CN104194945B - A kind of method of utilization screw mechanism for biodiesel - Google Patents
A kind of method of utilization screw mechanism for biodiesel Download PDFInfo
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- CN104194945B CN104194945B CN201410374933.7A CN201410374933A CN104194945B CN 104194945 B CN104194945 B CN 104194945B CN 201410374933 A CN201410374933 A CN 201410374933A CN 104194945 B CN104194945 B CN 104194945B
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Abstract
A kind of method of the utilization screw mechanism of the present invention for biodiesel.It is with animal and plant fat as primary raw material, using two steps type double screw extruder as flow reactor, using its continuous dispersion, shearing, constant pressure stream, backflow, devolatilization, the function of conveying, by two stage structures, when realizing that biodiesel is continuously produced, a step completes catalytic hydrogenation, isomery and dehydration, degassing.The method is used as reactor by two steps type twin screw, the threaded block combination of screw machine can make oils and fatss, in different phase, different reactions occur, shearing dispersion is carried out in the first rank, under strong shear, make oils and fatss, with hydrogen, catalytic hydrogenation quickly occur, liquid air speed and reaction efficiency is improved, and the continuous isomerization of high-temperature constant pressure is carried out in second-order and devolatilization is processed.Traditional reactor is different from, the invention belongs to the pusher reaction of continuous dynamic, under the conditions of screw rod lateral shear and radial pressure, produce high temperature and high pressure at short notice, be rapidly completed catalytic hydrogenation and isomerization, not only reaction efficiency is high, and the quality of biodiesel is high, steady quality.
Description
Technical field
The present invention relates to field of biodiesel oil, and in particular to a kind of method of utilization screw mechanism for biodiesel.
Background technology
It is esterified by the main component triglyceride by vegetable oil or animal grease or ester exchange reaction is changed into long-chain
Fatty-acid monoester, is the main path for producing biodiesel at present.As biodiesel raw material can regenerate, show good
The feature of environmental protection and sustainability, become the good succedaneum of diesel oil.Biodiesel is greatly developed to sustainable economic development, energy is advanced
Source substitutes, and mitigates ambient pressure, and control urban atmospheric pollution has important strategic importance.Therefore, the research of biodiesel and
Application develop in recent years quite rapid.
The primary raw material of biodiesel is animal and plant fat, can carry out ester exchange reaction by oils and fatss and lower 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, but invests and operating cost height, and technology stability is poor, it is difficult to control；Biological enzyme is anti-
Answer mild condition, non-pollutant discharge and without the need for washing, but catalyzing enzyme high expensive, and react slow, efficiency is low.
Further, since the ester exchange reaction of glyceride and lower alcohol is reversible reaction, the conversion ratio of oils and fatss is flat by thermodynamics
Weighing apparatus is limited, and with the raising of oils and fatss conversion ratio, the cost of unit conversion rate is continuously increased, and unstable due to glyceride stock
The content of factor, unconverted oils and fatss and all kinds of intermediate products affects the quality of final biodiesel.For example, European standard
EN14214 is required to the standard of biodiesel：Mono fatty acid glyceride, difatty acid glyceride and triglyceride exist
Mass concentration in product should be respectively smaller than 0.8%, 0.2% and 0.2%, and in actual production, mono fatty acid glyceride
Mass concentration is higher than then 3%.If by adding enough catalyst or extending response time raising conversion ratio, can cause to increase
Plus side-product even results in the biodiesel degraded for having converted.Therefore, efficient, steady quality, highly purified biodiesel are converted
Become development production of biodiesel at present and the Main way for using.
The method that Chinese invention patent CN1141993C discloses Acrawax under super critical condition, the method do not make
With catalyst, relatively low to glyceride stock requirement, the response time is short, and technique simplifies, but the technological reaction condition is harsh, pressure
Greatly, reaction temperature height (350-400 DEG C), stability is poor.
Chinese invention patent 101550349 discloses a kind of method of use preparing biodiesel by supercritical technology, the method
The appropriate mol ratio of oils and fatss and methanol by acidified for various oils and fatss eliminating water, esterification, after through process becomes equal under supercritical
Phase, carries out ester exchange reaction, and control pressure is 8-40MPA, temperature 300-450 DEG C.The invention shortens bio-oil conversion life
The pollution of the time of thing diesel oil, alkali-free or acid catalyst.But as the method for preparing biodiesel under supercritical condition is needed in high temperature height
Carry out under the conditions of pressure, cause higher producing cost and energy expenditure, and belong to batch production, technology stability is poor, especially
Which is that high temperature is easily caused biodiesel coking.
