 is provided with grease entrance, and reaction tower middle part is provided with gas-phase methanol entrance, and reaction tower top is provided with methanol eddy device; The bottom of stratification still 3 connects polarity storage tank 4, and middle part connects thick oily product storage tank 5; Described thick oily product storage tank 5 connects one-level rectifying tower 6, two-stage rectification tower 7, three grades of rectifying tower 8 successively, finally leads to grease storage tank 11; Described polarity storage tank 4 connects methyl alcohol flashing tower 9 and glycerine knockout tower 10 successively.
In above-mentioned production equipment, described catalytic reaction layer is to be mixed by filler and solid catalyst, by filler, makes to support the bed forming; Described methyl alcohol temperature raising layer is by tilting the symmetrical alternative arrangement of the column plate of heating of 10 ° or be comprised of the spiral plate body at 10 °, duplex inclination angle.The aspect ratio of described catalytic reaction layer and methyl alcohol temperature raising layer is: 4 ~ 10:1.
Below by concrete experimental data, illustrate that the present invention prepares the production method of biofuel:
Embodiment 1:
The soybean oil of 0.72kg/h enters (0.1MPa) reaction tower by pump E-1 from tower top, flow to CaO catalyst reaction layer 1 downwards, 82 ℃ of temperature, the methyl alcohol of 1kg/h is entered from tower waist by pump E-2,120 ℃ of temperature, gas-phase methanol upwards enters CaO catalyst reaction layer, react with soybean oil counter current contact, 94 ℃ of temperature of reaction, it is 1.1:1 by reflux ratio that unreacted methyl alcohol rises to tower top (83.2 ℃ of temperature), part is returned to reaction tower, and another part enters methyl alcohol storage tank 13.Reaction product is along flowing to 135 ℃ of temperature raising layer 2(temperature under bed), the methyl alcohol dissolving each other again gasifies and enters 1 reaction of CaO catalyst reaction layer at temperature raising layer 2, and other products flow to stratification in stratification still 3 under continuing.Lower floor is dissolved with the apolar substances such as the glycerine of methyl alcohol enters polarity storage tank 4, and upper strata is fatty acid methyl ester to enter thick oily product storage tank 5.Thick oily product steams the methyl alcohol of dissolving by one-level rectifying tower 6, enter methanol separator 12, bottoms steams lower boiling light biodiesel fuel component 0.184kg/h by two-stage rectification tower 7 again, finally by three grades of rectifying tower 8, steam high boiling heavy biodiesel fuel component 0.493kg/h, unreacted high boiling point grease 0.056kg/h returns to grease storage tank 11 and recycles.The product of polarity storage tank 4 first flashes off methyl alcohol through methyl alcohol flashing tower 9 and enters methanol separator 12, isolated methyl alcohol enters methyl alcohol storage tank 13 and recycles, then by glycerine knockout tower 10, the little water of generation is distilled out from tower top, at the bottom of tower, obtain by-product glycerin 0.053kg/h.
Embodiment 2:
The pretreated sewer oil of 1kg/h (acid number 3.2mgKOH/g) enters (0.2MPa) by pump E-1 from tower top and flows to Zr-SBA-15 catalyst reaction layer 1 downwards, 138 ℃ of temperature, the methyl alcohol of 3.56kg/h is entered from tower waist by pump E-2,180 ℃ of temperature, gas-phase methanol upwards enters Zr-SBA-15 catalyst reaction layer, react with pretreated sewer oil counter current contact, 160 ℃ of temperature of reaction, it is 1.2:1 by reflux ratio that unreacted methyl alcohol rises to tower top (140.4 ℃ of temperature), part is returned to reaction tower, and another part enters methyl alcohol storage tank 13.Reaction product is along flowing to 205 ℃ of temperature raising layer 2(temperature under bed), the methyl alcohol dissolving each other again gasifies and enters 1 reaction of Zr-SBA-15 beds at temperature raising layer 2, and other products flow to stratification in stratification still 3 under continuing.Lower floor is dissolved with the apolar substances such as the glycerine of methyl alcohol enters polarity storage tank 4, and upper strata is fatty acid methyl ester to enter thick oily product storage tank 5.Thick oily product steams the methyl alcohol of dissolving by one-level rectifying tower 6, enter methanol separator 12, bottoms steams lower boiling light biodiesel fuel component 0.255kg/h by two-stage rectification tower 7 again, finally by three grades of rectifying tower 8, steam high boiling heavy biodiesel fuel component 0.685kg/h, unreacted high boiling point grease (acid number is 0.01mgKOH/g) 0.078kg/h returns to grease storage tank 11 and recycles.The product of polarity storage tank 4 first flashes off methyl alcohol through methyl alcohol flashing tower 9, enter methanol separator 12, isolated methyl alcohol enters methyl alcohol storage tank 13 and recycles, and then by glycerine knockout tower 10, the 0.21g/h water of generation is distilled out from tower top, obtains by-product glycerin 0.074kg/h at the bottom of tower.
