CN104194949B - A kind of preparation method of biodiesel - Google Patents

A kind of preparation method of biodiesel Download PDF

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Publication number
CN104194949B
CN104194949B CN201410374922.9A CN201410374922A CN104194949B CN 104194949 B CN104194949 B CN 104194949B CN 201410374922 A CN201410374922 A CN 201410374922A CN 104194949 B CN104194949 B CN 104194949B
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biodiesel
fatss
oils
hydrogenation
preparation
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CN104194949A (en
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张辉
陈庆
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SICHUAN YANGMING ENERGY TECHNOLOGY Co Ltd
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SICHUAN YANGMING ENERGY TECHNOLOGY Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Abstract

The present invention proposes a kind of preparation method of biodiesel.The method passes through long-neck valve homogenizer, make oils and fatss obtain with hydrogen to move under shearing and condition of high voltage at high speed, liquid molecular bond bursting, makes oils and fatss form reaction interface with hydrogen in continuous moving, is rapidly completed pre-hydrotreating reaction, further, channel outlet quick release pressure of the method by long-neck valve homogenizer, makes pre- hydrogenation thing contact deep hydrogenation with catalyst, and product enters rotating separation machine, biodiesel is separated by rotating separation machine with micro side-product, and continuously reclaim.The present invention is not only achieved and continuously prepares biodiesel, and avoids oils and fatss reaction for a long time at high temperature, the conversion ratio of nickel greatly improved, opens continuous, cleaning, efficiently produce the new technology of biodiesel.

Description

A kind of preparation method of biodiesel
Technical field
The present invention relates to fuel area, and in particular to a kind of preparation method of biodiesel.
Background technology
Biodiesel is the biomass fuel extracting from renewable fat or grease, due to general vegetable oil and moves Thing oil molecule is 14～18 carbochain compositions, extremely similar to the diesel fuel characteristicses of the carbochain composition of 15 or so, therefore biological bavin Oil is used directly for Diesel engine or is used in mixed way with diesel oil.Biodiesel can be regenerated due to its raw material, shown The good feature of environmental protection and sustainability, become the good succedaneum of diesel oil.And biodiesel compared with petrifaction diesel also with Lower advantage：In biodiesel, sulfur content is low so that the discharge of sulfur dioxide and sulfide is low, can reduce by about 30% sulphur emissions； Without the aromatic series alkane can polluted by environment in biodiesel, thus waste gas is less than petrifaction diesel to human body infringement；Raw The biological degradability of thing diesel oil is high；- 20 DEG C of biodiesel condensation point, with preferable cryogenic engine startability, freeze-proof Can be excellent；Biodiesel flash-point is low, is not belonging to dangerous materials；Cetane number is high, with good fuel performance.
The primary raw material of biodiesel is animal and plant fat, can carry out ester exchange reaction by oils and fatss and short chain alcohol and be obtained Fatty acid ester, containing side-products such as glycerol, monoglyceride, two sweet esters in fatty acid ester, is obtained biodiesel by separation. Ester exchange reaction prepare biodiesel when, due to adopt technique and condition difference can be divided into chemical method, supercritical methanol technology and Biological enzyme.Wherein chemical method is mainly acid catalyzed process, base catalysiss method, needs to use bronsted lowry acids and bases bronsted lowry, it is necessary to be neutralized and wash, So as to produce substantial amounts of sewage, and can not reuse, bring higher catalyst cost；Supercritical methanol technology technique needs high temperature High pressure, reaction rate is fast, high conversion rate, pollution-free, but invests and operating cost is high, and technology stability is poor, it is difficult to control；Biological Enzyme process reaction condition is gentle, non-pollutant discharge and without the need for washing, but catalyzing enzyme high expensive, and reacts slow, and efficiency is low.
By ester exchange reaction the viscosity of natural oil can reduce, improve fuel volatility, indices and bavin Oil is close to.But the method needs excessive low-carbon alcohols, later stage to reclaim refined difficulty, and the saponification produced in reaction causes product Emulsifying is difficult to separate, and produces substantial amounts of esterification waste water and be difficult to process in production process, and the discharge of salkali waste (acid) liquid causes two to environment Secondary pollution.And the moisture and free fatty in raw oil material can have a strong impact on bio-diesel yield and quality.For further Biodiesel quality is improved, strengthens adaptability, make by catalytic hydrocracking method the fatty acid ester hydrogenation deoxidation in vegetable oil break Chain generates saturated alkane, and its performance can replace petrifaction diesel completely.
