CN104312733B - A kind of biodiesel and preparation method thereof - Google Patents
A kind of biodiesel and preparation method thereof Download PDFInfo
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- CN104312733B CN104312733B CN201410621025.3A CN201410621025A CN104312733B CN 104312733 B CN104312733 B CN 104312733B CN 201410621025 A CN201410621025 A CN 201410621025A CN 104312733 B CN104312733 B CN 104312733B
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- biodiesel
- acid
- preparation
- esterification
- reaction kettle
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- 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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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Liquid Carbonaceous Fuels (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to petrochemical industry, be specifically related to a kind of biodiesel and preparation method thereof, comprise the steps: step 1: use CO2Air in displacement reaction kettle of the esterification, by the reaction kettle of the esterification of monomer acids input heat-conducting oil heating, is simultaneously introduced high temperature resistant macropore polystyrene storng-acid cation exchange resin；Step 2: made the material in reaction kettle of the esterification be warming up to 130 160 DEG C in 30 minutes, be continuously added to DMM；Step 3: when extremely described material acid number is less than 1mgKOH/g, stops adding DMM, material is cooled to less than 80 DEG C blowings, obtains biodiesel semi-finished product；Step 4: when described biodiesel semi-finished product are cooled to 30 DEG C, adds after composite catalyst is sufficiently stirred for and gets product.The biodiesel that the inventive method prepares has good water-resistance, and it is immiscible to meet water, and winter, starting performance was good, can in any proportion with petrifaction diesel phase mixture, economic benefit is good.
Description
Technical field
The present invention relates to petrochemical industry, be specifically related to a kind of biodiesel and preparation method thereof.
Background technology
Biodiesel mainly produces with chemical method, by animal and plant fat and the low-carbon alcohols such as methanol, ethanol in nothing
Carry out ester exchange reaction under machine highly acid or strong alkali catalyst and high temperature, generate corresponding fatty acid methyl ester or
Ethyl ester, more scrubbed it is drying to obtain biodiesel.Methanol or ethanol can be recycled in process of production, raw
Side-product glycerol can be produced during product.Have the disadvantage that with this technique biodiesel synthesis: complex process,
Need subsequent treatment such as washing, be dried, considerably increase production cost.
Recently, people begin one's study and use biological enzyme biodiesel synthesis, i.e. lead to by animal oil and low-carbon alcohols
Cross lipase and carry out ester exchange reaction, prepare corresponding fatty acid methyl ester and ethyl ester.Enzymatic Synthesis of Biodiesel
Have that mild condition, alcohol consumption be little, the advantage of non-pollution discharge.But currently mainly problem has: to methanol and
The conversion ratio of ethanol is low, is typically only 40%-60%, due to current lipase to the esterification of long-chain fatty alcohol or
Transesterification effectively, and low to the short chain fatty alcohol such as conversion ratio such as methanol or ethanol.And short chain fatty alcohol is to enzyme
There is certain toxicity, make shorten the service life of enzyme.By-product glycerin and shipwreck are in recovery, not only to product shape
Become suppression, and glycerol is toxic to immobilized enzyme, also can make immobilized enzyme shortening in service life.
At present, producing biodiesel raw material both at home and abroad is animal and plant fat, such as Publication No. mostly
CN1570029, the Chinese invention patent application of entitled " method being prepared biodiesel by natural oil ",
This disclosure of the invention, with natural oil as raw material, is carried out with 1-3 carbon molecular weight under mineral acid catalyst effect
Transesterification, the method needs through steps such as dehydration, dealcoholysis, separation glycerol, distillations, and process is more multiple
Miscellaneous, energy consumption is the biggest, considerably increases the production cost of product.And directly with fatty acid as raw material production
The relevant report of biodiesel is the most few, and such as Publication No. CN1060089 is entitled: " C6-24 fat
Acid semicontinuous formicester operation mode and optimization " Chinese invention patent disclose: saturated with C6-24
It is raw material with unsaturated fatty acid, under conditions of methyl-hydrogen-sulfate monomethyl-sulfate is catalyst, carries out esterification with methanol,
This production method is relatively simple, and the response time is comparatively short, but the catalyst sulfuric acid hydrogen methyl ester used by reaction
Belong to extremely toxic substance, bring bigger hidden danger to production safety.