Chinese invention patent 1916114 discloses a kind of continuous, homogeneous method for preparing biodiesel, and the method will be natural
Oils and fatss etc. and methanol and alkali metal hydroxide and mixed liquor can be made to form homogeneous organic solvent mix jointly, form homogeneous body
System, sending into pipeline reactor carries out continuous esterification preparation biodiesel.The method enables oils and fatss fully to dissolve each other with methanol,
Reaction rate is accelerated, shortens the response time, but due to adopting alkali metal hydroxide as catalyst, therefore, rotten to equipment
Erosion is serious, and base catalyst loss is big, there is pollution.
102492560 B of Chinese invention patent CN disclose a kind of device of distribution type plant oil transesterification production and life
The method of product, the method are by vegetable oil lipid raw oil, low-carbon alcohols and pyridine trifluoromethyl sulfonic acid ionic-liquid catalyst
Mixture in reactor heated and stirred, react 3-5 hours；It is biphase that standing and reacting material is divided into weight, and separation is biphase.The method
Catalyst is the use of, and the response time is also longer.
The biodiesel prepared by ester exchange, due to the saturation difference of raw materials used middle carbochain, the fat that produces
Also there is a problem of in actual applications that fatty acid methyl esters self property determines is certain：Such as low temperature flow is poor, condensation, cold filter plugging point
Higher, it is impossible in very cold area and use in winter；In molecular structure, functional group containing aerobic causes calorific value relatively low；Viscosity compared with
Height, difficulty of transportation in diesel oil；Density is higher；Poor storage stability, is susceptible to oxidation deterioration etc..Especially this kind of biological bavin
In oil, oxygen content is high, it is difficult to reconciles with petrifaction diesel and uses.In addition, preparation of biodiesel is mainly using stirring still reaction
Device, pipeline reactor are reacted, and the process has that response time length, consumption of raw materials are big, mixing plant power consumption is big, must be through multiple
The problems such as repeating Exchange Ester Process to improve conversion ratio；In order to further improve reaction efficiency, generally adopt plus catalyst, use
Excessive short chain alcohol, reactor using High Temperature High Pressure or strengthen stirring intensity, or even adopt supercritical process.But due to biology
The glyceride stock composition of diesel oil is complex, containing satisfied fatty acid and unsaturated fatty acid, is higher fatty acid fat
Complex compound, therefore the quality stability of glyceride stock is poor, containing various polarity pairs such as glycerol in the biodiesel of preparation
Product, adds catalyst and excessive methanol etc., further results in the complexity of product, ultimately results in oils and fatss conversion reaction efficiency
Low, quality is unstable, biodiesel purity is low.
In order to further make biodiesel performance be close to petrifaction diesel performance, by the second filial generation of hydrogenation catalyst cracking process
Biodiesel makes the performance of biodiesel there occurs basic change.Compared with preparing biodiesel by ester interchange, hydrogenation catalyst
The biodiesel composition of cracking there occurs fundamental change, and generally yielded is the mixture of alkane, alkene, its physico-chemical property and bavin
Oil is sufficiently close to, and the leading indicator such as calorific capacity, viscosity, density, flash-point, boiling range is attained by the corresponding index of GB light diesel fuel will
Ask, so as to raise the fuel oil of high-quality, its fuel performance is even more than conventional petrifaction diesel.
Chinese invention patent CN101463272 discloses a kind of method that bio oil hydrotreating produces diesel oil, the method
Exist with the conditions of hydrotreating reaction in hydrogen, biological grease contacted with catalyst, employ the higher catalyst of activity,
Can carry out at a temperature of relatively low hydrotreating reaction, can enter under 400 DEG C of reaction conditions of temperature in air speed 5h-1, pressure 5MPa
Row hydrogenation.
