CN101029244A - Production of biological diesel oil - Google Patents
Production of biological diesel oil Download PDFInfo
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- CN101029244A CN101029244A CNA2007100346832A CN200710034683A CN101029244A CN 101029244 A CN101029244 A CN 101029244A CN A2007100346832 A CNA2007100346832 A CN A2007100346832A CN 200710034683 A CN200710034683 A CN 200710034683A CN 101029244 A CN101029244 A CN 101029244A
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- oil
- esterification
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- methyl esters
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
Production of biological diesel oil is carried out by adding into cation polyacrylamide 0.1-0.4wt% of waste oil, ungluing, vacuum-dewatering to obtain unglued crude oil, pre-heating for dewatered crude oil, entering into distilling tower, distilling for free fatty acid and steam simultaneously, heat-exchanging for distilled fatty acid by preheated dewatered crude oil, classified esterifying, de-coloring, removing impurities, inducing micron-fatty coloring matter and micron-solid high-dielectric material to aggregate at bottom, pumping supernatant and packing. It's simple, cheap, reliable and efficient and has friendly environment. It can be used for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of production method of biofuel, particularly adopting cheap sewer oil is the raw material production biofuel.
Background technology
Sewer oil is actually the notion of a general reference, is people's common names for all kinds of poor quality oils in life.Generally, sewer oil can be divided into following a few class: the one, the sewer oil of narrow sense, be about in the water drain greasy floating matter or with leftovers, the oil of leftovers (common name swill) of hotel, restaurant through simply processing, extracting; The 2nd, pork inferior, haslet, pigskin processing and the oil that refines the back output; The 3rd, after the oily access times that are used for fried food product surpass specified requirement, be repeated again to use or toward wherein adding the oil of reusing behind some fresh oils.
Sewer oil will be smelt qualified biofuel need remove mechanical impurity and colloid, adopts chemical process to need processes such as esterification, dealcoholysis, distillation purification.Mechanical impurity in the grease can be removed by simple filtration, and colloid is because of dissolving each other with grease, and simple filtration can't be removed at all, generally adopts sour waterization to come unstuck, or with phosphoric acid or with the vitriol oil or use oxalic acid, consumption is at 1-5%.Because the large usage quantity of mineral acid and oxalic acid is serious to equipment corrosion, discharges the back with waste water environment is caused new pollution; The esterification of sewer oil because of its acid number all more than 40, adopt chemical method production to need pre-esterification alcoholysis again, this processing step is many, the time is long, energy consumption is high, the methyl alcohol loss is big; For the biofuel that obtains the standard that reaches generally also need be distilled purification, no matter adopt which kind of its yield of distillation mode all at (for sewer oil) below 85%.
Summary of the invention
Purpose of the present invention aims to provide that a kind of technology is simple, reliable, recovery rate is high, production cost is low, save energy, environmentally friendly, is suitable for the production technique of large-scale industrial production.
The objective of the invention is to realize by following manner:
Processing step of the present invention comprises:
A, come unstuck: add after cation polypropylene acyl ammonia comes unstuck, again the vacuum hydro-extraction crude oil that must come unstuck;
B, resin acid separate: the crude oil preheating of will dewatering, enter distillation tower again, and free lipid acid and steam steam jointly, and the distillation tower bottoms is a grease, and the lipid acid that distills carries out heat exchange by preheating dehydration crude oil;
C, classification esterification: 1. grease adding sodium methylate and the methyl alcohol that the b step is obtained carries out esterification; Reaction finishes the back quiescent setting, and lower floor's glycerine methanol solution is emitted, and the upper strata methyl esters is delivered to dielectric gravity field decolouring removal of impurities;
2. the distilled fatty acid that will handle through heat exchange carries out esterification under melting state, finishes reaction 1 below when the acid number of lipid acid drops to, and neutralizes, dealcoholysis; Methyl esters washing after the dealcoholysis, through vacuum hydro-extraction, the methyl esters after the dehydration was pumped to dielectric gravity field decolouring removal of impurities when the methyl esters pH value was neutral;
D, decolouring removal of impurities: under 800-1500V voltage, by high dielectric material induce micron-sized fat-soluble pigment and micron-sized solid impurity to the bottom assemble, grow up, sedimentation, upper clear supernate then pump to the finished product jar.