Summary of the invention
The technical problem to be solved is: provides a kind of production process safety and environmental protection, prepares
The preparation method of the biodiesel that biodiesel fuel quality is good.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is:
The preparation method of a kind of biodiesel, comprises the steps:
Step 1: use CO2Air in displacement reaction kettle of the esterification, by the ester of monomer acids input heat-conducting oil heating
Change in reactor, be simultaneously introduced high temperature resistant macropore polystyrene storng-acid cation exchange resin；
Step 2: made the material in reaction kettle of the esterification be warming up to 130-160 DEG C in 30 minutes, be continuously added to
DMM；
Step 3: when extremely described material acid number is less than 1mgKOH/g, stops adding DMM, is lowered the temperature by material
To less than 80 DEG C blowings, obtain biodiesel semi-finished product；
Step 4: when described biodiesel semi-finished product are cooled to 30 DEG C, adds composite catalyst and is sufficiently stirred for
After get product, described composite catalyst nitrate compound, oleic acid, alcohols thing are anticorrosive with polyacids class
Agent mixing composition.
Preferably, in the preparation method of above-mentioned biodiesel, described composite catalyst is by following weight portion
Raw material mixes: nitrose 10-40 part, oleic-acid 20-30 part, alcohols preferred 50-60 part, polyacids class
0.00001-0.00005 part；Described nitrose is ethylene glycol formic acid esters, and described oleic-acid is oleic acid, described alcohol
Class is ethanolamine, and described polyacids class is dimeric dibasic acid.
Preferably, in the preparation method of above-mentioned biodiesel, the feeding quantity of described composite catalyst is biological
4/1000ths of diesel oil semi-manufactured goods quality.
Preferably, in the preparation method of above-mentioned biodiesel, described step 3 is particularly as follows: course of reaction takes
Sample detection material acid number, its time is spaced apart 2-4 hour, when extremely described material acid number is less than 1mg KOH/g,
Stop adding DMM, material is cooled to less than 80 DEG C blowings, obtains biodiesel semi-finished product.
Preferably, in the preparation method of above-mentioned biodiesel, described monomer acids is by Oleum Gossypii semen or Semen sojae atricolor
Fatty acid oil side-product when heat polymerization synthesis dimer (fatty acid) yl, in dimer (fatty acid) yl purification process
Obtaining, it includes the component composition of following mass percent: for 5-10% Palmic acid, 45-60% oleic acid, 30-50%
Isomerization fatty acid.
The life that another technical scheme that the present invention provides is prepared for providing the preparation method of a kind of above-mentioned biodiesel
Thing diesel oil.
The beneficial effects of the present invention is: the preparation method of the biodiesel of the present invention uses high temperature resistant macropore
Polystyrene storng-acid cation exchange resin is as catalyst, and it has the advantage that corrosivity is low, nontoxic,
The use reducing production equipment requires thus reduces production cost, the biology that the inventive method prepares
Diesel oil has good water-resistance, and chance water is immiscible, and starting performance was good, in the environment of-10 DEG C not winter
There is solidification and the difficult and hot air-resistance phenomenon of cold start-up；Life-time service will not occur metal erosion and swell rubber；
Flash-point is low, complies fully with GB diesel-fuel flash point requirement；Can in any proportion with petrifaction diesel phase mixture,
Economic benefit is good.
Accompanying drawing explanation
Fig. 1 is the structural representation of the preparation facilities of the biodiesel in the specific embodiment of the invention；
Label declaration:
1, reaction kettle of the esterification；2, methanol rectifying tower；3, methanol condenser；4, surge tank；5, methanol adds
Batch can.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, below in conjunction with embodiment also
Accompanying drawing is coordinated to be explained.
The design of most critical of the present invention is: the preparation method of biodiesel of the present invention uses DMM (dimethoxy
Methylmethane) as raw material, and with the addition of compound additive, improve the performance of gained biodiesel.
DMM (dimethoxymethane) high definition fuel is a kind of New-type fuel, with the main product of China's Coal Chemical Industry
Product dimethyl ether or methanol and metaformaldehyde are raw material, obtain after distillation pressurized catalysis.
Embodiment 1
The preparation method of a kind of biodiesel is provided, comprises the steps:
Step 1: use CO2Air in displacement reaction kettle of the esterification 1, by monomer acids input heat-conducting oil heating
In reaction kettle of the esterification, it is simultaneously introduced high temperature resistant macropore polystyrene storng-acid cation exchange resin；
Step 2: made the material in reaction kettle of the esterification be warming up to 130-160 DEG C in 30 minutes, then 30
DMM is added through methanol feed tank 5 continuously, the soda acid of material in attention response still in shot process in minute
Degree；
Step 3: when extremely described material acid number is less than (GB264-1983) mgKOH/g0.09, stops adding DMM,
After being sufficiently stirred for reacting 2 hours, mix with the stirring of front material through methanol rectifying tower 2 profit reduction and reserving to methanol condenser 3
React 2 hours, material is cooled to less than 70-80 DEG C blowing and is transported to semi-finished product tank (surge tank 4), obtain life
Thing diesel oil semi-finished product also continue cooling；
Step 4: when described biodiesel semi-finished product are cooled to 30 DEG C, adds the composite catalyzing of 4/1000ths
Agent (the preparation of composite catalyst；By nitrate compound, oleic acid, alcohols thing and polyacids class corrosion inhibitor
Mixing composition gets product, material combination: nitrose 10-40 part, oleic-acid 20-30 part, alcohols 50-60
Part, polyacids class be 100,000/.) keep 30 DEG C to be sufficiently stirred for 40 minutes after cool down and get product.