Chinese invention patent application number discloses a kind of Vegetable oil lipoprotein catalytic hydrodeoxygenation for 201010234198.1 and prepares The method of diesel hydrocarbons, its adopt molybdenum carbide catalyst, and add organic solvent, and at 250-350 DEG C, pressure is under 1-10Mpa Hydroprocessing vegetable oils fat obtains the diesel component containing high heating value alkane.
Chinese invention patent application number be 200910155272.8 patent of invention disclose a kind of catalysis of Vegetable oil lipoprotein plus The method that hydrogen deoxidation prepares diesel component, its adopt barium sulfate loaded palladium catalyst, and under hydro condition, reaction temperature is 230- 320 DEG C, pressure is 1-10Mpa, is catalyzed Vegetable oil lipoprotein hydrogenation deoxidation in organic solvent, is adapted as the diesel oil of automotive fuel Component.
Chinese invention patent 102690673A discloses a kind of method of catalytic hydrocracking preparation of biodiesel with vegetable oils, The method adds catalyst, hydrophilic acidic ionic liquid and plant Shan in the reactor, is filled with hydrogen, and reaction 18h stops, Cooling, add water extraction, and stratification takes upper oil phase, obtains biodiesel.
Chinese invention patent CN102199495A discloses a kind of method of bio-oil Hydrogenation for biodiesel, the party The catalyst that method is adopted is that it is anti-to adopt bio-oil and hydrogen using CuO as active component, using single SiO2 as carrier Thing is answered, in solid-bed reactor, controlling reaction temperature is 180～260 DEG C, and 4.0～8.0MPa of reaction pressure is anti-by hydrogenation Biodiesel should be prepared.
According to above-mentioned, the biodiesel composition that oils and fatss are obtained by catalytic hydrogenation cracking there occurs fundamental change, usual To be alkane, alkene, carbonyl compound, fatty acid mixture, and the physico-chemical property of these compounds is tapped with diesel oil ten Closely, the leading indicator such as calorific capacity, viscosity, density, flash-point is attained by GB unleaded gas and the corresponding index request of light diesel fuel. As hydrogen addition technology have references to petrifaction diesel hydrogenation, mainly entered by suspension bed fluidizing reactor, fixed bed tower reactor Row production, thus bio-oil elevated oxygen level, degradable characteristic determine the unstability in hydrogenation, although by constantly Improve catalyst and improve hydrogenation efficiency, but biodiesel hydrogenation still needs high temperature, long-time and low-speed at present, causes to react Efficiency declines, to catalyst requirement also more and more higher.
Content of the invention
The defect that there is temperature height, the conversion of time length, low-speed is hydrogenated with prepared by biodiesel for preparing at present, this Bright provide a kind of preparation method of biodiesel.The method makes oil by long-neck valve homogenizer under shearing and condition of high voltage Fat is obtained with hydrogen and is moved at high speed, liquid molecular bond bursting, makes oils and fatss form reaction interface with hydrogen in continuous moving, i.e., Pre-hydrotreating reaction can be rapidly completed, further, channel outlet quick release pressure of the method by long-neck valve homogenizer makes pre- Hydrogenation thing contacts deep hydrogenation with catalyst, and product is entered rotating separation machine, biodiesel is passed through with micro side-product Rotating separation machine is separated, and is continuously reclaimed.The present invention is not only achieved and continuously prepares biodiesel, and is avoided oils and fatss and existed Reacted under high temperature for a long time, the conversion ratio of nickel under the conditions of high volume space velocity greatly improved, opened continuous, clear The new technology of clean, efficient production biodiesel, with market using value.