When sewer oil was warmed up to 60-70 ℃ during described a went on foot, adds the 0.1-0.5 ‰ cation polypropylene acyl ammonia that takes up an area of the ditch oil quality and come unstuck.
Described b is distillation tower control residual voltage 0.22～0.87kPa in the step, and temperature is 230～260 ℃, feeds 0.4～0.6MPa steam.
The lipid acid that described b distilled in the step is used for preheating dehydration crude oil and carries out heat exchange, and when the lipid acid temperature that distills was reduced to 80-100 ℃, a part was delivered to trap and captured the lipid acid that other distills, and a part is delivered to hold-up vessel and stored.
During 1. described c goes on foot, grease obtainedly under temperature 55-65 ℃, pressure 0.2MPa, carry out esterification.
During 1. described c goes on foot, esterification finishes the back quiescent setting, because glycerine, methyl esters proportion differ bigger, two-layer about in still, being divided into very soon, when temperature of charge is reduced to 38-42 ℃, lower floor's glycerine methanol solution is emitted, send into climbing-film evaporator and remove methyl alcohol, Methanol Recovery is utilized, and glycerol liquor is delivered to the glycerine workshop and handled, and upper strata methyl esters pump is to dielectric gravity field decolouring removal of impurities.
During 2. described c goes on foot, add the methyl alcohol and the vitriol oil, carry out esterification under temperature 60-75 ℃, this esterifying kettle band alcohol tower, the dehydration of esterification limit, limit, backflow methyl alcohol advances pump entry, through the recycle pump Forced Mixing, has accelerated esterification.
In d goes on foot, in the dielectric gravity field container of high dielectric material barium titanate has been installed, voltage is risen to 800-1500V, micron-sized fat-soluble pigment is separated with biofuel with micron-sized solid impurity, fat-soluble pigment flash liberation rate reaches more than 90%, the granulometric impurity clearance reaches more than 99.5%, and the finished product loss is 1%, no waste liquid exhaust gas emission.
The present inventor once improves well to the technical process of production biofuel, no longer is that sour waterization is come unstuck simply, and the technology of coming unstuck is more reasonable, more helps meeting environmental protection requirement.And in the resin acid separating process, the waste heat that makes full use of the lipid acid that distills out comes the dehydration crude oil of gained of preceding step of preheating, has saved the energy.The also more environmental protection of decolouring removal of impurities process, decolorizing effect is better, and is more thorough.Thereby technical process of the present invention more meets modern environmental protection with respect to prior art, the requirement of save energy, and yield rate height, and production cost is low.
It is simple, reliable that method of the present invention also has technology, the characteristics that esterification rate is fast, average response can finish in 5 hours, acid number can be reduced to below the 1mgKOH/g, and conversion rate of fatty acid is up to more than 95%, and the finished product recovery rate is 92%, below the methanol consumption 125kg/ ton finished product, production cost is low, can not cause new pollution to environment, is suitable for large-scale industrial production.
Concrete step of preparation process of the present invention is:
A, come unstuck, sewer oil is imported glue kettle, be warmed up to 60-70 ℃, add oil quantity 0.1-0.5 ‰ cation polypropylene acyl ammonia (first furnishing 6 ‰ aqueous solution), stirrings, be incubated quiescent setting 6-12 hour, bleed off the bottom hydrosol, the vacuum hydro-extraction crude oil that must come unstuck again.
B, resin acid separate, to dewater again crude oil with pump be input into the interchanger preheating, the degassing enters extracting tower, residual voltage maintains 0.22～0.87kPa, temperature is 230～260 ℃, and feeds 0.4～0.6MPa steam, and free acid and steam steam jointly, the lipid acid that distills is used for preheating dehydration crude oil, when the lipid acid temperature that distills was reduced to 80-100 ℃, a part was got to trap with pump and is captured the lipid acid that other distills, and a part is got to hold-up vessel and stored.The net loss of crude oil is about 0.1～0.7%, and the acid value of oil and fat that obtains is below 1, and the acid number of distillatory lipid acid is more than 180.
