CN105670801A - Method for improving yield of biodiesel - Google Patents
Method for improving yield of biodiesel Download PDFInfo
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- CN105670801A CN105670801A CN201610026948.3A CN201610026948A CN105670801A CN 105670801 A CN105670801 A CN 105670801A CN 201610026948 A CN201610026948 A CN 201610026948A CN 105670801 A CN105670801 A CN 105670801A
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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
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- 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
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Catalysts (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a method for improving yield of biodiesel. The method comprises the following steps: adding a zeolite molecular sieve adsorbent, and carrying out pretreatment for Sapium sebiferum seed oil in order to obtain Sapium sebiferum seed oil; adding Sapium sebiferum seed oil, methanol and a magnetic nano-catalyst according to a weight ratio 100:20-30:1.0-2.0 into a reaction vessel in order to carry out an esterification reaction; and separating a biodiesel crude product and carrying out purification in order to obtain the biodiesel. The magnetic nano-catalyst is introduced into the esterification reaction with high catalysis efficiency and substantial catalysis effects, reaction time is shortened, and yield of biodiesel is increased; on the other hand, the magnetic nano-catalyst can be conveniently and rapidly separated and recycled by means of an exterior magnetic field, and repeated recycling is carried out. The method also has the advantages of simple preparation technology, energy saving, environmental protection, short reaction time, high yield, high product purity, etc.; the method has good social efficiency, ecological benefits, and economic benefits; large scale and industrial production are easy to realize.
Description
Technical field
The present invention relates to biomass energy technology field, especially a kind of method improving biodiesel yield.
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. Cortex Sapii Radicis (Sapiumsebiferum (L.) Roxb.), another name: cured subtree, Chinese tallow tree subtree, haze tallow tree, Aleurites montana, Hong Shu, Euphorbiaceae, sapium, deciduous tree. Cortex Sapii Radicis is stronger to the adaptability of soil, in great soil groups such as red soil, yellow earth, yellowish-brown soil, purple soil, brown earth, from sand to the soil of viscous differing texture, and acid, neutral or subalkaline soil, all can grow, be one of arbor species that salt-resistance is strong, be distributed mainly on each provinces and regions on the south China the Yellow River, north reaches Shaanxi, Gansu, is wherein maximum with Zhejiang. Cortex Sapii Radicis seed oil content is high, and oil yield reaches more than 40%, is one of big xylophyta of China four. Development potentiality accordingly, as biodiesel raw material is very big. Main method currently with Cortex Sapii Radicis seed 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 improving biodiesel yield. 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 improving biodiesel yield, comprises the following steps:
1. pretreatment of raw material: adding weight ratio in Cortex Sapii Radicis seed oil is the zeolite adsorbent of 0.8%-1.5%, is stirring 20-30min under 100-150r/min at rotating speed, can obtain Cortex Sapii Radicis seed oil;
2. esterification: Cortex Sapii Radicis seed oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:20-30:1.0-2.0, temperature be 60-65 DEG C, mixing speed be under 150-250r/min, carry out esterification 15-30min, obtain esterification products;
3. separating biodiesel crude product: be centrifugal 10-15min under 500-800r/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: biodiesel crude product obtained above is added to agitator, add the mixed adsorbent formed with magnesium silicate and polyvinyl lactam, its addition is the 1-3% of biodiesel crude product weight, under rotating speed 100-120r/min, stir 8-12min, 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 Cortex Sapii Radicis seed 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 also can be greatly improved.
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 magnesium silicate 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, Cortex Sapii Radicis seed oil was first carried out pretreatment with zeolite molecular sieve by the present invention before esterification, it is possible to the impurity of absorption Cortex Sapii Radicis seed 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 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 450r/min rotating speed, dropwise adding ammonia to pH value is 11; Control again temperature be 65 DEG C, rotating speed be 120r/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 3h at 80 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 43nm.
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 1:20; 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 7 times with distilled water, is 60 DEG C of dry 10h with microwave; last roasting 3h under 400 DEG C and nitrogen protection, can be prepared by .ZrO2-Fe3O4Magnetic nano-catalyst.
A kind of method improving biodiesel yield, comprises the following steps:
1. pretreatment of raw material: adding weight in Cortex Sapii Radicis seed oil is the zeolite adsorbent of 1.0kg, is stirring 20min under 100r/min at rotating speed, can obtain Cortex Sapii Radicis seed oil;
2. esterification: Cortex Sapii Radicis seed oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:20:1.0, temperature be 60 DEG C, mixing speed be under 150r/min, carry out esterification 30min, obtain esterification products;
3. separating biodiesel crude product: be centrifugal 15min under 600r/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: 96.21kg biodiesel crude product obtained above is added to agitator, add 25% mixed adsorbent formed with magnesium silicate and 75% polyvinyl lactam, its addition 1.5kg, stirs 12min under rotating speed 100r/min, can obtain biodiesel oil product 91.52kg.