The present invention adopts the following technical scheme that realization：
1) oils and fatss are mixed with mass ratio 2: 0.01-0.03 with activator, is made with the stator for matching by disperseing machine rotor Relative high speed rotation, makes oils and fatss under spiral impulsive force, and gap between the stator and the rotor is subject to powerful shearing force, rubs Wipe power, make effectively emulsifying, dispersion, so that oils and fatss activation；
2) by step 1) the activation oils and fatss for obtaining and hydrogen send into long-neck valve homogenizer, under high pressure and shear action, It is 200-250cm by a length, aperture is the long-neck valve of 0.5-1mm, and hydrogen to oil volume ratio control is 100: 1-300: 1, instead Passage is answered to arrange by heating in water bath constant at 80-100 DEG C, miscible fluid is obtained and moved at high speed, and liquid molecular bond bursting makes oils and fatss Reaction interface is formed with hydrogen miscible fluid, quick in passage occur pre-hydrotreating reaction；
3) the pre- hydrogenation thing obtained by long-neck valve homogenizer is in channel outlet quick release pressure, with honeycombed catalyst Plate face is contacted, and oils and fatss carry out deep hydrogenation by the honeycombed catalyst sheet material of the micro channel that gathers under pressure, are catalyzed Agent plate arranges temperature at 120-150 DEG C, and the carrier of hydrogenation catalyst can select amorphous silicon aluminium, silicon oxide, titanium oxide, zeolite point Son sieve, γ-Al2O3, catalysis activity agent selects Ni2P、Fe、Pd、Pt、MoP、CoP；
4) hydrogenation biodiesel is reclaimed in catalyst backboard face, send into rotating separation machine, moisture, byproduct gas, hydrogen Separation use is reclaimed Deng condensation, biodiesel is continuously reclaimed after rotating separation machine is separated, and obtains biodiesel, rotating separation The rotating speed of machine is separated into standard with uniform and stable, and favor speed is 1200-1800rpm.
In above-mentioned preparation method, preparation process 1) described in activator be polycarboxylate, triethanolamine, guanidine, in quaternary ammonium base One kind.
In above-mentioned preparation method, preparation process 1) described in oils and fatss be vegetable oil, including oleum lini, soybean oil, rubber seed Oil, Oleum Ricini, Oleum Gossypii semen, Oleum Brassicae campestriss, also can select kitchen waste oil, animal oil, but need preliminary refining to process.
In above-mentioned preparation method, preparation process 2) described in long-neck valve homogenizer be continuous high pressure, high shear reaction set Standby, the operation pressure of employing is constant in 5-15MPa, and miscible flow velocity is 150-200m/S, dynamic for constant pressure by high pressure reciprocating pump Power, it is 200-250cm that oils and fatss and hydrogen miscible fluid are delivered to a length for a length, and aperture is the long-neck of 0.5-1mm Valve, material produce high pressure, intensive shear, shock and cavitation, so that liquid molecular bond during by long-neck valve Explosion, liquid reaction interface increase, and are rapidly completed pre-hydrotreating reaction.
In above-mentioned preparation method, preparation process 3) described in cellular hydrogenation catalyst plate preferably with zeolite molecular sieve, γ- Al2O3One kind be carrier, with Ni2P, Fe, Pd, Pt, MoP, CoP do the cellular sheet material of catalysis activity agent, and wherein sheet material is arranged UNICOM's micropore of densely covered 0.1-0.5mm, sheet metal thickness 50-100mm.
In above-mentioned preparation method, preparation process 4) described in rotating separation machine be a kind of separating heavy and light component whirlpool Stream rotary separator, the separator include：Top arranges condensing units, reclaims volatilization gas and part moisture evaporation point；One The individual swirl-flow devices for forming vortex；Drainage system.Which is excellent when being characterized in that mixture rotates motion opposed polarity and The mixture of density is separated into heavy constituent and light component, and light component is with nonpolar hydrogenation biodiesel, separates in eddy flow The peripheral upper strata of body, restructuring are divided into polarity glycerol and fatty acid and trace impurity, and lower floor of the separation inside eddy flow works as separator Distinguish continuous drain to discharge when reaching drainage system.
