CN105969419A - Method for preparing high-quality biodiesel - Google Patents

Method for preparing high-quality biodiesel Download PDF

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CN105969419A
CN105969419A CN201610027162.3A CN201610027162A CN105969419A CN 105969419 A CN105969419 A CN 105969419A CN 201610027162 A CN201610027162 A CN 201610027162A CN 105969419 A CN105969419 A CN 105969419A
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biodiesel
oil
crude product
magnetic nano
rotating speed
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CN105969419B (en
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梁杰锋
杨云
蒋小平
李建华
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Zhongzhou Energy Holding Group Co.,Ltd.
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Guangxi Kuonengba Energy Technology Development Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
    • C10G3/42—Catalytic treatment
    • C10G3/44—Catalytic treatment characterised by the catalyst used
    • C10G3/45—Catalytic treatment characterised by the catalyst used containing iron group metals or compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • 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
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/10—Refining fats or fatty oils by adsorption
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • B01J2523/30—Constitutive chemical elements of heterogeneous catalysts of Group III (IIIA or IIIB) of the Periodic Table
    • B01J2523/305—Boron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • B01J2523/30—Constitutive chemical elements of heterogeneous catalysts of Group III (IIIA or IIIB) of the Periodic Table
    • B01J2523/31—Aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • B01J2523/40—Constitutive chemical elements of heterogeneous catalysts of Group IV (IVA or IVB) of the Periodic Table
    • B01J2523/48—Zirconium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • B01J2523/80—Constitutive chemical elements of heterogeneous catalysts of Group VIII of the Periodic Table
    • B01J2523/84—Metals of the iron group
    • B01J2523/842—Iron
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1011—Biomass
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/70—Catalyst aspects
    • C10G2300/706—Catalytic metal recovery
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    • 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
    • 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

The invention discloses a method for preparing high-quality biodiesel. The method comprises the following steps: adding a zeolite adsorbent for pre-treating cornus wilsoniana oil to obtain the pure cornus wilsoniana oil; adding pure cornus wilsoniana oil, methanol and a magnetic nano catalyst with the weight ratio of 100:15-25:0.8-1.2 in a reaction kettle for an esterification reaction; and separating a biodiesel crude product and purifying the biodiesel crude product to obtain the biodiesel According to the invention, the magnetic nano catalyst is introduced into the esterification reaction, the catalytic efficiency is high, and catalytic effect is obvious, reaction time is shortened, yield of the biodiesel is increased; the magnetic nano catalyst can be conveniently and rapidly separated and recovered according to the outer magnetic field, and enables multiple recycling. The method has the advantages of simple process, energy saving, environmental protection, short reaction time, high yield, and high product purity, and large scale and industrial production can be easily realized.

Description

A kind of preparation method of high-quality biodiesel
Technical field
The present invention relates to biomass energy technology field, the preparation method of a kind of high-quality biodiesel.
Background technology
Present Global oil demand constantly increases the contradiction gradually exhausted with fossil energy mesh, and energy resource supply situation is more come The most nervous, international market crude oil price persistently sharp rises, the diversification of the energy, renewableization and clean and become the mankind The inevitable choice of social development, exploitation biomass energy is one of direction solving global energy crisis, as novel replacement energy The biodiesel in source quickly grows in countries in the world.Biodiesel refers to oil crop such as Semen sojae atricolor, Brassica campestris L, cotton, Petiolus Trachycarpi etc., The water plant oils and fats such as Wild oil plant and engineering microalgae and animal oil, food garbage oil etc. are handed over by ester for raw oil Change or the reproducibility diesel fuel of replaced petrifaction diesel that thermochemical processes is made.