Chinese invention patent CN102876348A discloses a kind of method of Hydrogenation for biodiesel, and the method will be hydrogenated with
Refined effluent is sent into the gas-liquid separator above hydro dewaxing reactor and carries out gas-liquid separation；The refined oil that isolates is again through tower
After plate redistribution, with hydrogen adverse current by Hydrodewaxing catalyst bed, separate pour point depression generation oil and obtain biodiesel oil product,
The features such as biodiesel of production has high cetane number, low sulfur content and low condensation point.
Above-mentioned main employing fixed bed reactors, tank reactor or fluidized-bed reactor, not only equipment investment is big, and
Raw material needs pretreatment, as glyceride stock is high acid value oils and fatss or waste animal and vegetable oil, catalyst to oils and fatss in miscellaneous
Matter is extremely sensitive, easily aging, is typically only capable in relatively low air speed (5h-1Below) or higher reaction temperature (more than 300 DEG C)
Carry out, reaction efficiency is low, the hydrogenation for being even above petrifaction diesel is required to the respond of hydrogenation plant, so as to limit hydrogenation
The production of catalytic pyrolysiss biodiesel.
Content of the invention
Biodiesel is prepared for the cracking of current hydrogenation catalyst and there is low-speed reaction, reaction temperature height, reaction efficiency
The easily aging defect of low, catalyst, the present invention provide a kind of method of utilization screw mechanism for biodiesel.The method is using double
Stepwise double screw extruder makes oils and fatss disposably complete catalytic hydrogenation, isomery and dehydration, degassing, using double as reactor
The mechanical shearing of screw machine, reduces reaction temperature, improves the reaction efficiency under the conditions of high volume space velocity, resists catalyst
Aging is improved, and the biodiesel Cetane number for obtaining is high, steady quality, and strong adaptability can be with petrifaction diesel with arbitrary proportion
Reconcile and use.Avoid pollution of the acid base catalysator to environment, it is achieved that clean manufacturing biodiesel.
A kind of method of the utilization screw mechanism of the present invention for biodiesel, is with animal and plant fat as primary raw material, with double
Stepwise dual-screw-stem machine, leads to using its continuous dispersion, shearing, constant pressure stream, backflow, devolatilization, the function of conveying as flow reactor
Two stage structures are crossed, a step completes catalytic hydrogenation, isomery and dehydration, degassing when realizing that biodiesel is continuously produced.The method is led to
Two steps type double-screw reactor is crossed, the threaded block combination of screw machine can make oils and fatss, in different phase, different reactions occur,
First rank carries out shearing dispersion, makes oils and fatss, with hydrogen, catalytic hydrogenation quickly occur, improve in high volume space velocity under strong shear
Under the conditions of reaction efficiency, carry out the continuous isomery of high-temperature constant pressure and devolatilization in second-order and process, different from traditional reaction
Kettle, the invention belongs to the pusher reaction of continuous dynamic, under the conditions of screw rod lateral shear and radial pressure, is produced at short notice
High temperature and high pressure, is rapidly completed catalytic hydrogenation and isomery, and not only reaction efficiency is high, and the quality of biodiesel is high, and quality is steady
Fixed.
The present invention adopts the following technical scheme that realization：
1) oils and fatss are injected the first rank of warmed-up two steps type dual-screw-stem machine, the temperature setting of each conversion zone is followed successively by
80-100 DEG C, 100-120 DEG C, 100-110 DEG C, 100-90 DEG C, 90-80 DEG C, the first rank screw rod head pressure is 0.5-2MPa, main
Machine rotating speed is 200-300 rev/min, arranges vacuum volatilization, exclude the moisture in oils and fatss, three, four between second and third section is heated
Hydrogen pump is set between Duan Jiare, pumps into hydrogen, head arranges hydrogenation catalyst porous plate, by the dispersion of the first rank screw machine and
Constant pressure, under Hydrogen Vapor Pressure and screw rod constant-pressure conditions, due to the miscible fluid of hydrogen uniformly through the catalysis for being covered with micro channel
Agent porous plate, makes oils and fatss form homogeneous reaction interface with hydrogen, and quick catalysis are hydrogenated with, and continuous rotational shear screw rod was both provided
Stable reaction condition, while passing through to arrange temperature, Devolatilization device, catalytic porous plate in diverse location, realizes continuous-stable
Hydrogenation；
2) by the second-order for entering two steps type dual-screw-stem machine after the first rank screw rod catalytic hydrogenation, the temperature setting of each conversion zone
100-120 DEG C, 120-130 DEG C, 120-100 DEG C, 110-80 DEG C, 100-80 DEG C is followed successively by, second-order screw rod head pressure is 2-
5MPa, engine speed are 50-100 rev/min, arrange vacuum volatilization, by the gas of vacuum volatilization between the nine, the ten sections of heating
Separate after being collected and use, head arranges heterogeneous catalyst porous plate, in second-order screw rod lateral shear and radial pressure condition
Under, the biodiesel of n-alkane forms isomerized alkyl by heterogeneous catalyst porous plate, so as to improve the low of biodiesel
Warm mobility；
3) by step 2) product that obtains through polyethylene glycol fiber films filter membrane, by polyethylene glycol fiber films to micro-
Amount impurity absorption is filtered, and obtains high-purity biodiesel.