A kind of preparation method of biodiesel of the present invention, the method pass through long-neck valve homogenizer, in shearing and high-pressure section Make oils and fatss obtain with hydrogen to move under part at high speed, liquid molecular bond bursting, oils and fatss is formed in continuous moving with hydrogen anti- Answer interface, you can be rapidly completed pre-hydrotreating reaction, further, channel outlet quick release of the method by long-neck valve homogenizer Pressure, makes pre- hydrogenation thing contact deep hydrogenation with catalyst, and product enters rotating separation machine, makes biodiesel with micro pair Product is separated by rotating separation machine, and is continuously reclaimed.Avoid and under high-temperature and high-pressure conditions, be easily caused biodiesel coking drop The defect of solution, the response time is short, nickel efficiency greatly improved under the conditions of high volume space velocity, reduces wanting catalyst Ask.
A kind of preparation method of biodiesel proposed by the present invention, opens continuous, cleaning, highly effective hydrogenation production biology The new technology of matter diesel oil, technical process non-wastewater discharge；Volume space velocity 13h-1Under the conditions of conversion rate of products reach more than 97%, raw The acid number of thing diesel oil is fully achieved the standard of national biodiesel 6B/T20828-2007 less than 0.3mgKOH/g.
The characteristics of a kind of preparation method of biodiesel of the present invention, its protrusion and beneficial effect are：
1st, the preparation method of a kind of biodiesel of the invention, by shearing and the high pressure of long-neck valve homogenizer, makes oils and fatss Motion at high speed is obtained with hydrogen miscible fluid, liquid molecular bond bursting, oils and fatss form reaction interface with hydrogen in continuous moving, i.e., Pre-hydrotreating reaction can be rapidly completed, further, channel outlet quick release pressure of the method by long-neck valve homogenizer makes pre- Hydrogenation thing contact deep hydrogenation with catalyst, it is to avoid is hydrogenated with the conditions of high temperature, high pressure, long-time and is easily caused biodiesel Jiao Change the defect of degraded, nickel conversion ratio reaches more than 97% under the conditions of high volume space velocity.
2nd, the preparation method of a kind of biodiesel of the invention, makes mixture rotate motion using vortex fluid, no The hydrogenation biodiesel of same polarity and density and side-product sharp separation, continuous drain are not only realized being continuously separated, and are separated Purity is high, steady quality.
3rd, the preparation method of a kind of biodiesel of the invention, opens continuous, cleaning, efficiently produces the new of biodiesel Technique, technical process non-wastewater discharge, is suitable for large-scale production.
Description of the drawings
Fig. 1 is that a kind of long-neck valve homogenizer continuously hydrogen adding adopted by the preparation method of biodiesel of the invention is illustrated Figure.
Accompanying drawing 1 is numbered：1. oils and fatss and 2. long-neck valve of hydrogen, 3. honeycombed catalyst plate
Fig. 2 is that a kind of rotating vortex adopted by the preparation method of biodiesel of the invention separates schematic diagram.
Accompanying drawing 2 is numbered：1. moisture, 2. by-product of volatile matters gas-collecting pipe and 3. by-product of impurity and drainage tube
4. hydrogenation biodiesel 5. is hydrogenated with biodiesel drainage tube
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail, but this should not be interpreted as the present invention Scope be only limitted to Examples below.In the case of without departing from said method thought of the present invention, according to ordinary skill Various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
1) Oleum Gossypii semen is mixed with mass ratio 2: 0.02 with activator polycarboxylic acids sodium, by dispersion machine Forced Dispersion, in spiral shell Under rotation impulsive force, gap between the stator and the rotor is subject to powerful shearing force, frictional force, makes effectively emulsifying, dispersion, from And activate oils and fatss；
2) by step 1) to send into length be 250cm for the activation oils and fatss that obtain and hydrogen, long-neck valve homogenizing of the aperture for 0.8mm Machine, the pressure of employing are constant in 5MPa, and slurry flow velocity is 200m/S, and reaction channel is arranged constant in 80-100 by heating in water bath DEG C, miscible fluid obtains at high speed motion, and liquid molecular bond bursting makes miscible fluid quickly form reaction interface, occur in passage with Hydrogenation reaction；
3) the pre- hydrogenation thing obtained by long-neck valve homogenizer is in channel outlet quick release pressure, with honeycombed catalyst Plate face contact carry out deep hydrogenation, catalyst plates with zeolite molecular sieve as carrier, with Ni2P does the Cellular board of catalysis activity agent Material, wherein sheet material arrange the linked hole of 0.1mm, sheet metal thickness 100mm, and catalyst plates arrange temperature at 130 DEG C.