Biodiesel has the performance advantage of following uniqueness: (1) bioenergy is renewable performance: as regenerative resource, Different from petroleum reserves, it is obtained by agricultural and living resources, can supply will not be exhausted, and the biology of biodiesel Degradability is higher than common diesel, can realize biodegradation under natural situation, reduces the pollution to environment for human survival.(2) There is excellent environmental protection characteristic: be mainly manifested in owing in biodiesel, sulfur content is low so that sulfur dioxide and the row of sulfide Lower；Without the aromatic series alkane that can pollute environment in biodiesel, thus waste gas is less than diesel oil to human body infringement. (3) preferable greasy property, makes the abrasion of injection pump, engine cylinder-body and connecting rod reduce, and service life is long.(4) good Fuel performance: biodiesel Cetane number is high so that it is flammability is better than diesel oil, and combustion residue is that subacidity makes catalyst Extend with the service life of engine motor oil.(5) the raw material sources ratio preparing biodiesel is wide: include oil crop, Wild oil plant and alga plant oils and fats and animal oil can serve as raw material, it might even be possible to utilize giving up in catering trade Oil, waste oil as raw material, can accomplish to reclaim the advantages such as the purpose that rubbish turns waste into wealth.
China is the country that petroleum resources are the poorest, but woody oleiferous plants resource and abundant, along with to energy woody oleiferous plants The research of crop, the deepening continuously of development and utilization, biomass energy is huge in China's development potentiality, and development woody oleiferous plants is raw Thing diesel oil industry not only contributes to solve oil replacement, ecological environmental protection and agriculture, rural areas and farmers problem, also can be for China's forestry Industry brings new development opportunity.Wilson dogwood (Swida wilsoniana (Wanger.) Sojak), for deciduous tree, Fructus Corni Como belongs to.It is a kind of preferably multipurpose oil plant seeds.Wilson dogwood happiness light, cold-resistant, like deep, fertile and wet The soil of profit, also can grow at acid soil and limestone soil, and rudiment power is strong, and diseases and insect pests resistance is strong, lasts a long time, exceedes More than 200 years.Wilson dogwood is distributed widely in the Yellow River areas to the south, and integrated distribution is the limestone of the most southwestern various places in the Yangtze river basin District.Wilson dogwood oil is up to 77.68% containing oleic acid and linoleic acid, wherein oleic acid 38.3%, linoleic acid 38.85%, the life produced Thing diesel oil physicochemical property is good；Fruit can be utilized directly to process as raw material simultaneously and produce raw oil, low processing cost, Oil yield is high, can be as biodiesel basis raw oil, and development potentiality is very big.Biodiesel is prepared currently with wilson dogwood Main method is ester-interchange method, but traditional ester-interchange method mostly exists that catalytic efficiency is low, yield poorly, color and luster deeply, easily become Matter, response time length, etching apparatus, complex process, reaction temperature are high, energy consumption is relatively big, easily cause secondary pollution and by-product Thing loss, the shortcoming such as relatively costly.
Summary of the invention
The present invention is directed to the problem that tradition Production of Biodiesel Via Transesterification Method exists, it is provided that the preparation side of a kind of high-quality biodiesel Method.The present invention with magnetic nano solid acid as catalyst, the most not etching apparatus, moreover it is possible to improve catalytic efficiency significantly, can Shorten the response time and reduce energy consumption etc..
For realizing object above, the present invention is to be achieved through the following technical solutions:
The preparation method of a kind of high-quality biodiesel, comprises the following steps:
1. pretreatment of raw material: the zeolite adsorbent that weight ratio is 0.5%-1.0% is added in wilson dogwood oil, at rotating speed is Stir 15-20min under 200-250r/min, i.e. can get pure wilson dogwood oil；
2. esterification: by pure wilson dogwood oil, methanol and magnetic nano-catalyst with weight ratio as 100:15-25:0.8-1.2 Add in reactor, temperature be 60-65 DEG C, mixing speed be under 150-180r/min, carry out esterification 20-30min, Esterification products:
3. separate biodiesel crude product: by esterification products centrifugal 20-30min under rotating speed is 300-500r/min, staticly settle After, upper liquid is separated with subnatant, upper liquid is biodiesel crude product, and lower floor is glycerol:
4. purify biodiesel: biodiesel crude product obtained above is added to agitator, adds with kieselguhr and polyethylene The mixed adsorbent of amide composition, its addition is the 1.5-2.0% of biodiesel crude product weight, at rotating speed 120-150r/min Lower stirring 5-10min, i.e. can get biodiesel oil product.
The above magnetic nano-catalyst includes B2O3-Fe3O4、ZrO2-Fe3O4And Al2O3-Fe3O4。
The mixed adsorbent of the above kieselguhr and polyvinyl lactam composition is by 15-20% magnesium silicate and 80-85% polyethylene Amide forms.
