CN105695107A - Method for preparing biodiesel with euphorbia tirucalli as raw material - Google Patents

Method for preparing biodiesel with euphorbia tirucalli as raw material Download PDF

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Publication number
CN105695107A
CN105695107A CN201610027317.3A CN201610027317A CN105695107A CN 105695107 A CN105695107 A CN 105695107A CN 201610027317 A CN201610027317 A CN 201610027317A CN 105695107 A CN105695107 A CN 105695107A
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China
Prior art keywords
biodiesel
oil
raw material
crude product
pencil tree
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Pending
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CN201610027317.3A
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Chinese (zh)
Inventor
梁杰锋
杨云
蒋小平
李建华
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Guangxi Kuonengba Energy Technology Development Co Ltd
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Guangxi Kuonengba Energy Technology Development Co Ltd
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Priority to CN201610027317.3A priority Critical patent/CN105695107A/en
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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
    • 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)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Microbiology (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a method for preparing biodiesel with euphorbia tirucalli as a raw material. The method includes the following steps that a zeolite molecular sieve adsorbent is added to pretreat euphorbia tirucalli oil, and pure euphorbia tirucalli oil is obtained; the pure euphorbia tirucalli oil, methyl alcohol and a magnetic nanometer catalyst in the weight ratio of 100:(20-40):(0.3-1.5) are added into a reaction kettle to be subjected to an esterification reaction; a biodiesel crude product is separated and purified, and the biodiesel can be obtained. According to the method, as the magnetic nanometer catalyst is led into the esterification reaction, catalytic efficiency is high, the catalytic effect is remarkable, reaction time is shortened, and the yield of the biodiesel is increased; the biodiesel can be conveniently and rapidly separated and recycled through the magnetic nanometer catalyst according to an external magnetic field, and the magnetic nanometer catalyst can be recycled multiple times. The method further has the advantages that the preparing technology is simple, energy is saved, environment protection is achieved, reaction time is short, the yield is high, and the product purity is high, and has quite good social efficiency, ecological benefits and economic benefits, and large-scale production and industrial production can be easily achieved.