Embodiment 3:
The pretreated meal of 1kg/h kitchen waste oil (acid number 4.4mgKOH/g) enters (0.15MPa) reaction tower by pump E-1 from tower top, flows to H downwards
βcatalyst reaction layer 1,138 ℃ of temperature, the methyl alcohol of 1.45kg/h is entered from tower waist by pump E-2,190 ℃ of temperature, gas-phase methanol upwards enters H
βbeds, reacts with pretreated meal kitchen waste oil counter current contact, 150 ℃ of temperature of reaction, and it is 1.0:1 by reflux ratio that unreacted methyl alcohol rises to tower top (139.5 ℃ of temperature), and part is returned to reaction tower, and another part enters methyl alcohol storage tank 13.Reaction product is along flowing to 230 ℃ of temperature raising layer 2(temperature under bed), the methyl alcohol dissolving each other again gasifies and enters H at temperature raising layer 2
β1 reaction of catalyst reaction layer, other products flow to stratification in stratification still 3 under continuing.Lower floor is dissolved with the apolar substances such as the glycerine of methyl alcohol enters polarity storage tank 4, and upper strata is fatty acid methyl ester to enter thick oily product storage tank 5.Thick oily product steams the methyl alcohol of dissolving by one-level rectifying tower 6, enter methanol separator 12, bottoms steams lower boiling light biodiesel fuel component 0.312kg/h by two-stage rectification tower 7 again, finally by three grades of rectifying tower 8, steam high boiling heavy biodiesel fuel component 0.638kg/h, unreacted high boiling point grease 0.069kg/h returns to grease storage tank 11 and recycles.The product of polarity storage tank 4 first flashes off methyl alcohol through methyl alcohol flashing tower 9, enter methanol separator 12, isolated methyl alcohol enters methyl alcohol storage tank 13 and recycles, and then by glycerine knockout tower 10, the 0.29g/h water of generation is distilled out from tower top, obtains by-product glycerin 0.081kg/h at the bottom of tower.
Claims (10)
1. a production equipment for biofuel, comprises tower reactor integrated apparatus and rectifying tower, flashing tower, knockout tower; Described tower reactor integrated apparatus is comprised of reaction tower and stratification still, and reaction tower is tube structure, and reaction tower upper strata is catalytic reaction layer, and lower floor is methyl alcohol temperature raising layer, and the bottom of methyl alcohol temperature raising layer connects stratification still; The top of catalytic reaction layer is provided with grease entrance, and reaction tower middle part is provided with gas-phase methanol entrance, and reaction tower top is provided with methanol eddy device; The bottom of stratification still connects polarity storage tank, and middle part connects thick oily product storage tank; Described thick oily product storage tank connects one-level rectifying tower, two-stage rectification tower, three grades of rectifying tower successively, finally leads to grease storage tank; Described polarity storage tank connects methyl alcohol flashing tower and glycerine knockout tower successively.
2. production equipment according to claim 1, is characterized in that: described catalytic reaction layer is to be mixed by filler and solid catalyst, by filler, makes to support the bed forming; Described methyl alcohol temperature raising layer is to be formed by the symmetrical alternative arrangement of the column plate of heating of 10 ° of tilting.
3. production equipment according to claim 1, is characterized in that: described methyl alcohol temperature raising layer is comprised of the spiral plate body at 10 °, duplex inclination angle.
4. production equipment according to claim 1, is characterized in that: the aspect ratio of described catalytic reaction layer and methyl alcohol temperature raising layer is: 4 ~ 10:1.