Compared with prior art, advantages of the present invention and beneficial effect:
1, magnetic nano-catalyst is incorporated in the production of biodiesel by the present invention, and wherein magnetic nano-catalyst has instead Answer the features such as interface is big, surface area is big, resistance to mass tranfer is little, reaction condition is gentle, active height, activity stability are good so that Catalytic efficiency is high in the esterification reaction, catalytic effect is notable for it, thus shortens the response time and improve the productivity of biodiesel. On the other hand magnetic nano-catalyst can facilitate according to exterior magnetic field, is isolated rapidly, reclaims, can repeatedly circulate profit With, overcome non magnetic nanocatalyst difficulty to reclaim, shortcoming that cost is high, to alleviate environmental pollution, improve enterprise's productivity effect, Realize resources circulation and efficiently utilize significant.
2, the present invention utilizes Renewable resource wilson dogwood oil to prepare biodiesel, can effectively solve Present Global energy crisis and Problem of environmental pollution, the biodiesel of production not only quality obtains bigger raising, and productivity is also promoted to from existing 70-80% About 90%.
3, the present invention uses absorption method to purify biodiesel, simple to operate, low cost, can effectively solve power consumption big with " three Useless " emission problem；Select the mixture of kieselguhr and polyvinyl lactam composition as adsorbent, be possible not only to adsorb very well life The impurity such as the free acid of thing diesel oil, methanol, glycerol, glyceride, the most also have good dehydrating effect, can overcome life Thing diesel oil color and luster is deep, perishable and conventional distil-lation method exists the problem such as complex process, big, the response time length of power consumption.
4, the present invention first carried out pretreatment with zeolite molecular sieve to shinyleaf yellowhorn oil before esterification, can adsorb wilson dogwood The impurity of oil and part free acid so that the soap that esterification reaction process produces is few, alleviates follow-up refined coarse biodiesel Difficulty.
5, the inventive method have that preparation technology is simple, catalytic efficiency is high, energy-conserving and environment-protective, productivity is high, the response time is short, Product purity advantages of higher, has good social efficiency, ecological benefits and economic benefit, easily realizes scale, industry Metaplasia is produced.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, but is not limited to protection scope of the present invention.
Embodiment 1
Magnetic nano-catalyst used by the present embodiment is Al2O3-Fe3O4.Its preparation method comprises the following steps:
A. magnetic Fe3O4The preparation of Nano microsphere: be the FeCl of 1:2.5 by mass ratio2And FeCl3It is dissolved in distilled water water, Being passed through nitrogen, stir under 1000r/min rotating speed, dropwise adding ammonia to pH value is 12；Controlling temperature again is 75 DEG C, turns Speed is 300r/min, stirs 2h, is cooled to room temperature after reaction, utilizes Magnetitum adsorption to collect Fe3O4Microgranule, with distillation Water cleans to neutral, is vacuum dried 3h, obtains magnetic Fe at temperature is 75 DEG C3O4Nano microsphere, the particle diameter of microsphere is 35nm.
b.Al2O3-Fe3O4The preparation of magnetic nano-catalyst: be the magnetic Fe of 1:10 by mass ratio3O4Nano microsphere and sulfur Acid aluminum solutions adds to ultrasonic stirrer, adds and magnetic Fe3O4Nano microsphere mass ratio is the ethanol of 1:40, at rotating speed Being at 65 DEG C for 450r/min, temperature, being added dropwise over ammonia to pH is 12, after ultrasonic agitation 3h, and the product warp of gained Magneto separate, then clean 8 times with distilled water, it is 75 DEG C of dry 5h with microwave, finally roasting under 500 DEG C and nitrogen are protected 3h, can be prepared by Al2O3-Fe3O4Magnetic nano-catalyst.