4) hydrogenation biodiesel is reclaimed in catalyst backboard face, send into rotating separation machine, moisture, byproduct gas, hydrogen Separation use is reclaimed Deng condensation, biodiesel is continuously reclaimed after rotating separation machine is separated, and obtains biodiesel, rotating separation The rotating speed of machine is 1200rpm.
By test, 1 oils and fatss of embodiment are in volume space velocity 13h-1Under the conditions of biodiesel hydrogenation conversion be 97%, obtain To biodiesel performance indications be fully achieved standard GB/T/T20828-2007《Diesel fuel reconciles with biological bavin Oil》Key index, specific targets are as follows：
Embodiment 2
1) kitchen waste oil is mixed with mass ratio 2: 0.01-0.02 with activator triethanolamine, forces to divide by dispersion machine Dissipate and form activation oils and fatss；
2) by step 1) the activation oils and fatss for obtaining and hydrogen send into long-neck valve homogenizer, under high pressure and shear action, By a length be 200cm, aperture for 1mm long-neck valve, reaction channel arranged by heating in water bath constant at 80-100 DEG C, Miscible fluid obtains motion, liquid molecular bond bursting at high speed, makes oils and fatss quickly form reaction interface with hydrogen miscible fluid, in passage Generation pre-hydrotreating reaction；
3) the pre- hydrogenation thing obtained by long-neck valve homogenizer is in channel outlet quick release pressure, with honeycombed catalyst Plate face contact carries out deep hydrogenation, catalyst plates with titanium oxide as carrier, with the cellular sheet material that Fe does catalysis activity agent, wherein Sheet material arranges the linked hole of 0.5mm, sheet metal thickness 50mm, and catalyst plates arrange temperature at 150 DEG C.
4) hydrogenation biodiesel is reclaimed in catalyst backboard face, send into rotating separation machine, moisture, byproduct gas, hydrogen Separation use is reclaimed Deng condensation, biodiesel is continuously reclaimed after rotating separation machine is separated, and obtains biodiesel, rotating separation The rotating speed of machine is 1800rpm.
By test, the biodiesel that embodiment 2 is obtained is in volume space velocity 14h-1Under the conditions of biodiesel hydrogenation turn Rate is 98%, and performance indications are fully achieved standard GB/T/T20828-2007《Diesel fuel mediation biodiesel》Close Key index, specific targets are as follows：
Embodiment 3
1) soybean oil is mixed with mass ratio 2: 0.01 with activator guanidine, activation oil is formed by dispersion machine Forced Dispersion Fat；
2) by step 1) the activation oils and fatss for obtaining and hydrogen send into long-neck valve homogenizer, under high pressure and shear action, It is 200cm by a length, aperture is the long-neck valve of 0.5mm, and reaction channel is arranged constant in 80-100 by heating in water bath DEG C, miscible fluid obtains motion, liquid molecular bond bursting at high speed, makes oils and fatss quickly form reaction interface with hydrogen miscible fluid, logical There is pre-hydrotreating reaction in road；
3) the pre- hydrogenation thing obtained by long-neck valve homogenizer is in channel outlet quick release pressure, with honeycombed catalyst Plate face contact carry out deep hydrogenation, catalyst plates with zeolite molecular sieve as carrier, with the cellular sheet material that Pd does catalysis activity agent, Wherein sheet material arranges the linked hole of 0.3mm, sheet metal thickness 60mm.Catalyst plates arrange temperature at 120 DEG C.
4) hydrogenation biodiesel is reclaimed in catalyst backboard face, send into rotating separation machine, moisture, byproduct gas, hydrogen Separation use is reclaimed Deng condensation, biodiesel is continuously reclaimed after rotating separation machine is separated, and obtains biodiesel, rotating separation The rotating speed of machine is 1300rpm.