C, classification esterification:
1. acid number is pumped into esterifying kettle at the grease below 1, add under sodium methylate and methyl alcohol, temperature 55-65 ℃, pressure 0.2MPa and carry out alcoholysis reaction.Reaction finishes the back quiescent setting, because glycerine, methyl esters proportion differ bigger, in still, be divided into two-layer up and down very soon, when temperature of charge is reduced to 40 ℃, lower floor's glycerine methanol solution is emitted, pump into climbing-film evaporator and remove methyl alcohol, the Methanol Recovery utilization, glycerol liquor is delivered to the glycerine workshop and is handled, and upper strata methyl esters pump is to dielectric gravity field decolouring removal of impurities;
2. acid number is pumped into esterifying kettle at the distilled fatty acid more than 180 under melting state, add the methyl alcohol and the vitriol oil, carry out esterification under temperature 60-75 ℃, this esterifying kettle band alcohol tower, the dehydration of esterification limit, limit, backflow methyl alcohol advances pump entry, through the recycle pump Forced Mixing, accelerated esterification.When dropping to, acid number finishes reaction, neutralization, dealcoholysis below 1.Methyl esters pump to water washing tank after the dealcoholysis is washed, when the methyl esters pH value is neutral through vacuum hydro-extraction.Methyl esters pump after the dehydration is to dielectric gravity field decolouring removal of impurities.
D, decolouring removal of impurities, under 800-1500V voltage, by the high dielectric material barium titanate induce micron-sized fat-soluble pigment and micron-sized solid impurity to the bottom assemble, grow up, sedimentation, upper clear supernate then pump to the finished product jar.
Process characteristic of the present invention is:
1, cation polypropylene acyl ammonia degumming technology.Positively charged macromolecular material has the intensive neutralizing effect to electronegative particle, contains a large amount of electronegative colloids in the sewer oil, and cation polypropylene acyl ammonia has neutralization, winding effect, the colloid more than 90% in the oil can be deviate from.Compare the characteristics such as its no burn into is pollution-free, cost is low that solely show with ordinary method.2, the present invention has the isolating characteristics of less energy-consumption---and when general raw produce adopted fractionation by distillation, crude product needed with steam or thermal oil preheating, and finished product need be used water quench, consumes a large amount of energy.And self trapping technique---promptly come the preheating crude product, the finished product that is cooled is captured fresh finished product more conversely, avoided the use water coolant, reduce pre-thermal energy source more than 1/2, separate total energy-conservation the reaching about 2/3 of link with finished product.3, the present invention is attached to dielectric gravity field decolouring impurity removing technology in the technology of the present invention well.: when specific inductivity between two kinds of materials differs more than 10 times (ξ 1 ξ 2), their the different sites place is subjected in non-homogeneous dielectric gravity field dielectric field force Fd differ 100 to 150 times.Particulate is assembled gradually and is grown up, thereby it can be separated with other medium because stressed difference will inevitably be moved to some specific directions.Use processing method decolouring removal of impurities of the present invention to have and fat-soluble pigment flash liberation rate can be reached more than 90%, the granulometric impurity clearance reaches more than 99.5%, and the finished product loss is 1%, no waste liquid exhaust gas emission.Chemical method cost before having broken away from is higher, and when being the sorbent material decolouring with atlapulgite or activated carbon, loss is big, and waste residue is many, environment is had the situation of certain pollution.
Embodiment
Embodiments of the invention are intended to illustrate the present invention rather than the present invention are further limited.
Embodiment
1, come unstuck
Pump into 15 tons of crude oils in glue kettle, be heated to 60-70 ℃, 6 ‰ cation polypropylene acyl ammonia soln 250-1250kg are poured into, stirred 2 hours, static then 8 hours, the bottom hydrosol is bled off (waste water advances oil trap to be handled).Upper strata crude oil reheat to 100 ℃ is poured the 250kg saturated brine into, stirs 1 hour, static 8 hours, the bottom aqueous solution is bled off (waste water advances oil trap to be handled) again.Crude oil after coming unstuck is beaten to the vacuum drying tank dehydration with pump, and the crude oil after the dehydration is input into the interchanger preheating with pump.