In above-mentioned preparation method, preparation process 1), step 2) described in two steps type dual-screw-stem machine engaged for two steps type in the same direction
Or incorgruous extruding machine with two screw rods engaging, be a kind of flow reactor advanced by rotational shear, be made up of two ranks, the first rank with
The composition of second-order can be respectively：Engagement is extruded with meshed double screw in the same direction, is engaged and incorgruous meshed double screw in the same direction in the same direction
Extrusion, incorgruous engagement are extruded with meshed double screw in the same direction with incorgruous meshed double screw extrusion, incorgruous engagement, wherein the first rank screw rod
Draw ratio >=25, preferably screw diameter 35-65mm, arrange and there is shearing, dispersion, the threaded block of conveying；Second-order screw rod major diameter
Than >=40, preferred screw diameter 45-75mm is arranged and be there is shearing, engagement, backflow, the threaded block of conveying, and the threaded block that flows back sets
Put to guarantee the time of staying of the reaction mass in screw rod in 10-15 minutes, by two stage structures, it is possible to achieve biodiesel connects
During continuous production, one step completes catalytic hydrogenation, isomerization.
In above-mentioned preparation method, preparation process 1), step 2) described in the preferably double ranks of two steps type dual-screw-stem machine be in the same direction
The double screw extruder of engagement.
In above-mentioned preparation method, preparation process 1) described in oils and fatss its main components for triglyceride animals and plants
The oils and fatss of oils and fatss, preferably C12-C16, the acid value of oils and fatss can be within 120mgKOH/g, with wider adaptability.
In above-mentioned preparation method, preparation process 1) described in hydrogen pump-in pressure be 0.5-1MPa.
In above-mentioned preparation method, preparation process 1) described in hydrogenation catalyst porous plate be tungsten, nickel, cobalt, molybdenum, copper oxidation
Thing or phosphide are supported on the porous sheet material of Bauxite Sintering, and wherein aperture is 0.1-0.5mm.
In above-mentioned preparation method, preparation process 1) described in two steps type dual-screw-stem machine arrange between second and third section is heated true
Empty devolatilization, devolatilization vacuum pressure are 0.6-0.8MPa.
In above-mentioned preparation method, preparation process 2) described in heterogeneous catalyst porous plate be Metal Palladium, zirconium, thorium, niobium load
In the porous sheet material that basalt, pyrophillite are sintered, wherein aperture is 0.1-0.5mm.
In above-mentioned preparation method, preparation process 2) described in two steps type dual-screw-stem machine arrange between the nine, the ten sections of heating true
Empty devolatilization, devolatilization vacuum pressure are 1.0-1.5MPa.
In above-mentioned preparation method, preparation process 3) described in polyethylene glycol fiber films fibre gap be 0.05-0.1 μm,
It is 0.2-0.5MPa to arrange mould difference during Purification by filtration, and the extremely strong polar character of polyethylene glycol fiber films is micro- with biodiesel
The impurity of amount has strong adsorption interconnection function, so as to obtaining high-purity biodiesel.
