CN105695106A - Preparation method for biodiesel - Google Patents
Preparation method for biodiesel Download PDFInfo
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- CN105695106A CN105695106A CN201610026895.5A CN201610026895A CN105695106A CN 105695106 A CN105695106 A CN 105695106A CN 201610026895 A CN201610026895 A CN 201610026895A CN 105695106 A CN105695106 A CN 105695106A
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- biodiesel
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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
-
- 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
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
-
- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/12—Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
-
- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
- C10L2290/542—Adsorption of impurities during preparation or upgrading of a fuel
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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
Abstract
The invention discloses a preparation method for biodiesel. The preparation method comprises the following steps that symplocos paniculata oil is pretreated by adding a diatomaceous earth adsorbent to obtain pure symplocos paniculata oil; the pure symplocos paniculata oil, methyl alcohol and a magnetic nanocatalyst are added into a reaction kettle for an esterification reaction according to the weight ratio of 100:(30-50):(0.5-1.0); crude biodiesel separation and purification are performed, and then the biodiesel can be obtained. According to the preparation method, the magnetic nanocatalyst is introduced into the esterification reaction, the catalytic efficiency is high, the catalytic effect is significant, therefore, the reaction time is shortened, and the biodiesel yield is increased; on the other hand, the magnetic nanocatalyst can be conveniently and quickly separated and recycled according to an external magnetic field and can be cyclically utilized for multiple times. The method has the advantages of being simple in preparation technology, economical in energy, environmentally friendly, short in reaction time, high in yield and product purity and the like and has the very good social benefit, ecological benefit and economic benefit, and scale and industrialized production is easy to achieve.
Description
Technical field
The present invention relates to biomass energy technology field, the preparation method of especially a kind of biodiesel。
Background technology
Present Global oil demand constantly increases the contradiction gradually exhausted with fossil energy order; energy resource supply situation is more and more nervous; international market crude oil price continues to sharp rise; the diversification of the energy, renewableization and clean the inevitable choice becoming human social development; exploitation biomass energy is one of direction solving global energy crisis, and the biodiesel as novel alternative energy 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., and the water plant oils and fats such as Wild oil plant and engineering microalgae and animal oil, food garbage wet goods are the reproducibility diesel fuel of the replaced petrifaction diesel that raw oil is made by ester exchange or thermochemical processes。
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 biological degradability of biodiesel is higher than common diesel, biodegradation can be realized under natural situation, reduce 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 the discharge of sulfur dioxide and sulfide is low；Without the aromatic series alkane that environment can be polluted in biodiesel, thus human body is damaged lower than diesel oil by waste gas。(3) good greasy property, makes the abrasion of injection pump, engine cylinder-body and connecting rod reduce, long service life。(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 extend the service life of catalyst and 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, the waste oil in catering trade, waste oil even can be utilized as raw material, it is possible to accomplish to reclaim the advantages such as the purpose that turns waste into wealth of rubbish。
