CN101293205B - Magnetic solid base catalyst for biological diesel oil production and method for producing the same - Google Patents

Magnetic solid base catalyst for biological diesel oil production and method for producing the same Download PDF

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Publication number
CN101293205B
CN101293205B CN200810047999XA CN200810047999A CN101293205B CN 101293205 B CN101293205 B CN 101293205B CN 200810047999X A CN200810047999X A CN 200810047999XA CN 200810047999 A CN200810047999 A CN 200810047999A CN 101293205 B CN101293205 B CN 101293205B
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magnetic
solid base
biodiesel
base catalyst
catalyst
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CN101293205A (en
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黄凤洪
郭萍梅
李文林
杨湄
黄庆德
夏伏建
刘昌盛
万楚筠
钮琰星
邓乾春
程小英
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Oil Crops Research Institute of Chinese Academy of Agriculture Sciences
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Oil Crops Research Institute of Chinese Academy of Agriculture Sciences
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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
    • 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

Abstract

The present invention relates to a magnetic solid alkali catalyst used in biological diesel production and a preparation method thereof. The present invention takes carbonyl iron powder, Fe3O4, Ni2O3 and Co2O3 powder as the magnetic matrix and silicate as the active material; adopts ultrasonic and/or mechanical stirring and calcining methods to prepare silicate-coated magnetic solid catalyst with the grain diameter of 20 to 100 meshes. The present invention is applied in the reaction of preparing biological diesel by using stearic exchange; permanent magnet or magnetic field is adopted to achieve the high-efficiency and rapid separation and recovery of the catalyst and the product; the recovered catalyst can be continuously used in biological diesel transformation for 11 to 20 times without any activation treatment; the transformation rate is above 96 percent and the yield rate is above 99 percent; the product quality index is consistent with GB/T 20828-2007. The obtained biological diesel product needs no post treatment such as neutralization and abstersion, etc., thus simplifying the technique, reducing the production cost of the biological diesel and reducing the pollution.

