CN105950301A - Method for preparing biodiesel oil - Google Patents

Method for preparing biodiesel oil Download PDF

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Publication number
CN105950301A
CN105950301A CN201610270608.5A CN201610270608A CN105950301A CN 105950301 A CN105950301 A CN 105950301A CN 201610270608 A CN201610270608 A CN 201610270608A CN 105950301 A CN105950301 A CN 105950301A
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CN
China
Prior art keywords
methanol
reaction
soap stock
oil
biodiesel
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Pending
Application number
CN201610270608.5A
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Chinese (zh)
Inventor
蓝汉才
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Individual
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Individual
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Publication date
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Priority to CN201610270608.5A priority Critical patent/CN105950301A/en
Publication of CN105950301A publication Critical patent/CN105950301A/en
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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/04Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
    • C11C3/10Ester interchange
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS 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
    • C10L1/00Liquid carbonaceous fuels
    • C10L1/02Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B13/00Recovery of fats, fatty oils or fatty acids from waste materials
    • C11B13/02Recovery of fats, fatty oils or fatty acids from waste materials from soap stock
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS 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
    • C10L2200/00Components of fuel compositions
    • C10L2200/04Organic compounds
    • C10L2200/0461Fractions defined by their origin
    • C10L2200/0469Renewables or materials of biological origin
    • C10L2200/0476Biodiesel, i.e. defined lower alkyl esters of fatty acids first generation biodiesel
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Liquid Carbonaceous Fuels (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention relates to a method for preparing biodiesel oil. The method comprises the steps of subjecting a refined byproduct, i.e., niger, of a vegetable oil refinery, which serves as a raw material to concentrated drying, then, subjecting the dried material and methanol to an ester exchange reaction for 60 minutes in the presence of a sulfuric acid catalyst at the low temperature of 60 DEG C to 65 DEG C so as to produce corresponding fatty acid methyl esters, then, carrying out washing and drying, thereby obtaining the biodiesel oil and a byproduct, i.e., crude glycerol, wherein the esterification rate reaches 99.5%. The method has the advantages that the process is simple, the catalyzing speed is high, the conversion ratio is high, the operation is convenient, the reaction time is short, the reaction is free of pollution, and the aftertreatment is easy, thereby belonging to green chemical technologies.