A kind of method of the utilization screw mechanism of the present invention for biodiesel, is with animal and plant fat as primary raw material, with double
Stepwise dual-screw-stem machine, leads to using its continuous dispersion, shearing, constant pressure stream, backflow, devolatilization, the function of conveying as flow reactor
Two stage structures are crossed, a step completes catalytic hydrogenation, isomery and dehydration, degassing when realizing that biodiesel is continuously produced.The method is led to
Two steps type double-screw reactor is crossed, the threaded block combination of screw machine can make oils and fatss, in different phase, different reactions occur,
First rank carries out shearing dispersion, makes oils and fatss, with hydrogen, catalytic hydrogenation quickly occur, carry out high temperature in second-order under strong shear
Continuous isomery under constant pressure and devolatilization are processed, different from traditional reactor, the invention belongs to the pusher reaction of continuous dynamic,
Under the conditions of screw rod lateral shear and radial pressure, produce high temperature and high pressure at short notice, be rapidly completed catalytic hydrogenation and isomery.
Using the mechanical shearing of screw machine, reaction temperature is reduced, improve the reaction efficiency under the conditions of high volume space velocity, make catalysis
Agent ageing resistance is improved, and the biodiesel Cetane number for obtaining is high, steady quality, and strong adaptability can be with petrifaction diesel with any
Ratio reconciles and uses.Avoid pollution of the acid base catalysator to environment, it is achieved that clean manufacturing biodiesel.
At 80-130 DEG C, volume space velocity 8-12h-1Under the conditions of, hydrogenation of net product conversion ratio reaches more than 96%, and Cetane number surpasses
95% is crossed, the standard of national biodiesel GB/T20828-2007 is fully achieved.
The characteristics of a kind of method of the utilization screw mechanism of the present invention for biodiesel, its protrusion and beneficial effect are：
1st, method of a kind of utilization screw mechanism of the invention for biodiesel, the method adopt two steps type twin-screw extrusion
Machine, makes oils and fatss disposably complete catalytic hydrogenation, isomery and dehydration, degassing, using the mechanical shearing of screw machine, reduces anti-
Temperature is answered, air speed and reaction efficiency is improve, improves catalyst ageing resistance, the biodiesel Cetane number for obtaining is high, matter
Amount is stable.Avoid pollution of the acid base catalysator to environment, it is achieved that clean manufacturing biodiesel.
2nd, method of a kind of utilization screw mechanism of the invention for biodiesel, in screw rod lateral shear and radial pressure condition
Under, oils and fatss are increased with hydrogen interface at short notice, are rapidly completed hydrogenation, and air speed is high, reaction temperature is low, reaction efficiency is high, urge
Agent life-span length.
3rd, method of a kind of utilization screw mechanism of the invention for biodiesel, the low temperature stream that biodiesel is improved by isomery
Dynamic property, strong adaptability can be reconciled with arbitrary proportion with petrifaction diesel and be used.
4th, method of a kind of utilization screw mechanism of the invention for biodiesel, belongs to the pusher reaction of continuous dynamic, biological
Diesel quality is stable, technique is easily controllable, it is to avoid is difficult to control to the defect of technique in reactor intermittent reaction, is suitable for
Large, medium and small type large-scale production.
Description of the drawings
Fig. 1 is a kind of utilization screw mechanism of the invention to be illustrated for the equipment that adopted of method of biodiesel and technological process
Figure.
Accompanying drawing 1 is numbered：
1. 3. 3 sections 4. 4 sections 5. 5 sections of one section of 2. two-stage nitration
6. 7. first rank screw rod of vacuum volatilization 8. is hydrogenated with 10. 6 sections of 9. hydrogenation catalyst plate of pump
11. 7 sections of 12. 8 sections of 13. 9 sections of 14. ten sections of 15. vacuum volatilizations
16. isocatalysis plate, 17. second-order screw rod, 18. filter membrane
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) the first rank that Oleum Brassicae campestriss inject warmed-up two steps type dual-screw-stem machine is engaged in the same direction, screw slenderness ratio 30, spiral shell
Shank diameter 35mm, the temperature setting of each conversion zone are followed successively by 80-100 DEG C, 100-120 DEG C, 100-110 DEG C, 100-90 DEG C, 90-
80 DEG C, the first rank screw rod head pressure is 1MPa, and engine speed is 200 revs/min, between second and third section is heated arranges vacuum
Devolatilization, excludes the moisture in oils and fatss, between three, four sections of heating arranges hydrogen pump, pumps into hydrogen, and head arranges tungsten oxide and is supported on
The porous sheet material of Bauxite Sintering, by dispersion and the constant pressure of the first rank screw machine, makes oils and fatss be formed with hydrogen homogeneous
Reaction interface, quick catalysis are hydrogenated with；
2) engaged by the second-order for entering two steps type screw machine after the first rank screw rod catalytic hydrogenation in the same direction, screw slenderness ratio
40, screw diameter 45mm, the temperature setting of each conversion zone are followed successively by 100-120 DEG C, 120-130 DEG C, 120-100 DEG C, 110-80
DEG C, 100-80 DEG C, second-order screw rod head pressure be 5MPa, engine speed be 100 revs/min, the nine, the ten sections heating between set
Vacuum volatilization is put, head arranges the porous sheet material that palladium is supported on basalt sintering, in second-order screw rod lateral shear and footpath
To under pressure condition, the biodiesel isomerization of n-alkane in the very short time, so that improve the low temperature flow of biodiesel
Property, separate after being collected by the gas of vacuum volatilization and use；
3) using step 2) product that obtains through polyethylene glycol fiber films as filter membrane, by polyethylene glycol fiber films
To trace impurity adsorption filtration, high-purity biodiesel is obtained.