By test, embodiment 3 is in volume space velocity 15h-1Under the conditions of biodiesel hydrogenation conversion be 97%, obtain Biodiesel performance indications are fully achieved standard GB/T/T20828-2007《Diesel fuel mediation biodiesel》Close Key index, specific targets are as follows：
Embodiment 4
1) rubber seed oil is mixed with mass ratio 2: 0.03 with activator quaternary ammonium base, work is formed by dispersion machine Forced Dispersion Carburetion fat；
2) by step 1) the activation oils and fatss for obtaining and hydrogen send into long-neck valve homogenizer, under high pressure and shear action, It is 220cm by a length, aperture is the long-neck valve of 0.8mm, and reaction channel is arranged constant in 80-100 by heating in water bath DEG C, miscible fluid obtains motion, liquid molecular bond bursting at high speed, makes oils and fatss quickly form reaction interface with hydrogen miscible fluid, logical There is pre-hydrotreating reaction in road；
3) the pre- hydrogenation thing obtained by long-neck valve homogenizer is in channel outlet quick release pressure, with honeycombed catalyst Plate face contact carry out deep hydrogenation, catalyst plates with zeolite molecular sieve as carrier, with the cellular sheet material that Pt does catalysis activity agent, Wherein sheet material arranges the linked hole of 0.4mm, sheet metal thickness 100mm.Catalyst plates arrange temperature at 140 DEG C.
4) hydrogenation biodiesel is reclaimed in catalyst backboard face, send into rotating separation machine, moisture, byproduct gas, hydrogen Separation use is reclaimed Deng condensation, biodiesel is continuously reclaimed after rotating separation machine is separated, and obtains biodiesel, rotating separation The rotating speed of machine is 1500rpm.
Embodiment 5
1) oleum lini is mixed with mass ratio 2: 0.01 with activator polycarboxylic acids amine, work is formed by dispersion machine Forced Dispersion Carburetion fat；
2) by step 1) the activation oils and fatss for obtaining and hydrogen send into long-neck valve homogenizer, under high pressure and shear action, By a length be 250cm, aperture for 1mm long-neck valve, reaction channel arranged by heating in water bath constant at 80-100 DEG C, Miscible fluid obtains motion, liquid molecular bond bursting at high speed, makes oils and fatss quickly form reaction interface with hydrogen miscible fluid, in passage Generation pre-hydrotreating reaction；
3) the pre- hydrogenation thing obtained by long-neck valve homogenizer is in channel outlet quick release pressure, with honeycombed catalyst Plate face contact carries out deep hydrogenation, and catalyst plates are with γ-Al2O3For carrier, with the cellular sheet material that CoP does catalysis activity agent, its Middle sheet material arranges the linked hole of 0.2mm, sheet metal thickness 80mm.Catalyst plates arrange temperature at 120 DEG C.
4) hydrogenation biodiesel is reclaimed in catalyst backboard face, send into rotating separation machine, moisture, byproduct gas, hydrogen Separation use is reclaimed Deng condensation, biodiesel is continuously reclaimed after rotating separation machine is separated, and obtains biodiesel, rotating separation The rotating speed of machine is 1800rpm.