China is the country that petroleum resources are relatively poor; but woody oleiferous plants resource and abundant; along with to the research of energy woody oleiferous plants crop, the deepening continuously of development and utilization; biomass energy is huge in China's development potentiality; development woody oleiferous plants Biodiesel not only contributes to solve oil replacement, ecological environmental protection and agriculture, rural areas and farmers problem, also can for bring new development opportunity for China's forestry industry。Symplocoris Paniculatae (Symplocospaniculata (Thunb.) Miq), has another name called ash seed tree wooden, broken, Wu Yu, son wood, grid bavin etc., belongs to machaka or dungarunga for Symplocaceae mountain vitriol。The weather of happiness warm and moist and deep fertile sand loam, like light also slightly resistance to shade, deep-rootedness seeds, strong adaptability, resist cold, drought-resistant barren-resistant。For China originate in seeds, have a very wide distribution, north from Liaoning, reach Sichuan, Yunnan, Fujian, Taiwan in the south, mountain region, North China is common wild。In Symplocoris Paniculatae blade, every 100g contains Vc22.36mg and abundant mineral, containing crude protein 12.78%～13.85%, crude fibre 16.25%, also has 17 seed amino acids, and content is not low, and the highest glutamic acid reaches 3.43mg/100g；Symplocoris Paniculatae seed oil-containing is about 30%。Two kinds of unsaturated fatty acids in sandal oil, namely oleic acid and linoleic acid content are up to about 85%。Development potentiality accordingly, as biodiesel raw material is very big。Main method currently with Symplocoris Paniculatae biodiesel is ester-interchange method, but traditional ester-interchange method mostly exists that catalytic efficiency is low, yield poorly, color and luster is deep, apt to deteriorate, response time length, etching apparatus, complex process, reaction temperature high, energy consumption is relatively big, easily cause secondary pollution and byproduct losses, the shortcoming such as relatively costly。
Summary of the invention
The present invention is directed to tradition Production of Biodiesel Via Transesterification Method Problems existing, it is provided that the preparation method of a kind of biodiesel。The present invention with magnetic nano solid acid for catalyst, not only not etching apparatus, moreover it is possible to improve catalytic efficiency significantly, the response time can be shortened and reduce energy consumption etc.。
For realizing object above, the present invention is achieved through the following technical solutions:
The preparation method of a kind of biodiesel, comprises the following steps:
1. pretreatment of raw material: adding weight ratio in sandal oil is the diatomite adsorbant of 0.8-1.2%, is stirring 20-30min under 120-150r/min at rotating speed, can obtain pure sandal oil；
2. esterification: pure sandal oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:30-50:0.5-1.0, temperature be 50-55 DEG C, mixing speed be under 120-180r/min, carry out esterification 35-45min, obtain esterification products；
3. separating biodiesel crude product: be centrifugal 8-12min under 500-1000r/min by esterification products at rotating speed, after staticly settling, upper liquid 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, add the mixed adsorbent formed with bentonite and polyvinyl lactam, its addition is the 1.2-2.0% of biodiesel crude product weight, under rotating speed 150-180r/min, stir 5-8min, biodiesel oil product can be obtained。
The above magnetic nano-catalyst includes B2O3-Fe3O4、ZrO2-Fe3O4And Al2O3-Fe3O4。
The mixed adsorbent of the above bentonite and polyvinyl lactam composition is made up of 30-40% bentonite and 60-70% polyvinyl lactam。
Compared with prior art, advantages of the present invention and beneficial effect:
1, the present invention utilizes Renewable resource sandal oil to prepare biodiesel, can effectively solve Present Global energy crisis and problem of environmental pollution, and the biodiesel of production not only quality obtains bigger raising, and productivity is also promoted to about 50% from existing about 60%。
2, magnetic nano-catalyst is incorporated in the production of biodiesel by the present invention, wherein magnetic nano-catalyst has the features such as reaction interface is big, surface area is big, resistance to mass tranfer is little, reaction condition is gentle, active height, activity stability are good, catalytic efficiency is high in the esterification reaction, catalytic effect is notable to make it, thus shortening the response time and improving the productivity of biodiesel。Magnetic nano-catalyst can facilitate according to exterior magnetic field on the other hand, it is isolated rapidly, reclaims, can recycled for multiple times, overcome non magnetic nanocatalyst difficulty to reclaim, shortcoming that cost is high, to alleviating environmental pollution, improve enterprise's productivity effect, realize resources circulation and efficiently utilize significant。