Description

A kind of magnetic solid base catalyst that is used for production of biodiesel and preparation method thereof
Technical field
The present invention relates to a kind of magnetic solid base catalyst that is used for production of biodiesel and preparation method thereof, belong to catalysis material and oil and fat chemical application.
Background technology
Biodiesel is the environment-friendly fuel that a kind of alternative petrifaction diesel uses, its sulfur content is low, aromatic hydrocarbon content is few, the oxygen content height, the flash-point height, discharge amount of exhaust gas is few, compare with other alternative fuel such as natural gas, liquefied petroleum gas, ethanol etc., substantially do not need existing engine apparatus is changed, the use that can directly act as a fuel can also mix use with mineral diesel with arbitrary proportion as additive.
At present, catalyst system therefor liquid soda acid homogeneous catalyst normally mainly contains the concentrated sulfuric acid, Na0H, KOH etc. in the biodiesel manufacture process.Mainly is that it is cheap with NaOH etc. as catalyst, but also has the post processing complexity, easily causes critical defects such as three-waste pollution environment.
Therefore, the research report of solid catalysis conversion biodiesel is more and more, in existing literature, Chen Wenwei etc. are raw material with the Chinese tallow tree, utilize homemade novel nano magnetic solid catalyst to prepare the Chinese tallow biodiesel, esterification yield reaches more than 96% under the optimum reaction condition, but the serviceability repeatedly of not mentioned catalyst etc.In existing publication, as described in CN1580190A, CN1664072A, CN 1718679, CN101126032, adopt common solid acid, base catalysis to prepare method of bio-diesel oil, can simplify technology, avoid pollution environment.CN 101033406A directly uses preparing biological diesel oil catalyzed by silicate, can reuse 3～5 times.CN1891787A adopts and contains Ni 2O 3, Co 2O 3, Fe 2O 3Etc. magnetic material sintering solid magnetic catalyst catalysis for preparing biodiesel oil together, can under the effect of magnetic field, better separate with the biodiesel of liquid condition, the solid magnetic catalyst of recovery can be used for the next batch reaction after 50 ℃ of calcining 2h regeneration.Therefore, the serviceability repeatedly of catalyst and high efficiente callback utilization are still urgent problem in the present biodiesel solid catalysis transformation technology.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of magnetic solid base catalyst of using production of biodiesel and preparation method thereof at the deficiency of above-mentioned prior art existence, and it has the advantages that the catalyst activity is high, serviceability is good repeatedly, the separation recovery is easy and organic efficiency is high.
The present invention is that to address the above problem the technical scheme that is adopted as follows: by the magnetic matrix be coated on the outer silicate clad of magnetic matrix and form, described magnetic matrix comprises carbonyl iron dust, Fe 3O 4Powder, Ni 2O 3Powder or Co 2O 3Powder.
Press such scheme, described silicate comprises sodium metasilicate or potassium silicate, or the mixture of both arbitrary proportions.
Press such scheme, described Fe 3O 4, Ni 2O 3, Co 2O 3Powder magnetic matrix is a nano particle.
Press such scheme, the particle diameter of described catalyst is 20～100 orders, described Fe 3O 4, Ni 2O 3, Co 2O 3The particle diameter of powder magnetic matrix is less than or equal to 20nm.
Magnetic solid catalyst preparation method's of the present invention technical scheme is: silicate is dissolved in 10～100 ℃, accounts in the water of silicate quality 100～900%, form colloidal sol, the mol ratio of pressing metallic element Fe in Si and the magnetic matrix or Ni or Co added the magnetic matrix in 1: 1～10: 1, carrying out magnetic nuclear disperses, make the magnetic matrix surface coat the silicate clad, then with it under 30～100 ℃ of conditions, behind vacuum drying 0.5～2h, again through 150～800 ℃ of calcining 0.5～5h, cooled catalyst grinds and sieves, and promptly gets particle diameter 20～100 purpose magnetic solid base catalysts.
Press such scheme, the dispersion of described magnetic nuclear adopts mechanical agitation to disperse and/or ultrasonic wave disperses, perhaps mechanical dispersed with stirring ultrasonic wave dispersion more earlier.The condition that mechanical agitation is disperseed is to carry out mechanical agitation and disperse 10～120min at 20～100 ℃, 100～900r/min; The condition that ultrasonic wave disperses is to carry out ultrasonic wave and disperse 10～180min at 20～100 ℃, ultrasonic operating frequency 20～100KHz, ultrasonic power 20～1000W.
The application process of the present invention in preparation production biodiesel is:
Prepared magnetic solid base catalyst and grease, low-carbon alcohols added in the reflux condensate device that band stirs or in magnetic field fluidized bed in proportion react, after reaction finishes, magnetic catalyst absorption is reclaimed, tell the upper phase product with permanent magnet or magnetic field; With upper phase product standing demix, obtain coarse biodiesel and glycerine mutually, coarse biodiesel is distilled out low-carbon alcohols respectively mutually with glycerine, promptly obtain neutral biodiesel and glycerine.
The magnetic catalyst of above-mentioned recovery is used for the reaction of next group biodiesel repeatedly and transforms.
The reaction condition that described grease and low-carbon alcohols, magnetic solid base catalyst react in the reflux condensate device that band stirs is: low-carbon alcohols and grease mol ratio are 3～30: 1, magnetic solid base catalyst particle diameter 20～100 orders, addition is an oil quality 1～20%, 40～100 ℃ of reaction temperatures, stir speed (S.S.) 100～800r/min, reaction time 0.5～5h.