2, resin acid separates
The crude oil that will dewater is input into interchanger 1,2,3 with pump, and (interchanger 1,2 is the processed oil preheating to distillation tower, interchanger 3 is the thermal oil preheating), at vacuum tightness 0.22～0.87kPa, temperature is 230～260 ℃, and feed under 0.4～0.6MPa steam the free fatty acids in the crude oil is steamed, distilled fatty acid is cooled to 80-100 ℃ in interchanger 1,2, a part is got to trap with pump and captured the lipid acid that other distills, and a part is got to hold-up vessel and stored.The acid number of distilled fatty acid guarantees more than 180.Bottoms is a grease, and acid number is below 1.
3, the classification esterification
Acid number is pumped into esterifying kettle for 16 tons at the grease below 1, add 4 ton of 5% methanol solution of sodium methylate, temperature 55-65 ℃, below the pressure 0.3Mp, reacted 2.5 hours, it is stopped reaction that sampling, stratographic analysis grease are converted into that fatty acid methyl ester reaches more than 95%, and reaction pumps into setting tank with material in the still, static layering after finishing immediately.Lower floor's glycerine methanol solution is emitted, pump into climbing-film evaporator and remove methyl alcohol, the Methanol Recovery utilization, glycerol liquor is delivered to the glycerine workshop and is handled, and upper strata methyl esters pump is to dielectric gravity field decolouring removal of impurities;
The lipid acid of acid number more than 180 is pumped into esterifying kettle for 14 tons, add 6 tons of methyl alcohol, the 200kg vitriol oil, temperature 60-75 ℃, reacted 6-8 hour, new Henkel Production Flow Chart, pure tower dehydration, backflow methyl alcohol is through recycle pump and material Forced Mixing, sampling analysis acid number 1 following stopped reaction, soda ash is neutralized to pH value 6.5.The intensification dealcoholysis, 110 ℃ stop dealcoholysis, methyl esters pump to the water washing tank after the dealcoholysis is washed, when the methyl esters pH value is neutral through vacuum hydro-extraction.Methyl esters pump after the dehydration is to dielectric gravity field decolouring removal of impurities.
4, decolouring
Under 800-1500 volt voltage, by the high dielectric material barium titanate induce micron-sized fat-soluble pigment and micron-sized solid impurity to the bottom assemble, grow up, sedimentation.1 hour upper back stillness of night, but pump was to the finished product jar.Pump into methyl esters to be decoloured again, the circulation of beginning in week when treating bottom pigment thickness, is discharged viscous fluid methyl esters total loss rate 1%.
The biofuel recovery rate that the inventive method is produced is more than 92%, methyl alcohol consumption 125kg/ ton biofuel, and 280 yuan of/ton biofuel of energy consumption (contain coal), methyl ester conversion rate is more than 95%.Acid number of biodiesel is below 1, and color and luster is below 1, density 8.6-8.9, and 2 ℃ of cold filter clogging temperatures, 0 ℃ of condensation point, cetane value 49 to 52, meets petrochemical industry No. zero diesel oil standard fully by flash-point 110-160 ℃.
Claims (7)
1, a kind of production method of biofuel, it is characterized in that: processing step comprises:
A, come unstuck: add after cation polypropylene acyl ammonia comes unstuck, again the vacuum hydro-extraction crude oil that must come unstuck;
B, resin acid separate: the crude oil preheating of will dewatering, enter distillation tower again, and free lipid acid and steam steam jointly, and the distillation tower bottoms is a grease, and the lipid acid that distills carries out heat exchange by preheating dehydration crude oil;
C, classification esterification: 1. grease adding sodium methylate and the methyl alcohol that the b step is obtained carries out esterification; Reaction finishes the back quiescent setting, and lower floor's glycerine methanol solution is emitted, and the upper strata methyl esters is delivered to dielectric gravity field decolouring removal of impurities;
2. the distilled fatty acid that will handle through heat exchange carries out esterification under melting state, finishes reaction 1 below when the acid number of lipid acid drops to, and neutralizes, dealcoholysis; Methyl esters washing after the dealcoholysis, through vacuum hydro-extraction, the methyl esters after the dehydration was pumped to dielectric gravity field decolouring removal of impurities when the methyl esters pH value was neutral;
D, decolouring removal of impurities: under 800-1500V voltage, by high dielectric material induce micron-sized fat-soluble pigment and micron-sized solid impurity to the bottom assemble, grow up, sedimentation, upper clear supernate then pump to the finished product jar.