5. a method that adopts the production equipment production biofuel described in described claim 1 ~ 4 any one, is characterized in that: comprise the following steps:
(1) glyceride stock enters reaction tower from the grease entrance on reaction tower top, methyl alcohol enters reaction tower from the middle part of reaction tower, the methyl alcohol that enters reaction tower rises and enters catalyst reaction layer with gas phase state, grease reacts with gas-phase methanol counter current contact through catalyst reaction layer downwards, unreacted methyl alcohol rises to tower top and returns to reaction tower by methanol eddy device, and another part enters methyl alcohol storage tank;
(2) reaction product flows into temperature raising layer downwards along bed, and the methyl alcohol dissolving each other with product again gasifies and enters beds and react with grease at temperature raising layer, and other products continue to flow into stratification in stratification still downwards;
(3) after reaction product stratification, lower floor is polarity, enters polarity storage tank, and upper strata is thick oily product, enters thick oily product storage tank;
(4) thick oily product steams the methyl alcohol of dissolving by one-level rectifying tower, methyl alcohol enters methyl alcohol storage tank and recycles after methanol separator separation, the thick oily product that single flash goes out steams lower boiling light constituent biofuel by two-stage rectification tower again, finally by three grades of rectifying tower, steam high boiling heavy constituent biofuel, at the bottom of tower, remaining unreacted high boiling point grease returns to grease storage tank and recycles;
(5) polarity first flashes off methyl alcohol enter methanol separator through flashing tower, and isolated methyl alcohol enters methyl alcohol storage tank and recycles, and the product after flash distillation distills out the water of generation by glycerine knockout tower from tower top, obtain by-product glycerin at the bottom of tower.
6. the production method of biofuel according to claim 5, is characterized in that: described grease comprises: one or more mixing of rapeseed oil, soybean oil, peanut oil or non-grain Vegetable oil lipoprotein or pretreated meal kitchen waste oil, sewer oil, acidification oil.
7. the production method of biofuel according to claim 5, is characterized in that: described catalyzer is solid alkali CaO, MgO, K
2o-Cao, NaY, KZSM-5, Ca-K/MCM41 or solid acid ZrO
2, Zr-SBA-15, SO
4 2-/ SBA-15, H
β, SO
4 2-a kind of in/C.
8. the production method of biofuel according to claim 5, is characterized in that: the mol ratio of described catalyzed reaction methyl alcohol and grease is 20～100:1.
9. the production method of biofuel according to claim 5, is characterized in that: described reaction bed temperature is 60 ℃～220 ℃; Described temperature raising layer temperature is 120 ℃～230 ℃; Described reaction pressure is the spontaneous pressure of methyl alcohol under corresponding temperature of reaction, and pressure range is: 0.1～5.6MPa.
10. the production method of biofuel according to claim 5, is characterized in that: described light constituent biofuel is the ester class product that is less than C18, and heavy constituent biofuel is the ester class product that is more than or equal to C18.
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Cited By (6)
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| 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 |
| CN106588958A (en) * | 2015-10-14 | 2017-04-26 | 上虞新和成生物化工有限公司 | Production system and method for continuously preparing alkynol di-Grignard reagent |
| CN108373947A (en) * | 2018-04-08 | 2018-08-07 | 淮阴师范学院 | A kind of process units and preparation method of composite biodiesel |
| CN108949366A (en) * | 2018-07-13 | 2018-12-07 | 中国科学院青岛生物能源与过程研究所 | A kind of ester exchange process and device can be used for producing biodiesel |
| CN110055121A (en) * | 2019-04-25 | 2019-07-26 | 唐山金利海生物柴油股份有限公司 | A kind of biodiesel prepares the device and its application method of lubricating oil |
| CN110172377A (en) * | 2019-06-20 | 2019-08-27 | 成都恒润高新科技股份有限公司 | A method of biodiesel is continuously prepared using waste animal and vegetable oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106588958A (en) * | 2015-10-14 | 2017-04-26 | 上虞新和成生物化工有限公司 | Production system and method for continuously preparing alkynol di-Grignard reagent |
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| CN108373947A (en) * | 2018-04-08 | 2018-08-07 | 淮阴师范学院 | A kind of process units and preparation method of composite biodiesel |
| CN108949366A (en) * | 2018-07-13 | 2018-12-07 | 中国科学院青岛生物能源与过程研究所 | A kind of ester exchange process and device can be used for producing biodiesel |
| CN110055121A (en) * | 2019-04-25 | 2019-07-26 | 唐山金利海生物柴油股份有限公司 | A kind of biodiesel prepares the device and its application method of lubricating oil |
| CN110172377A (en) * | 2019-06-20 | 2019-08-27 | 成都恒润高新科技股份有限公司 | A method of biodiesel is continuously prepared using waste animal and vegetable oil |
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| CN104031747B (en) | 2016-02-24 |
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Application publication date: 20140910 Assignee: TAIYUAN NEW PROCESS TECHNOLOGY Co.,Ltd. Assignor: Taiyuan University of Technology Contract record no.: X2022140000005 Denomination of invention: A production device and method of biodiesel Granted publication date: 20160224 License type: Exclusive License Record date: 20220518 |