Embodiment 2
The preparation method of a kind of biodiesel, comprises the steps: before pan feeding with in CO2 replacement reaction kettle
Air, by the reaction kettle of the esterification 1 of monomer acids input heat-conducting oil heating, be simultaneously introduced D008 high temperature resistant
Punching polystyrene storng-acid cation exchange resin.When making material be warming up to 130-160 DEG C in 30 minutes,
DMM is continuously added to from methanol feed tank 5.The material acid number of sampling detection at regular intervals in course of reaction,
During until material acid number is less than 1mgKOH/g, stops adding DMM, material is cooled to 80 DEG C to transfer
Material, obtains vegetable oil methyl ester (novel biodiesel semi-finished product).Inject when vegetable oil methyl ester is cooled to 30 DEG C
Tank 6, is slowly added to get product after composite catalyst is sufficiently stirred for, and described composite catalyst is by following weight portion
Raw material mix: ethylene glycol formic acid esters 10 parts, oleic acid 20 parts, ethanolamine 50 parts, dimeric dibasic acid 0.00001
Part.
Comparative example 1
The preparation method of a kind of biodiesel, comprises the steps: to refer to accompanying drawing 1, is put into by monomer acids and uses
In the reaction kettle of the esterification 1 of heat-conducting oil heating, be simultaneously introduced D008 high temperature resistant punching polystyrene highly acid sun from
Sub-exchange resin.When material is warming up to 130-160 DEG C, methanol is continuously added to from methanol feed tank 5.Reaction
During at regular intervals sampling detection material acid number, until material acid number less than 1mgKOH/g time, stop
Only add methanol, material is cooled to less than 80 DEG C blowings, obtains biodiesel finished product.
Above-mentioned added catalyst is D008 high temperature resistant punching polystyrene storng-acid cation exchange resin,
Its feeding quantity is the 8-15% of monomer acids charging quality；Total addition of methanol is monomer acids charging quality
0.4-0.6 times, course of reaction sample interval is 2-4 hour, detects material acid number, until material acid number is little
When 1mgKOH/g, stop adding methanol.
Water vapour and the methanol gas of excess that course of reaction generates are directly entered methanol rectifying tower 2 and separate
Purifying, filler used by rectifying column is corrugated wire gauze packing, and tower reactor steam heats, and tower top methanol is through first
Entering surge tank 4 after alcohol condenser 3 condensation, the methanol of surge tank 4 is partly into methanol feed tank 5, and one
Partial reflux reenters methanol rectifying tower 2, and the methanol purity purified through methanol rectifying tower can weigh more than 98%
New methanol needed for course of reaction.
The preparation method gained biodiesel of above-mentioned comparative example biodiesel has the drawback that 1, condensation point and solidifying
Filter point is high；2: kinematic viscosity is bigger than normal；3, flash-point is high；4, water-resistance is poor.
Embodiment and comparative example gained biodiesel performance comparison:
1, by biodiesel 5Kg of comparative example 1 and embodiment 1 gained biodiesel 5Kg respectively with two bottles
The DMM high definition fuel of 5Kg is mixed, and after being sufficiently stirred for 40 minutes, respectively takes 500lm mixture respectively
Adding 500lm water, quickly shake causes water oil and is thoroughly mixed into milky oil mixing with water solution, quiet is put in platform
The time of oil-water separation is observed on face.Result: the time added with one bottle of oil-water separation of additive is 20 minutes
Within；And the time of the most additivated one bottle of oil-water separation is 8 hours.
2, by biodiesel 5Kg of comparative example 1 and embodiment 1 gained biodiesel 5Kg respectively with two bottles
The chemical industry light oil of 5Kg is mixed, and after being sufficiently stirred for 40 minutes, respectively takes 500lm mixture and is separately added into
500lm water, quickly shake causes water oil and is thoroughly mixed into milky oil mixing with water solution, quiet is put on table top sight
Examine the time of oil-water separation.Result: within being 40 minutes added with time of one bottle of oil-water separation of additive；
And the time of the most additivated one bottle of oil-water separation is more than 8 hours.