By test, 1 oils and fatss of embodiment are in liquid volume air speed 8h-1Under the conditions of to biodiesel hydrogenation conversion be 98%
More than, the biodiesel performance indications for obtaining are fully achieved standard GB/T/T20828-2007《Diesel fuel reconciles to be used
Biodiesel》Key index, specific targets are as follows：
Embodiment 2
1) the first rank that soybean oil injects warmed-up two steps type dual-screw-stem machine is engaged in the same direction, screw slenderness ratio 25, spiral shell
Shank diameter 40mm, the temperature setting of each conversion zone are followed successively by 80-100 DEG C, 100-120 DEG C, 100-110 DEG C, 100-90 DEG C, 90-
80 DEG C, the first rank screw rod head pressure is 2MPa, and engine speed is 28 revs/min, arranges vacuum and take off between second and third section is heated
Wave, exclude the moisture in oils and fatss, hydrogen pump is set between three, four sections of heating, pump into hydrogen, head arranges nickel phosphide and is supported on aluminum
The porous sheet material of Tu Kuang sintering, by dispersion and the constant pressure of the first rank screw machine, forms oils and fatss and hydrogen homogeneous anti-
Interface, quick catalysis is answered to be hydrogenated with；
2) by the incorgruous engagement of the second-order for entering two steps type dual-screw-stem machine after the first rank screw rod catalytic hydrogenation, screw slenderness ratio
52, screw diameter 55mm, the temperature setting of each conversion zone are followed successively by 100-120 DEG C, 120-130 DEG C, 120-100 DEG C, 110-80
DEG C, 100-80 DEG C, second-order screw rod head pressure be 3MPa, engine speed be 80 revs/min, the nine, the ten sections heating between set
Vacuum volatilization is put, head arranges the porous sheet material that zirconium is supported on pyrophillite sintering, in second-order screw rod lateral shear and footpath
To under pressure condition, the biodiesel isomerization of n-alkane in the very short time, so that improve the low temperature flow of biodiesel
Property, separate after being collected by the gas of vacuum volatilization and use；
3) using step 2) product that obtains through polyethylene glycol fiber films as filter membrane, by polyethylene glycol fiber films
To trace impurity adsorption filtration, high-purity biodiesel is obtained.