The preparation method of a kind of high-quality biodiesel, comprises the following steps:
1. pretreatment of raw material: the zeolite adsorbent of 0.5kg is added in wilson dogwood oil, under rotating speed is 200r/min Stirring 20min, i.e. can get pure wilson dogwood oil；
2. esterification: pure wilson dogwood oil, methanol and magnetic nano-catalyst are added anti-with weight ratio for 100:15:0.8 Answer in still, temperature be 60 DEG C, mixing speed be under 180r/min, carry out esterification 20min, obtain esterification products；
3. separate biodiesel crude product: by esterification products centrifugal 30min under rotating speed is 300r/min, after staticly settling, will Upper liquid separates with subnatant, and upper liquid is biodiesel crude product, and lower floor is glycerol；
4. purify biodiesel: 96.24kg biodiesel crude product obtained above is added to agitator, adds with 15% diatom Soil and the mixed adsorbent 1.5kg of 85% polyvinyl lactam composition, stir 5min under rotating speed 150r/min, i.e. can be given birth to Thing diesel product 89.74kg.
Embodiment 2
Magnetic nano-catalyst used by the present embodiment is ZrO2-Fe3O4.Its preparation method comprises the following steps:
A. magnetic Fe3O4The preparation of Nano microsphere: be the FeCl of 1:3 by mass ratio2And FeCl3It is dissolved in distilled water water, logical Entering nitrogen, stir under 800r/min rotating speed, dropwise adding ammonia to pH value is 11；Control again temperature be 78 DEG C, rotating speed be 250r/min, stirs 1.5h, is cooled to room temperature after reaction, utilizes Magnetitum adsorption to collect Fe3O4Microgranule is clear with distilled water It is washed till neutrality, at temperature is 80 DEG C, is vacuum dried 2h, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 45nm.
b.ZrO2-Fe3O4The preparation of magnetic nano-catalyst: by magnetic Fe_3O_4 Nano microsphere that mass ratio is 1:12 and nitric acid Zirconium solution adds to ultrasonic stirrer, adds and magnetic Fe3O4Nano microsphere mass ratio is the ethanol of 1:25, at rotating speed is 400r/min, temperature are at 63 DEG C, and being added dropwise over ammonia to pH is 11, and after ultrasonic agitation 3.5h, the product of gained is through magnetic Separate, then clean 7 times with distilled water, be 65 DEG C of dry 5h with microwave, finally roasting 2h under 400 DEG C and nitrogen are protected, Can be prepared by .ZrO2-Fe3O4Magnetic nano-catalyst.
The preparation method of a kind of high-quality biodiesel, comprises the following steps:
1. pretreatment of raw material: the zeolite adsorbent of 0.8kg is added in wilson dogwood oil, is 225r/min at rotating speed Lower stirring 18min, i.e. can get pure wilson dogwood oil；
2. esterification: pure wilson dogwood oil, methanol and magnetic nano-catalyst are added anti-with weight ratio for 100:20:1.0 Answer in still, temperature be 62 DEG C, mixing speed be under 160r/min, carry out esterification 25min, obtain esterification products:
3. separate biodiesel crude product: by esterification products centrifugal 25min under rotating speed is 400r/min, after staticly settling, will Upper liquid separates with subnatant, and upper liquid is biodiesel crude product, and lower floor is glycerol:
4. purify biodiesel: 95.87kg biodiesel crude product obtained above is added to agitator, adds with 18% Kieselguhr and the mixed adsorbent 1.7kg of 82% polyvinyl lactam composition, stir 8min under rotating speed 130r/min, To biodiesel oil product 90.62kg.
Embodiment 3
Magnetic nano-catalyst used by the present embodiment is B2O3-Fe3O4.Its preparation method comprises the following steps:
A. magnetic Fe3O4The preparation of Nano microsphere: be the FeCl of 1:3.5 by mass ratio2And FeCl3It is dissolved in distilled water water, Being passed through nitrogen, stir under 700r/min rotating speed, dropwise adding ammonia to pH value is 10；Controlling temperature again is 70 DEG C, rotating speed For 200r/min, stir 3h, after reaction, be cooled to room temperature, utilize Magnetitum adsorption to collect Fe3O4Microgranule, uses distilled water Clean to neutral, at temperature is 70 DEG C, is vacuum dried 3h, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 55nm.
b.B2O3-Fe3O4The preparation of magnetic nano-catalyst: be the magnetic Fe of 1:8 by mass ratio3O4Nano microsphere and Boron Nitride Solution adds to ultrasonic stirrer, adds and magnetic Fe3O4Nano microsphere mass ratio is the ethanol of 1:25, at rotating speed is 350r/min, temperature are at 60 DEG C, and being added dropwise over ammonia to pH is 10, and after ultrasonic agitation 3h, the product of gained divides through magnetic From, then clean 7 times with distilled water, it is 70 DEG C of dry 8h with microwave, finally roasting 2h under 500 DEG C and nitrogen are protected, i.e. B can be prepared2O3-Fe3O4Magnetic nano-catalyst.