Description

A kind of preparation method of biodiesel
Technical field
The present invention relates to the preparation method of a kind of biodiesel.
Background technology
The exhaustive exploitation of petroleum resources result in the oil crisis growed in intensity at present, and oil price one rises Rise again, not only annoying the development of auto industry, and the world local in the century that becomes history War fuse cord.How to reduce the dependence to oil, force scientists to strive to find the replacement of oil Fuel.Biodiesel is because of biodegradable, avirulence, environmental sound can be from regenerated resources Middle acquisition, and receive the extensive concern of people.
Biodiesel i.e. fatty acid methyl ester, mainly makes with vegetable oil and animal oil as raw material, Being the petroleum diesel succedaneum of high-quality, it can meet No. 2 discharge standards in Europe.With traditional diesel oil phase Ratio, its major advantage is: greasy property is good, stores, transports, uses safety, and anti-knock properties are good, can Biodegradation, for regenerated resources, nontoxic, burning is completely.Biodiesel is environmentally friendly fuel.
Affecting the commonly used subject matter of biodiesel at present is Cost Problems, with vegetable oil or animal Oil carries out transesterification reaction for raw material and produces biodiesel, although can obtain the preferably biological bavin of quality Oil, but also it is difficult to popularization and application in China at present.China's nigre of vegetable oil yield is huge, former soap Foot is only used as acidification oil, rudimentary soap, discarded, causes waste, and pollutes environment.And to plant Thing oil soap stock is that raw material is prepared biodiesel and can be made full use of soap stock, turns waste into wealth, is substantially reduced life The production cost of thing diesel oil, promotes the popularization and application of biodiesel.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of biodiesel, the method is to use Vegetable oil lipoprotein By-product soap (oily) foot of factory's refine is raw material, through concentrate drying, then with methanol at sulfuric acid catalysis Agent carries out ester exchange reaction at low temperature 60-65 DEG C, and soap stock esterification yield reaches 99.5%, finished product yield Height, it is high that finished product obtains purity, and obtains side-product crude glycerine.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of preparation method of biodiesel, it is characterised in that: the method is with the refine of Vegetable oil lipoprotein factory By-product soap stock be raw material, through concentrate drying, then with methanol at sulfuric acid catalyst at low temperature Carrying out ester exchange reaction at 60-65 DEG C, after reaction 60min, esterification yield reaches 99.5%;Methanol with The mol ratio of raw oil is 100: 1, and the ester exchange of acid catalysis production technology two continuous operations of needs is anti- Answering device to react, in reactor 1, methanol is 1: 0.95 with the mol ratio of fatty acid, sulphuric acid The 1-2% that addition is soap stock weight, in reactor 2, methanol with the mol ratio of fatty acid is 1: 1.2, the addition of sulphuric acid is the 1-2% of soap stock weight, generates corresponding fatty acid methyl ester, then warp Washing i.e. obtains biodiesel after drying, and obtain side-product crude glycerine.
The invention have the advantage that technique is simple, Catalysis Rate fast, conversion ratio is high, easy to operate, anti- Between Ying Shi short, to react pollution-free, post processing easy, belongs to green chemistry process.There is reaction condition temperature With, produce the advantages such as waste water is few, product can be easily separated, this process efficient, environmental protection, simultaneously can Reduce equipment investment, reduce production cost.Side-product glycerol and a small amount of soap that vinegar switching phase produces are easy In recycling, there is good industrial prospect.
Detailed description of the invention
A kind of method utilizing oil foot and waste oil preparing biological diesel oil, the method is by Vegetable oil lipoprotein factory essence Refining by-product soap stock be raw material, through concentrate drying, then with methanol at sulfuric acid catalyst at low temperature Carrying out ester exchange reaction at 60-65 DEG C, after reaction 60min, esterification yield reaches 99.5%;Methanol is with former The mol ratio of material oil is 100: 1, and acid catalysis production technology needs the ester exchange reaction of two continuous operations Device reacts, and in reactor 1, methanol is 1: 0.95 with the mol ratio of fatty acid, adding of sulphuric acid Entering the 1-2% that amount is soap stock weight, in reactor 2, methanol is 1: 1.2 with the mol ratio of fatty acid, The addition of sulphuric acid is the 1-2% of soap stock weight, generates corresponding fatty acid methyl ester, more scrubbed dry After i.e. obtain biodiesel, and obtain side-product crude glycerine.
Due to the fact that two reactors of employing, in reactor 1 soap stock excess, in reactor 2 Methanol excess, it is therefore intended that reaction thoroughly, makes soap stock esterification yield be up to 99.5%, and finished product yield is high, It is the highest that finished product obtains purity.
Specifically comprise the following steps that
1) soap stock concentrates;Use Vacuum film evaporation technique, the vacuum level requirements 720 when this technique concentrates More than millimetres of mercury, operate temperature 70-85 DEG C;The soap stock standard obtained is as follows: aqueous less than 1%, Natural flow is kept during color and luster Gartner colorimetric less than 9,20 DEG C;
For ensureing that the water content of finished product, below set quota, need to increase by one before above-mentioned evaporation technology Road predrainage operation;Predrainage uses spiral heater, is passed through the steaming that gauge pressure is 2,000 grams/cm Vapour heats indirectly, carries out under 700 millimetres of mercury vacuum;When the moisture of soap stock is not more than 35%, Fat content is less than 24%, when soap stock content is about 44%, can stop dehydration;After predrainage Concentration soap stock concentrate by above-mentioned requirements;
Concentrator uses soap stock thickener, also referred to as scraper plate thin-film concentrator, is commonly used to process temperature-sensitive Property, high viscosity, high boiling point and foaming substance, its effect is better than other kinds of vaporizer.Scraper plate The heat-transfer effect of membrane evaporator is good, and particularly viscosity is more than the feed liquid of 100 centipoises, its heat transfer system Number declines the least.Both the above equipment is provided by Zhengzhou four-dimension grain and oil equipment and technologies company limited.
2) ester exchange workshop section
Enrichment materials soap stock enters reactor 1, adds adjuvant methanol and catalyst sulfuric acid in this together;Send out Fatty acid methyl ester and glycerol is generated after biochemical reaction;After settlement separate, fatty acid methyl ester enters anti- Answer device 2, add methanol and catalyst sulfuric acid in this together, make responseless material react further with Improve the yield of product;Reactor 2 fatty acid methyl ester out enters scrubbing tower, uses dilute hydrochloric acid at this Aqueous solution washs, to dispose the sodium hydroxide carried secretly in fatty acid methyl ester, afterwards fatty acid methyl Ester methyl ester removal drying section;Reactor scrubbing tower through heavy phase mixture such as settlement separate glycerol, methanol, Enter methanol distillation column tower top after rectification in the lump to obtain the methanol of 99.9% and can return to reactor circulates Use;G & W out at the bottom of tower goes crude glycerine to give process workshop section;
3) methyl ester drying section
The fatty acid methyl ester come by ester exchange workshop section is through one-level exsiccator, secondary drying device, by methyl ester In water evaporates remove;It is dried and carries out under vacuum, fatty acid methyl ester after drying It is biodiesel oil product, pump pressurization sends into finished product basin;
The above is only the preferred embodiment of the present invention, it is noted that for the art For those of ordinary skill, under the premise without departing from the principles of the invention, it is also possible to make some improvement And retouching, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (1)

1. the preparation method of a biodiesel, it is characterised in that: the method is to use plant The by-product soap stock of oils and fats factory refine is raw material, through concentrate drying, then with methanol at sulphuric acid Catalyst carries out ester exchange reaction at low temperature 60-65 DEG C, and after reaction 60min, esterification yield reaches To 99.5%;Methanol is 100: 1 with the mol ratio of raw oil, and acid catalysis production technology needs The transesterification reactor of two continuous operations is reacted, in reactor 1, and methanol and fat The mol ratio of acid is 1: 0.95, and the addition of sulphuric acid is the 1-2% of soap stock weight, in reaction In device 2, methanol is 1: 1.2 with the mol ratio of fatty acid, and the addition of sulphuric acid is soap stock weight The 1-2% of amount, generates corresponding fatty acid methyl ester, more scrubbed i.e. obtains biodiesel after drying.
CN201610270608.5A 2016-04-28 2016-04-28 Method for preparing biodiesel oil Pending CN105950301A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610270608.5A CN105950301A (en) 2016-04-28 2016-04-28 Method for preparing biodiesel oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610270608.5A CN105950301A (en) 2016-04-28 2016-04-28 Method for preparing biodiesel oil

Publications (1)

Publication Number Publication Date
CN105950301A true CN105950301A (en) 2016-09-21

Family

ID=56915492

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610270608.5A Pending CN105950301A (en) 2016-04-28 2016-04-28 Method for preparing biodiesel oil

Country Status (1)

Country Link
CN (1) CN105950301A (en)

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WD01 Invention patent application deemed withdrawn after publication
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Application publication date: 20160921