2, the production method of a kind of biofuel according to claim 1 is characterized in that: when sewer oil was warmed up to 60-70 ℃ during described a went on foot, adds the 0.1-0.5 ‰ cation polypropylene acyl ammonia that takes up an area of the ditch oil quality and come unstuck.
3, the production method of a kind of biofuel according to claim 1 is characterized in that: described b is distillation tower control residual voltage 0.22～0.87kPa in the step, and temperature is 230～260 ℃, feeds 0.4～0.6MPa steam.
4, the production method of a kind of biofuel according to claim 1, it is characterized in that: the lipid acid that described b distilled in the step is used for preheating dehydration crude oil and carries out heat exchange, when the lipid acid temperature that distills is reduced to 80-100 ℃, a part is delivered to trap and is captured the lipid acid that other distills, and a part is delivered to hold-up vessel and stored.
5, the production method of a kind of biofuel according to claim 1 is characterized in that: during 1. described c goes on foot, grease obtainedly carry out esterification under temperature 55-65 ℃, pressure 0.2MPa.
6, the production method of a kind of biofuel according to claim 1, it is characterized in that: during 1. described c goes on foot, esterification finishes the back quiescent setting, owing to glycerine, methyl esters proportion differ bigger, is divided into two-layer up and down in still very soon, when temperature of charge is reduced to 38-42 ℃, lower floor's glycerine methanol solution is emitted, send into climbing-film evaporator and remove methyl alcohol, the Methanol Recovery utilization, glycerol liquor is delivered to the glycerine workshop and is handled, and upper strata methyl esters pump is to dielectric gravity field decolouring removal of impurities.
7, the production method of a kind of biofuel according to claim 1, it is characterized in that: during 2. described c goes on foot, the distilled fatty acid that to handle through heat exchange is under melting state, add the methyl alcohol and the vitriol oil, carry out esterification, this esterifying kettle band alcohol tower under temperature 60-75 ℃, the dehydration of esterification limit, limit, backflow methyl alcohol advances pump entry, through recycle pump Forced Mixing, enhance esterification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100346832A CN101029244A (en) | 2007-04-06 | 2007-04-06 | Production of biological diesel oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100346832A CN101029244A (en) | 2007-04-06 | 2007-04-06 | Production of biological diesel oil |
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| Publication Number | Publication Date |
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| CN101029244A true CN101029244A (en) | 2007-09-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2007100346832A Pending CN101029244A (en) | 2007-04-06 | 2007-04-06 | Production of biological diesel oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232141A (en) * | 2014-09-28 | 2014-12-24 | 深圳市日东生物能源有限公司 | Method for preparing biodiesel from illegal cooking oil, acid oil and waste animal and plant grease |
| CN106811308A (en) * | 2016-12-23 | 2017-06-09 | 惠州市鑫隆环保科技有限公司 | A kind of preparation method of industrial fuel oil |
| CN109181793A (en) * | 2018-11-02 | 2019-01-11 | 广西南宁高斯特科贸有限公司 | A kind of preparation method of biofuel oil |
| CN110331030A (en) * | 2019-08-19 | 2019-10-15 | 福建钰融科技有限公司 | A kind of regenerating waste oil degumming agent and its methods for making and using same |
-
2007
- 2007-04-06 CN CNA2007100346832A patent/CN101029244A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232141A (en) * | 2014-09-28 | 2014-12-24 | 深圳市日东生物能源有限公司 | Method for preparing biodiesel from illegal cooking oil, acid oil and waste animal and plant grease |
| CN104232141B (en) * | 2014-09-28 | 2015-12-09 | 深圳市日东生物能源有限公司 | A kind of method of sewer oil, acidification oil, preparing biological diesel oil from waste animals and plants grease |
| CN106811308A (en) * | 2016-12-23 | 2017-06-09 | 惠州市鑫隆环保科技有限公司 | A kind of preparation method of industrial fuel oil |
| CN109181793A (en) * | 2018-11-02 | 2019-01-11 | 广西南宁高斯特科贸有限公司 | A kind of preparation method of biofuel oil |
| CN110331030A (en) * | 2019-08-19 | 2019-10-15 | 福建钰融科技有限公司 | A kind of regenerating waste oil degumming agent and its methods for making and using same |
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