Description

A kind of method preparing biodiesel for raw material with pencil tree
Technical field
The present invention relates to biomass energy technology field, especially a kind of method preparing biodiesel for raw material with pencil tree。
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。Pencil tree (EuphorbiatirucalliL.), also known as milk bush, green coral, blue or green Corallium Japonicum Kishinouye, Cycas revoluta, ferrum sieve, Os Draconis tree, angle's rod etc., it it is Euphorbiaceae euphorbia, upright shrub or dungarunga, originating in the Mediterranean littoral in Africa, showing the ground such as Hong Kong, the Penghu Archipelago, Taiwan, Hainan, the U.S., Malaysia, India, Britain and France also has distribution。Containing abundant Hydrocarbon in the milk of pencil tree, and similar to the composition of oil。Research is had to point out that 100kg pencil tree stem just can extract the oil substance of 8kg。Pencil tree branch contains abundant milk, rich in 12 kinds of hydrocarbons, and rich in the Hydrocarbon of the similar petroleum components such as alkene, terpene, sterol in milk, it is possible to directly or be mixed into crude oil with other materials, as fuel oil replacement oil。Therefore pencil tree is a kind of petroleum plant。Can act also as the raw material producing biogas, its biogas output more general twig greenweed height 5-10 times, the development potentiality as biodiesel raw material is very big。Main method currently with pencil tree 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 a kind of method preparing biodiesel for raw material with pencil tree。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:
A kind of method preparing biodiesel for raw material with pencil tree, comprises the following steps:
1. pretreatment of raw material: adding weight ratio in pencil tree oil is the zeolite adsorbent of 1.2-1.5%, is stirring 20-30min under 120-150r/min at rotating speed, can obtain pure pencil tree oil；
2. esterification: pure pencil tree oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:20-40:0.3-1.5, temperature be 60-65 DEG C, mixing speed be under 150-200r/min, carry out esterification 25-35min, obtain esterification products；
3. separating biodiesel crude product: be centrifugal 5-10min under 800-1000r/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 2-4% of biodiesel crude product weight, under rotating speed 80-100r/min, stir 10-20min, biodiesel oil product can be obtained。
The above magnetic nano-catalyst includes B2O3-Fe3O4、ZrO2-Fe3O4And Al2O3-Fe3O4。
The mixed adsorbent of the above magnesium silicate and polyvinyl lactam composition is made up of 30-40% magnesium silicate and 60-70% polyvinyl lactam。
Compared with prior art, advantages of the present invention and beneficial effect:
1, the present invention utilizes Renewable resource pencil tree 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 promoted to about 85%。
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, pencil tree oil was first carried out pretreatment with zeolite molecular sieve by the present invention before esterification, it is possible to the impurity of absorption pencil tree 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 B2O3-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 300r/min rotating speed, dropwise adding ammonia to pH value is 12；Control again temperature be 60 DEG C, rotating speed be 100r/min, stir 1h, 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 65nm。
b.B2O3-Fe3O4The preparation of magnetic nano-catalyst: magnetic Fe_3O_4 Nano microsphere and Boron Nitride solution that mass ratio is 1:9 are added to ultrasonic stirrer; adding with magnetic Fe_3O_4 Nano microsphere mass ratio is the ethanol of 1:20; be 300r/min, temperature at rotating speed it is at 56 DEG C; being added dropwise over ammonia to pH is 12, and after ultrasonic agitation 3h, the product of gained is through Magneto separate; clean 6 times with distilled water again; being 70 DEG C of dry 8h with microwave, finally roasting 2h under 460 DEG C and nitrogen protection, can be prepared by B2O3-Fe3O4Magnetic nano-catalyst。
A kind of method preparing biodiesel for raw material with pencil tree, comprises the following steps:
1. pretreatment of raw material: adding weight in 100kg pencil tree oil is the zeolite adsorbent of 1.2kg, is stirring 30min under 150r/min at rotating speed, can obtain pure pencil tree oil；
2. esterification: pure pencil tree oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:20:1.5, temperature be 65 DEG C, mixing speed be under 200r/min, carry out esterification 25min, 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: the biodiesel crude product of the above-mentioned 99.12kg of obtaining is added to agitator, add the mixed adsorbent 2kg formed with 10% bentonite and 90% polyvinyl lactam, under rotating speed 100r/min, stir 20min, 95.68kg biodiesel oil product can be obtained。
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 FeCl3Being dissolved in distilled water water, pass into nitrogen, stir under 550r/min rotating speed, dropwise adding ammonia to pH value is 12；Control again temperature be 70 DEG C, rotating speed be 120r/min, stir 3.5h, after reaction, be cooled to room temperature, utilize Magnetitum adsorption to collect Fe3O4Microgranule, cleans to neutral with distilled water, is vacuum drying 2h at 75 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 50nm。
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 1:35; be 250r/min, temperature at rotating speed it is at 50 DEG C; being added dropwise over ammonia to pH is 11; after ultrasonic agitation 4h; the product of gained is through Magneto separate, then cleans 6 times with distilled water, is 65 DEG C of dry 10h with microwave; last roasting 3h under 4500 DEG C and nitrogen protection, can be prepared by .ZrO2-Fe3O4Magnetic nano-catalyst。
A kind of method preparing biodiesel for raw material with pencil tree, comprises the following steps:
1. pretreatment of raw material: adding weight in 100kg pencil tree oil is the zeolite adsorbent of 1.3kg, is stirring 25min under 130r/min at rotating speed, can obtain pure pencil tree oil；
2. esterification: pure pencil tree oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:30:1.0, temperature be 60 DEG C, mixing speed be under 170r/min, carry out esterification 30min, obtain esterification products；
3. separating biodiesel crude product: be centrifugal 8min under 900r/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: the biodiesel crude product of the above-mentioned 98.82kg of obtaining is added to agitator, add the mixed adsorbent 3kg formed with 20% bentonite and 80% polyvinyl lactam, under rotating speed 90r/min, stir 15min, 92.68kg biodiesel oil product can be obtained。
Embodiment 3
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 400r/min rotating speed, dropwise adding ammonia to pH value is 12；Control again temperature be 55 DEG C, rotating speed be 200r/min, stir 1.5h, after reaction, be cooled to room temperature, utilize Magnetitum adsorption to collect Fe3O4Microgranule, cleans to neutral with distilled water, is vacuum drying 2h at 75 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 75nm。
b.Al2O3-Fe3O4The preparation of magnetic nano-catalyst: be the magnetic Fe of 1:11 by mass ratio3O4Nano microsphere and aluminum sulfate solution add to ultrasonic stirrer, add and magnetic Fe3O4Nano microsphere mass ratio is the ethanol of 1:30; be 300r/min, temperature at rotating speed it is at 60 DEG C; being added dropwise over ammonia to pH is 12; after ultrasonic agitation 4h; the product of gained is through Magneto separate, then cleans 7 times with distilled water, is 70 DEG C of dry 5.5h with microwave; last roasting 3h under 450 DEG C and nitrogen protection, can be prepared by Al2O3-Fe3O4Magnetic nano-catalyst。
A kind of method preparing biodiesel for raw material with pencil tree, comprises the following steps:
1. pretreatment of raw material: adding weight in 100kg pencil tree oil is the zeolite adsorbent of 1.4kg, is stirring 20min under 120r/min at rotating speed, can obtain pure pencil tree oil；
2. esterification: pure pencil tree oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:40:0.3, temperature be 62 DEG C, mixing speed be under 150r/min, carry out esterification 35min, obtain esterification products；
3. separating biodiesel crude product: be centrifugal 5min 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: the biodiesel crude product of the above-mentioned 98.36kg of obtaining is added to agitator, add the mixed adsorbent 3.5kg formed with 30% bentonite and 70% polyvinyl lactam, under rotating speed 80r/min, stir 10min, 94.12kg biodiesel oil product can be obtained。

Claims (3)

1. the method preparing biodiesel for raw material with pencil tree, it is characterised in that comprise the following steps:
(1) pretreatment of raw material
Adding weight ratio in pencil tree oil is the zeolite adsorbent of 1.2-1.5%, is stirring 20-30min under 120-150r/min at rotating speed, can obtain pure pencil tree oil；
(2) esterification
Pure pencil tree oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:20-40:0.3-1.5, temperature be 60-65 DEG C, mixing speed be under 150-200r/min, carry out esterification 25-35min, obtain esterification products；
(3) biodiesel crude product is separated
Being centrifugal 5-10min under 800-1000r/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 2-4% of biodiesel crude product weight, stirs 10-20min, can obtain biodiesel oil product under rotating speed 80-100r/min。
2. a kind of method preparing biodiesel for raw material with pencil tree according to claim 1, it is characterised in that: described magnetic nano-catalyst includes B2O3-Fe3O4、ZrO2-Fe3O4And Al2O3-Fe3O4。
3. a kind of method preparing biodiesel for raw material with pencil tree 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 10-30% magnesium silicate and 70-90% polyvinyl lactam。
CN201610027317.3A 2016-01-15 2016-01-15 Method for preparing biodiesel with euphorbia tirucalli as raw material Pending CN105695107A (en)

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Publication number Priority date Publication date Assignee Title
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Application publication date: 20160622