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 1:2.5 by mass ratio2And FeCl3Being dissolved in distilled water water, pass into nitrogen, stir under 350r/min rotating speed, dropwise adding ammonia to pH value is 12; Control again temperature be 65 DEG C, rotating speed be 120r/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 3h at 60 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 58nm.
b.B2O3-Fe3O4The preparation of magnetic nano-catalyst: magnetic Fe_3O_4 Nano microsphere and Boron Nitride solution that mass ratio is 1:15 are added to ultrasonic stirrer; adding with magnetic Fe_3O_4 Nano microsphere mass ratio is the ethanol of 1:25; be 300r/min, temperature at rotating speed it is at 55 DEG C; being added dropwise over ammonia to pH is 11, and after ultrasonic agitation 2.5h, the product of gained is through Magneto separate; clean 5 times with distilled water again; being 65 DEG C of dry 6h with microwave, finally roasting 3h under 500 DEG C and nitrogen protection, can be prepared by B2O3-Fe3O4Magnetic nano-catalyst.
A kind of method improving biodiesel yield, comprises the following steps:
1. pretreatment of raw material: adding weight in Cortex Sapii Radicis seed oil is the zeolite adsorbent of 1.2kg, is stirring 25min under 120r/min at rotating speed, can obtain Cortex Sapii Radicis seed oil;
2. esterification: Cortex Sapii Radicis seed oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:25:1.5, temperature be 62 DEG C, mixing speed be under 180r/min, carry out esterification 23min, obtain esterification products;
3. separating biodiesel crude product: be centrifugal 13min under 700r/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: 97.57kg biodiesel crude product obtained above is added to agitator, add 30% mixed adsorbent formed with magnesium silicate and 70% polyvinyl lactam, its addition 2.0kg, stirs 10min under rotating speed 110r/min, can obtain biodiesel oil product 92.32kg.
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 500r/min rotating speed, dropwise adding ammonia to pH value is 12; Control again temperature be 70 DEG C, rotating speed be 150r/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 2h at 70 DEG C in temperature, obtains magnetic Fe3O4Nano microsphere, the particle diameter of microsphere is 65nm.
b.Al2O3-Fe3O4The preparation of magnetic nano-catalyst: be the magnetic Fe of 1:10 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 11; after ultrasonic agitation 4h; the product of gained is through Magneto separate, then cleans 6 times with distilled water, is 60 DEG C of dry 6h with microwave; last roasting 3h under 500 DEG C and nitrogen protection, can be prepared by Al2O3-Fe3O4Magnetic nano-catalyst.
A kind of method improving biodiesel yield, comprises the following steps:
1. pretreatment of raw material: adding weight in Cortex Sapii Radicis seed oil is the zeolite adsorbent of 1.4kg, is stirring 28min under 140r/min at rotating speed, can obtain Cortex Sapii Radicis seed oil;
2. esterification: Cortex Sapii Radicis seed oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:30:1.8, temperature be 64 DEG C, mixing speed be under 230r/min, carry out esterification 16min, obtain esterification products;
3. separating biodiesel crude product: be centrifugal 11min 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: 95.91kg biodiesel crude product obtained above is added to agitator, add 35% mixed adsorbent formed with magnesium silicate and 65% polyvinyl lactam, its addition 2.5kg, stirs 8min under rotating speed 120r/min, can obtain biodiesel oil product 92.78kg.
Claims (3)
1. the method improving biodiesel yield, it is characterised in that comprise the following steps:
(1) pretreatment of raw material
Adding weight ratio in Cortex Sapii Radicis seed oil is the zeolite adsorbent of 0.8%-1.5%, is stirring 20-30min under 100-150r/min at rotating speed, can obtain Cortex Sapii Radicis seed oil;
(2) esterification
Cortex Sapii Radicis seed oil, methanol and magnetic nano-catalyst are added in reactor with weight ratio for 100:20-30:1.0-2.0, temperature be 60-65 DEG C, mixing speed be under 150-250r/min, carry out esterification 15-30min, obtain esterification products;
(3) biodiesel crude product is separated
Being centrifugal 10-15min under 500-800r/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) biodiesel is purified
Biodiesel crude product obtained above is added to agitator, add the mixed adsorbent formed with magnesium silicate and polyvinyl lactam, its addition is the 1-3% of biodiesel crude product weight, stirs 8-12min, can obtain biodiesel oil product under rotating speed 100-120r/min.
2. a kind of method improving biodiesel yield 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 improving biodiesel yield according to claim 1 or claim 2, it is characterised in that: the mixed adsorbent of described magnesium silicate and polyvinyl lactam composition is made up of 25-35% magnesium silicate and 65-75% polyvinyl lactam.
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Citations (3)
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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 |
| CN101812378A (en) * | 2010-03-08 | 2010-08-25 | 中山大学 | Biodiesel and preparation method thereof |
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2016
- 2016-01-15 CN CN201610026948.3A patent/CN105670801A/en active Pending
Patent Citations (3)
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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 |
| CN101812378A (en) * | 2010-03-08 | 2010-08-25 | 中山大学 | Biodiesel and preparation method thereof |
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| 周建伟 等: "《新能源化学》", 31 August 2009, 郑州大学出版社 * |
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Application publication date: 20160615 |