The preparation method of a kind of high-quality biodiesel, comprises the following steps:
1. pretreatment of raw material: the zeolite adsorbent of 1.0kg is added in wilson dogwood oil, is 250r/min at rotating speed Lower stirring 15min, i.e. can get pure wilson dogwood oil；
2. esterification: pure wilson dogwood oil, methanol and magnetic nano-catalyst are added anti-with weight ratio for 100:25:1.2 Answer in still, temperature be 65 DEG C, mixing speed be under 150r/min, carry out esterification 30min, obtain esterification products；
3. separate biodiesel crude product: by esterification products centrifugal 20min under rotating speed is 500r/min, after staticly settling, will Upper liquid separates with subnatant, and upper liquid is biodiesel crude product, and lower floor is glycerol；
4. purify biodiesel: 94.75kg biodiesel crude product obtained above is added to agitator, adds with 20% silicon Diatomaceous earth and the mixed adsorbent 2kg of 80% polyvinyl lactam composition, stir 10min under rotating speed 120r/min, the most available Biodiesel oil product 88.69kg.

Claims (3)

1. the preparation method of a high-quality biodiesel, it is characterised in that comprise the following steps:
(1) pretreatment of raw material
The zeolite adsorbent that weight ratio is 0.5-1.0% is added in wilson dogwood oil, stirs under rotating speed is 200-250r/min Mix 15-20min, i.e. can get pure wilson dogwood oil；
(2) esterification
Pure wilson dogwood oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:15-25:0.8-1.2, Temperature be 60-65 DEG C, mixing speed be under 150-180r/min, carry out esterification 20-30min, obtain esterification products:
(3) biodiesel crude product is separated
By esterification products centrifugal 20-30min under rotating speed is 300-500r/min, after staticly settling, upper liquid and subnatant are divided From, upper liquid is biodiesel crude product, and lower floor is glycerol:
(4) biodiesel is purified
Biodiesel crude product obtained above is added to agitator, adds the mixing and absorption formed with kieselguhr and polyvinyl lactam Agent, its addition is the 1.5-2.0% of biodiesel crude product weight, stirs 5-10min under rotating speed 120-150r/min, I.e. can get biodiesel oil product.
A kind of preparation method of high-quality biodiesel, it is characterised in that: described magnetic nano-catalyst Including B2O3-Fe3O4、ZrO2-Fe3O4And Al2O3-Fe3O4。
The preparation method of a kind of high-quality biodiesel the most according to claim 1 or claim 2, it is characterised in that: described kieselguhr is with poly- The mixed adsorbent of ethernamine composition is made up of 15-20% magnesium silicate and 80-85% polyvinyl lactam.
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CN101492603A (en) * 2008-01-23 2009-07-29 华中农业大学 Method for producing biodiesel by using tallowseed oil and special solid catalyst thereof
CN102397777A (en) * 2011-09-29 2012-04-04 中兴能源（湖北）有限公司 Preparation method of activated rice husk ash and application of activated rice husk ash to purification of biodiesel
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CN1891787A (en) * 2005-07-07 2007-01-10 南昌大学 Production technology for preparing biodiesel by solid magnetic catalyst
CN101492603A (en) * 2008-01-23 2009-07-29 华中农业大学 Method for producing biodiesel by using tallowseed oil and special solid catalyst thereof
CN101314721A (en) * 2008-04-14 2008-12-03 田珩 Method for preparing biological diesel oil with rubber seed oil and process thereof
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Publication number Priority date Publication date Assignee Title
CN108707484A (en) * 2018-06-28 2018-10-26 鹿寨知航科技信息服务有限公司 A method of preparing low acid value biodiesel using acidification oil

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