3, by biodiesel 5Kg of comparative example 1 and embodiment 1 or 2 gained biodiesel 5Kg respectively with
The mineral oil of two bottles of 5Kg together, after being sufficiently stirred for 40 minutes, respectively takes 500lm mixture and is separately added into
500lm water, quickly shake causes water oil and is thoroughly mixed into milky oil mixing with water solution, quiet is put on table top sight
Examine the time of oil-water separation.Result: within being 30 minutes added with time of one bottle of oil-water separation of additive；
And the time of the most additivated one bottle of oil-water separation is 8 hours.
4, by biodiesel 500ml of ratio 1 and embodiment 1 gained biodiesel 500ml respectively with two bottles
The GB mineral diesel of 500ml is mixed, and after being sufficiently stirred for 1 minute, respectively takes 500lm mixture and puts respectively
Enter automobile-used oil circuit sealing rings, rubber mass oil pipe, common sebific duct, observe after quiet bubble 12h by bubble thing.Result: a
Oil sealing ring had the most swelling, rubber mass oil pipe and common sebific duct are had obvious swellability；And b is oily
By bubble thing then stand intact.
5, biodiesel 500ml of ratio 1 is inserted with embodiment 1 gained biodiesel 500ml simultaneously set
It is calculated as-10 DEG C of condensation detectors, takes out after 4h and observe.Result: a oil has been frozen into white solid；And b
Oil is transparent gloss liquid.
In sum, the power performance, low of the novel biodiesel that biodiesel oil preparing process of the present invention prepares
Startup temperature performance, anticorrosive swelling resistance are comprehensively improved, and oil product saturated vapour pressure is notable
Reduce, effectively solve high temperature vapour lock problem, solve biodiesel simultaneously and meet the technical barrier that aqueous phase is molten,
Reach the effect of oil-water separation.This fuel applications is fully able to substitute existing petrifaction diesel on motor vehicles,
And good power effect can be reached, it is not necessary to and change vehicle and just can normally use, can be any with GB diesel oil
Ratio mixes, and does not affect vehicle power and performance, and fuel consumption is suitable with GB diesel oil, super quality and competitive price.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every profit
The equivalents made by description of the invention and accompanying drawing content, or directly or indirectly it is used in relevant technology
Field, is the most in like manner included in the scope of patent protection of the present invention.
Claims (6)
1. the preparation method of a biodiesel, it is characterised in that comprise the steps:
Step 1: use CO2Air in displacement reaction kettle of the esterification, by the ester of monomer acids input heat-conducting oil heating
Change in reactor, be simultaneously introduced high temperature resistant macropore polystyrene storng-acid cation exchange resin；
Step 2: made the material in reaction kettle of the esterification be warming up to 130-160 DEG C in 30 minutes, be continuously added to two
Methoxyl group methane；
Step 3: when extremely described material acid number is less than 1mgKOH/g, stops adding dimethoxymethane, will
Material is cooled to less than 80 DEG C blowings, obtains biodiesel semi-finished product；
Step 4: when described biodiesel semi-finished product are cooled to 30 DEG C, adds composite catalyst and is sufficiently stirred for
After get product, described composite catalyst is that ethylene glycol formic acid esters, oleic acid, ethanolamine mix group with dimeric dibasic acid
Become.
The preparation method of biodiesel the most according to claim 1, it is characterised in that described being combined is urged
Agent is mixed by the raw material of following weight portion: ethylene glycol formic acid esters 10-40 part, oleic acid 20-30 part, second
Hydramine 50-60 part, dimeric dibasic acid 0.00001-0.00005 part.
The preparation method of biodiesel the most according to claim 2, it is characterised in that described being combined is urged
The feeding quantity of agent is 4/1000ths of biodiesel semi-manufactured goods quality.
The preparation method of biodiesel the most according to claim 1, it is characterised in that described step 3
Particularly as follows: course of reaction sampling detection material acid number, its time is spaced apart 2-4 hour, to described material acid number
During less than 1mgKOH/g, stop adding dimethoxymethane, material is cooled to less than 80 DEG C blowings,
Biodiesel semi-finished product.
The preparation method of biodiesel the most according to claim 1, it is characterised in that described monomer
Acid is the side-product when heat polymerization synthesizes dimer (fatty acid) yl by Oleum Gossypii semen or soya fatty acid, two
In polyglycerol fatty acid purification process obtain, it include following mass percent component composition: for 5-10% Palmic acid,
45-60% oleic acid, 30-50% isomerization fatty acid.
6. according to the biodiesel prepared by the preparation method of the biodiesel described in any one of claim 1-5.
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| CN201410621025.3A CN104312733B (en) | 2014-11-06 | 2014-11-06 | A kind of biodiesel and preparation method thereof |
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