Claims (6)

1. a kind of preparation method of biodiesel, is characterized in that shearing and the high pressure by long-neck valve homogenizer, make oils and fatss with Hydrogen miscible fluid is obtained and is moved at high speed, liquid molecular bond bursting, is rapidly completed pre-hydrotreating reaction, and is passed through long-neck valve homogenizer Channel outlet quick release pressure, make pre- hydrogenation thing contact deep hydrogenation with catalyst, realize continuously hydrogen adding preparation biomass Diesel oil, concrete preparation method are as follows：
1) oils and fatss are mixed with mass ratio 2: 0.01-0.03 with activator, by disperseing machine rotor relative with the stator work for matching High speed rotation, make oils and fatss under spiral impulsive force, gap between the stator and the rotor is subject to powerful shearing force, friction Power, effectively emulsifying, dispersion is made, so that oils and fatss activation；
2) by step 1) the activation oils and fatss that obtain send into long-neck valve homogenizer with hydrogen, under high pressure and shear action, by one Individual length is 200-250cm, and aperture is the long-neck valve of 0.5-1mm, and hydrogen to oil volume ratio control is 100: 1-300: 1, reaction channel Arranged constant at 80-100 DEG C by heating in water bath, miscible fluid obtains motion at high speed, and liquid molecular bond bursting makes oils and fatss and hydrogen Miscible fluid forms reaction interface, and pre-hydrotreating reaction occurs in passage；
3) the pre- hydrogenation thing obtained by long-neck valve homogenizer is in channel outlet quick release pressure, with honeycombed catalyst plate face Contact carries out deep hydrogenation, and catalyst plates arrange temperature at 120-150 DEG C, the carrier of hydrogenation catalyst from amorphous silicon aluminium, Silicon oxide, titanium oxide, zeolite molecular sieve, γ-Al2O3, catalysis activity agent selects Ni2P、Fe、Pd、Pt、MoP、CoP；
4) hydrogenation biodiesel is reclaimed in catalyst backboard face, send into rotating separation machine, including moisture, byproduct gas, hydrogen Reclaim to separate in interior component condensation and use, hydrogenation biodiesel is continuously reclaimed after rotating separation machine is separated, and obtains biology Matter diesel oil, the rotating speed of rotating separation machine is 1200-1800rpm.
2. a kind of preparation method of biodiesel according to claim 1, is characterized in that：Preparation process 1) described in oil Fat is oleum lini, soybean oil, rubber seed oil, Oleum Ricini, Oleum Gossypii semen, Oleum Brassicae campestriss, the kitchen waste oil of preliminary refining process or pre- essence The animal oil that refining is processed.
3. a kind of preparation method of biodiesel according to claim 1, is characterized in that：Preparation process 1) described in work Agent is polycarboxylate, triethanolamine, guanidine, the one kind in quaternary ammonium base, and described dispersion machine is made with the stator for matching by rotor Relative high speed rotation, makes oils and fatss under spiral impulsive force, and gap between the stator and the rotor is subject to powerful shearing force, rubs Wipe power, make effectively emulsifying, dispersion, so that oils and fatss activation.
4. a kind of preparation method of biodiesel according to claim 1, is characterized in that：Preparation process 2) described in length Neck valve homogenizer is continuous high pressure, high shear consersion unit, and the operation pressure of employing is constant in 5-15MPa, miscible flow velocity For 150-200m/S, it is constant-voltage power by high pressure reciprocating pump, oils and fatss and hydrogen miscible fluid is delivered to a length for 200- 250cm, long-neck valve of the aperture for 0.5-1mm, material by during long-neck valve, produce high pressure, intensive shear, shock and Cavitation, so that liquid molecular bond bursting, the increase of liquid reaction interface, are rapidly completed pre-hydrotreating reaction.
5. a kind of preparation method of biodiesel according to claim 1, is characterized in that：Preparation process 3) described in honeybee Nest shape catalyst plates are with zeolite molecular sieve, γ-Al2O3One kind be carrier, with Ni2P, Fe, Pd, Pt, MoP, CoP make catalysis and live Property agent cellular sheet material, wherein sheet material arrange gather 0.1-0.5mm linked hole, sheet metal thickness 50-100mm.
6. a kind of preparation method of biodiesel according to claim 1, is characterized in that：Preparation process 4) described in rotation Turn the vortex rotary separator that seperator is a kind of separating heavy and light component, the separator includes：Top arranges condensation Device, reclaims volatilization gas and part moisture evaporation point；One swirl-flow devices that can form vortex；Drainage system；Which is excellent When being characterized in that mixture rotates motion, the mixture of opposed polarity and density is separated into heavy constituent and light component, and light component is There is nonpolar hydrogenation biodiesel, separate on the peripheral upper strata of rotary fluid, recombinate and be divided into polarity glycerol and fatty acid and micro- Amount impurity, lower floor of the separation inside eddy flow distinguishes continuous drain and discharges when separator reaches drainage system.
CN201410374922.9A 2014-08-01 2014-08-01 A kind of preparation method of biodiesel Expired - Fee Related CN104194949B (en)

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