3, the present invention adopts absorption method to purify biodiesel, simple to operate, cost is low, can effectively solve that power consumption is big and " three wastes " emission problem；Select the mixture of bentonite and polyvinyl lactam composition as adsorbent, it is possible not only to adsorb the impurity such as the free acid of biodiesel, methanol, glycerol, glyceride very well, also there is good dehydrating effect simultaneously, it is possible to overcome biodiesel color and luster deep, perishable and conventional distil-lation method exists the problem such as complex process, big, the response time length of power consumption。
4, sandal oil was first carried out pretreatment with kieselguhr by the present invention before esterification, it is possible to the impurity of absorption sandal oil and part free acid so that the soap that esterification reaction process produces is few, alleviates the difficulty of follow-up refining coarse biodiesel。
5, the inventive method has that preparation technology is simple, energy-conserving and environment-protective, catalytic efficiency is high, the response time is short, productivity is high, product purity advantages of higher, has good social efficiency, ecological benefits and economic benefit, it is easy to realize scale, industrialization produces。
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 FeCl3Being dissolved in distilled water water, pass into nitrogen, stir under 1000r/min rotating speed, dropwise adding ammonia to pH value is 12；Control again temperature be 75 DEG C, rotating speed be 350r/min, stir 2.5h, after reaction, be cooled to room temperature, utilize Magnetitum adsorption to collect Fe3O4Microgranule, cleans to neutral with distilled water, is vacuum drying 3h at 75 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 31nm。
b.Al2O3-Fe3O4The preparation of magnetic nano-catalyst: be the magnetic Fe of 1:20 by mass ratio3O4Nano microsphere and aluminum sulfate solution add to ultrasonic stirrer, add and magnetic Fe3O4Nano microsphere mass ratio is the ethanol of 1:40; be 450r/min, temperature at rotating speed it is at 65 DEG C; being added dropwise over ammonia to pH is 12; after ultrasonic agitation 3h; the product of gained is through Magneto separate, then cleans 8 times with distilled water, is 75 DEG C of dry 5h with microwave; last roasting 3h under 500 DEG C and nitrogen protection, can be prepared by Al2O3-Fe3O4Magnetic nano-catalyst。
The preparation method of a kind of biodiesel, comprises the following steps:
1. pretreatment of raw material: add the diatomite adsorbant of 0.8g in 100g sandal oil, is stirring 30min under 120r/min at rotating speed, can obtain pure sandal oil；
2. esterification: pure sandal oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:30:1.0, temperature be 50 DEG C, mixing speed be under 120r/min, carry out esterification 45min, obtain esterification products；
3. separating biodiesel crude product: be centrifugal 12min under 500r/min by esterification products at rotating speed, after staticly settling, upper liquid separated with subnatant, upper liquid is biodiesel crude product, and lower floor is glycerol；
4. purify biodiesel: 96.14g biodiesel crude product obtained above is added to agitator, add the mixed adsorbent 1.2g formed with 35% bentonite and 65% polyvinyl lactam, under rotating speed 150r/min, stir 8min, biodiesel oil product 91.12g can be obtained。
Embodiment 2
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 FeCl3Being dissolved in distilled water water, pass into nitrogen, stir under 700r/min rotating speed, dropwise adding ammonia to pH value is 11；Control again temperature be 70 DEG C, rotating speed be 300r/min, stir 3h, after reaction, be cooled to room temperature, utilize Magnetitum adsorption to collect Fe3O4Microgranule, cleans to neutral with distilled water, is vacuum drying 3h at 70 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 48nm。
b.B2O3-Fe3O4The preparation of magnetic nano-catalyst: be the magnetic Fe of 1:8 by mass ratio3O4Nano microsphere and Boron Nitride solution add to ultrasonic stirrer, add and magnetic Fe3O4Nano microsphere mass ratio is the ethanol of 1:25; be 350r/min, temperature at rotating speed it is at 60 DEG C; being added dropwise over ammonia to pH is 10; after ultrasonic agitation 3h; the product of gained is through Magneto separate, then cleans 7 times with distilled water, is 70 DEG C of dry 8h with microwave; last roasting 2h under 500 DEG C and nitrogen protection, can be prepared by B2O3-Fe3O4Magnetic nano-catalyst。