By test, 2 oils and fatss of embodiment are in liquid volume air speed 10h-1Under the conditions of to biodiesel hydrogenation conversion be
More than 96%, the biodiesel performance indications for obtaining are fully achieved standard GB/T/T20828-2007《Diesel fuel is adjusted
With with biodiesel》Key index, specific targets are as follows：
Embodiment 3
1) by incorgruous for the first rank of two steps type dual-screw-stem machine warmed-up for kitchen recovery oils and fatss injection engagement, screw slenderness ratio
40, screw diameter 45mm, the temperature setting of each conversion zone are followed successively by 80-100 DEG C, 100-120 DEG C, 100-110 DEG C, 100-90
DEG C, 90-80 DEG C, the first rank screw rod head pressure be 2MPa, engine speed be 300 revs/min, second and third section heating between set
Vacuum volatilization is put, the moisture in oils and fatss is excluded, hydrogen pump is set between three, four sections of heating, pump into hydrogen, head arranges copper oxide
The porous sheet material of Bauxite Sintering is supported on, by dispersion and the constant pressure of the first rank screw machine, oils and fatss is formed with hydrogen
Homogeneous reaction interface, quick catalysis are hydrogenated with；
2) engaged by the second-order for entering two steps type dual-screw-stem machine after the first rank screw rod catalytic hydrogenation in the same direction, screw slenderness ratio
48, screw diameter 65mm, the temperature setting of each conversion zone are followed successively by 100-120 DEG C, 120-130 DEG C, 120-100 DEG C, 110-80
DEG C, 1 thorium be supported on basalt sintering porous sheet material, under the conditions of second-order screw rod lateral shear and radial pressure,
The biodiesel isomerization of n-alkane in very short time, so as to improve the low temperature flow of biodiesel, by vacuum volatilization
Gas be collected after separate use；
3) using step 2) product that obtains through polyethylene glycol fiber films as filter membrane, by polyethylene glycol fiber films
To trace impurity adsorption filtration, high-purity biodiesel is obtained.
By test, 3 oils and fatss of embodiment are in liquid volume air speed 9h-1Under the conditions of to biodiesel hydrogenation conversion be 96%
More than.
Embodiment 4
1) nibble incorgruous with the first rank that the compound lard of Petiolus Trachycarpi oil injects warmed-up two steps type dual-screw-stem machine for sunflower oil
Close, screw slenderness ratio 32, screw diameter 65mm, the temperature setting of each conversion zone are followed successively by 80-100 DEG C, 100-120 DEG C, 100-
110 DEG C, 100-90 DEG C, 90-80 DEG C, the first rank screw rod head pressure is 1.52MPa, and engine speed is 200 revs/min, the
2nd, vacuum volatilization is set between three sections of heating, excludes the moisture in oils and fatss, hydrogen pump is set between three, four sections of heating, pumps into hydrogen
Gas, head arrange the porous sheet material that phosphating sludge is supported on Bauxite Sintering, by dispersion and the constant pressure of the first rank screw machine,
Oils and fatss are made to form homogeneous reaction interface with hydrogen, quick catalysis are hydrogenated with；
2) by the incorgruous engagement of the second-order for entering two steps type dual-screw-stem machine after the first rank screw rod catalytic hydrogenation, screw slenderness ratio
45, screw diameter 75mm, the temperature setting of each conversion zone are followed successively by 100-120 DEG C, 120-130 DEG C, 120-100 DEG C, 110-80
DEG C, 100-80 DEG C, second-order screw rod head pressure be 5MPa, engine speed be 100 revs/min, the nine, the ten sections heating between set
Vacuum volatilization is put, head arranges the porous sheet material that niobium is supported on pyrophillite sintering, in second-order screw rod lateral shear and footpath
To under pressure condition, the biodiesel isomerization of n-alkane in the very short time, so that improve the low temperature flow of biodiesel
Property, separate after being collected by the gas of vacuum volatilization and use；
3) using step 2) product that obtains through polyethylene glycol fiber films as filter membrane, by polyethylene glycol fiber films
To trace impurity adsorption filtration, high-purity biodiesel is obtained.
By test, 4 oils and fatss of embodiment are in liquid volume air speed 12h-1Under the conditions of to biodiesel hydrogenation conversion be
More than 96%.
Claims (6)
1. a kind of utilization screw mechanism is characterized in that by two steps type double screw extruder, using spiral shell for the method for biodiesel
When the threaded block combination of bar machine realizes that biodiesel is continuously produced, one step completes catalytic hydrogenation, isomery and dehydration, degassing, tool
Preparation is as follows：
1) oils and fatss are injected the first rank of warmed-up two steps type dual-screw-stem machine, the temperature setting of each conversion zone is followed successively by 80-100
DEG C, 100-120 DEG C, 100-110 DEG C, 100-90 DEG C, 90-80 DEG C, the first rank screw rod head pressure be 0.5-2MPa, engine speed
For 200-300 rev/min, vacuum volatilization is set between second and third section is heated, is excluded the moisture in oils and fatss, is heated at three, four sections
Between hydrogen pump is set, pump into hydrogen, head arranges hydrogenation catalyst porous plate, by dispersion and the constant pressure of the first rank screw machine,
Oils and fatss are made to form homogeneous reaction interface with hydrogen, quick catalysis are hydrogenated with；
2) by the second-order for entering two steps type dual-screw-stem machine after the first rank screw rod catalytic hydrogenation, the temperature setting of each conversion zone is successively
For 100-120 DEG C, 120-130 DEG C, 120-100 DEG C, 110-80 DEG C, 100-80 DEG C, second-order screw rod head pressure is 2-5MPa,
Engine speed is 50-100 rev/min, arranges vacuum volatilization, received by the gas of vacuum volatilization between the nine, the ten sections of heating
Separate after collection and use, head arranges heterogeneous catalyst porous plate, under the conditions of second-order screw rod lateral shear and radial pressure, just
The biodiesel isomerization of structure alkane, so that improve the low temperature flow of biodiesel；
3) by step 2) product that obtains through polyethylene glycol fiber films filter membrane, by polyethylene glycol fiber films to micro miscellaneous
Matter adsorption filtration, obtains high-purity biodiesel；
Wherein preparation process 1), step 2) described in two steps type dual-screw-stem machine be two steps type in the same direction engagement or incorgruous meshed double screw
Extruder, is a kind of flow reactor advanced by rotational shear, is made up of two ranks, and the composition of the first rank and second-order is distinguished
For：Engagement is nibbled with incorgruous with incorgruous meshed double screw extrusion, incorgruous engagement with meshed double screw in the same direction extrusion, in the same direction engagement in the same direction
Close twin-screw extrusion, incorgruous engagement to extrude with meshed double screw in the same direction, wherein the first rank screw slenderness ratio >=25, arrange to have and cut
The threaded block for cut, disperse, conveying；Second-order screw slenderness ratio >=40, arrange and there is shearing, engagement, backflow, the screw thread of conveying
Block, the threaded block that flows back are provided to ensure that the time of staying of the reaction mass in screw rod in 10-15 minutes, by two stage structures,
When realizing that biodiesel is continuously produced, a step completes catalytic hydrogenation, isomerization.
2. a kind of utilization screw mechanism according to claim 1 is characterized in that for the method for biodiesel：Preparation process
1), step 2) described in the double rank of two steps type dual-screw-stem machine be the double screw extruder of engagement in the same direction.
3. a kind of utilization screw mechanism according to claim 1 is characterized in that for the method for biodiesel：Preparation process is 1)
The animal and plant fat of described oils and fatss its main components for triglyceride, the acid value of oils and fatss 120mgKOH/g with
Interior, with wider adaptability.
4. a kind of utilization screw mechanism according to claim 1 is characterized in that for the method for biodiesel：Preparation process is 1)
Described hydrogen pump-in pressure is 0.5-1MPa.
5. a kind of utilization screw mechanism according to claim 1 is characterized in that for the method for biodiesel：Preparation process is 1)
Described hydrogenation catalyst porous plate is that tungsten, nickel, cobalt, molybdenum, the oxide of copper or phosphide are supported on Bauxite Sintering and form
Porous sheet material, wherein aperture be 0.1-0.5mm；Preparation process 2) described in heterogeneous catalyst porous plate be palladium, zirconium, thorium, niobium
Basalt, the porous sheet material of pyrophillite sintering is supported on, wherein aperture is 0.1-0.5mm.
6. a kind of utilization screw mechanism according to claim 1 is characterized in that for the method for biodiesel：Preparation process is 3)
The fibre gap of described polyethylene glycol fiber films is 0.05-0.1 μm, and it is 0.2-0.5MPa to arrange mould difference during Purification by filtration,
The extremely strong polar character of polyethylene glycol fiber films, has strong adsorption interconnection function with micro impurity in biodiesel, so as to
Obtain high-purity biodiesel.
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| CN100410349C (en) * | 2006-09-07 | 2008-08-13 | 中国林业科学研究院林产化学工业研究所 | Method for producing biological diesel oil through homogeneous successive reaction |
| CN101463272B (en) * | 2007-12-20 | 2012-09-05 | 中国石油化工股份有限公司 | Method for generating diesel by hydrotreating biological oil |
| CN101550349A (en) * | 2008-03-31 | 2009-10-07 | 西安市宝润实业发展有限公司 | Method for preparing biodiesel by supercritical technology |
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