The preparation method of a kind of biodiesel, comprises the following steps:
1. pretreatment of raw material: add the diatomite adsorbant of 1.0g in 100g sandal oil, is stirring 25min under 130r/min at rotating speed, can obtain pure sandal oil；
2. esterification: pure sandal oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:40:0.7, temperature be 52 DEG C, mixing speed be under 150r/min, carry out esterification 40min, obtain esterification products；
3. separating biodiesel crude product: be centrifugal 10min under 800r/min by esterification products at rotating speed, after staticly settling, upper liquid separated with subnatant, upper liquid is biodiesel crude product, and lower floor is glycerol；
4. purify biodiesel: 97.13g biodiesel crude product obtained above is added to agitator, add the mixed adsorbent 1.5g formed with 45% bentonite and 55% polyvinyl lactam, under rotating speed 180r/min, stir 5min, biodiesel oil product 90.65g can be obtained。
Embodiment 3
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 FeCl3Being dissolved in distilled water water, pass into 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 300r/min, stir 2.5h, after reaction, be cooled to room temperature, utilize Magnetitum adsorption to collect Fe3O4Microgranule, cleans to neutral with distilled water, is vacuum drying 2h at 80 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 39nm。
b.ZrO2-Fe3O4The preparation of magnetic nano-catalyst: magnetic Fe_3O_4 Nano microsphere and zirconium nitrate solution that mass ratio is 1:12 are added to ultrasonic stirrer, adds and magnetic Fe3O4Nano microsphere mass ratio is the ethanol of 1:25; be 400r/min, temperature at rotating speed it is at 63 DEG C; being added dropwise over ammonia to pH is 11; after ultrasonic agitation 3.5h; the product of gained is through Magneto separate, then cleans 7 times with distilled water, is 65 DEG C of dry 5h with microwave; last roasting 2h under 400 DEG C and nitrogen protection, can be prepared by .ZrO2-Fe3O4Magnetic nano-catalyst。
The preparation method of a kind of biodiesel, comprises the following steps:
1. pretreatment of raw material: add the diatomite adsorbant of 1.2g in 100g sandal oil, is stirring 20min under 150r/min at rotating speed, can obtain pure sandal oil；
2. esterification: pure sandal oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:50:0.5, temperature be 55 DEG C, mixing speed be under 180r/min, carry out esterification 35min, obtain esterification products；
3. separating biodiesel crude product: be centrifugal 8min under 1000r/min by esterification products at rotating speed, after staticly settling, upper liquid separated with subnatant, upper liquid is biodiesel crude product, and lower floor is glycerol；
4. purify biodiesel: 97.56g biodiesel crude product obtained above is added to agitator, add the mixed adsorbent 1.8g formed with 55% bentonite and 45% polyvinyl lactam, under rotating speed 160r/min, stir 6min, biodiesel oil product 91.93g can be obtained。
Claims (3)
1. the preparation method of a biodiesel, it is characterised in that comprise the following steps:
(1) pretreatment of raw material
Adding weight ratio in sandal oil is the diatomite adsorbant of 0.8-1.2%, is stirring 20-30min under 120-150r/min at rotating speed, can obtain pure sandal oil；
(2) esterification
Pure sandal oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:30-50:0.5-1.0, temperature be 50-55 DEG C, mixing speed be under 120-180r/min, carry out esterification 35-45min, obtain esterification products；
(3) biodiesel crude product is separated
Being centrifugal 8-12min under 500-1000r/min by esterification products at rotating speed, after staticly settling, upper liquid separated with subnatant, upper liquid is biodiesel crude product, and lower floor is glycerol；
(4) biodiesel is purified
Biodiesel crude product obtained above is added to agitator, add the mixed adsorbent formed with bentonite and polyvinyl lactam, its addition is the 1.2-2.0% of biodiesel crude product weight, stirs 5-8min, can obtain biodiesel oil product under rotating speed 150-180r/min。
2. the preparation method of a kind of biodiesel according to claim 1, it is characterised in that: described magnetic nano-catalyst includes B2O3-Fe3O4、ZrO2-Fe3O4And Al2O3-Fe3O4。
3. the preparation method of a kind of biodiesel according to claim 1 or claim 2, it is characterised in that: the mixed adsorbent of described bentonite and polyvinyl lactam composition is made up of 35-55% bentonite and 45-65% polyvinyl lactam。
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