The reaction condition that described grease and low-carbon alcohols, magnetic solid base catalyst react in the fluid bed of band externally-applied magnetic field is: external magnetic field intensity 0.01T～0.05T, magnetic-particle diameter are 20～100 orders, and flow rate of liquid is 1～10 * 10 -2M/s, 20～100 ℃ of reaction temperatures, reaction time 1～5h, low-carbon alcohols and grease mol ratio are 3～30: 1, the magnetic solid base catalyst addition is 1～20% of an oil quality.
Described grease comprises one or more the mixing in Chinese tallow tree Chinese catalpa oil, waste grease, microbial grease, soybean oil, palm oil, cottonseed oil, lard, butter, sheep oil, sesame oil, peanut oil, the rapeseed oil.
Described low-carbon alcohols is methyl alcohol, ethanol, propyl alcohol, butanols, or both mixing arbitrarily, the low-carbon alcohols that steams recycling use again.
The invention has the beneficial effects as follows:
1, compares with common solid catalyst, adopt the usability repeatedly of the silicate magnetic solid base catalyst of the present invention's preparation to be greatly enhanced, without any activation processing, can use repeatedly 11～20 times, the biodiesel conversion ratio is still more than 96%, yield is more than 99%, and product quality indicator meets GB/T 20828-2007 standard, has significantly reduced production cost.
2, adopt the catalyst for ester exchange reaction of magnetic solid base as vegetable and animals oils and low-carbon alcohols, post catalyst reaction can separate recovery fast with externally-applied magnetic field, the realization catalyst efficiently separates fast with product, simplify technology, solved problems such as common solid base catalyst difficult separation and recycling.
3, adopt magnetic solid base catalyst, the product that obtains does not need post processings such as neutralization, washing, and without sewage discharge has solved traditional liquid-phase catalyst and prepared problems such as the corrosivity to equipment, the post processing of biodiesel existence is loaded down with trivial details, contaminated environment.
The specific embodiment
Below describe embodiments of the invention in detail.
Embodiment 1:
Raw material: sodium metasilicate, nanometer Fe 3O 4, cottonseed oil, methyl alcohol;
Take by weighing the 20g sodium metasilicate, it is dissolved in 50 ℃ the 20g water, the mol ratio of pressing Si and Fe adds magnetic nuclear Fe at 2: 1 3O 4Earlier carry out mechanical agitation and disperse 20min, under 40 ℃, ultrasonic operating frequency 28KHz, ultrasonic power 75W condition, carry out ultrasonic wave then and disperse 40min, make the magnetic matrix surface coat the silicate active material at 50 ℃, 400r/min, 40 ℃ of vacuum drying 1h, 200 ℃ of calcining 2.5h.Cooled catalyst grinds and sieves, and gets particle diameter 40 purpose magnetic solid base catalysts.
By weight 200g cottonseed oil and 60g methyl alcohol are added in the 500mL there-necked flask, add the above-mentioned prepared catalyst of 20g again, be heated to 70 ℃, stir speed (S.S.) 300r/min, back flow reaction 1.5 hours, stop reaction, with Nd-Fe-B permanent magnet catalyst absorption is reclaimed, tell upper phase, standing demix obtains coarse biodiesel and crude glycerine, decompression distillation is removed methyl alcohol and is obtained the 199.8g biodiesel, yield 99.9% obtains glycerine 19.8g, and the biodiesel conversion ratio that adopts gas Chromatographic Determination to obtain is 97.2%.
The cottonseed oil and the methyl alcohol that continue to add same amount in there-necked flask carry out the next batch reaction, and step is the same, and catalyst uses 12 times so repeatedly, estimates each biodiesel conversion ratio, and its catalytic activity is still more than 96% after 12 times.The result is as follows.
Table 1 magnetic solid catalyst catalysis cottonseed oil prepares the usability repeatedly of biodiesel
Figure GSB00000234037800041
The assay method and the measurement result of every quality index see Table 2, and GB/T 20828-2007 all is up to state standards.
Embodiment 2:
Raw material: potassium silicate, carbonyl iron dust, acid value is the waste grease of 19mgKOH/g, methyl alcohol;
Take by weighing the 20g potassium silicate, it is dissolved in 50 ℃ the 30g water, the mol ratio of pressing Si and Fe adds magnetic nuclear carbonyl iron dust at 1.5: 1, carry out mechanical agitation at 50 ℃, 400r/min and disperse 20min, make the magnetic matrix surface coat the silicate active material, 50 ℃ of vacuum drying 1h calcine 3h for 400 ℃ then.Cooled catalyst grinds and sieves, and gets particle diameter 20 purpose magnetic solid base catalysts.
With acid value is the abandoned oil process removal of impurities of 19mgKOH/g, dewater, after the pre-treatments such as depickling, obtain impurity content less than 0.1%, acid value is less than the raw oil material of 3mgKOH/g, then pretreated abandoned oil of 200g and 60g methyl alcohol are added in the 500mL there-necked flask, the magnetic solid base catalyst that adds the above-mentioned preparation of 10g again, be heated to 70 ℃, stir speed (S.S.) 400r/min, after the back flow reaction 2 hours, stop reaction, with Nd-Fe-B permanent magnet catalyst absorption is reclaimed, tell upper phase, standing demix obtains coarse biodiesel and crude glycerine, decompression distillation is removed methyl alcohol and is obtained the 199.5g biodiesel, yield 99.6% obtains glycerine 19.6g, and the biodiesel conversion ratio that adopts gas Chromatographic Determination to obtain is 96.1%.
Continue to add pretreated abandoned oil of same amount and methyl alcohol in there-necked flask, carry out the next batch reaction, step is the same, and after catalyst used 11 times so repeatedly, its catalytic activity was still more than 96%.
The assay method and the measurement result that obtain every quality index of biodiesel product see Table 2, and GB/T 20828-2007 all is up to state standards.
Embodiment 3:
Raw material: potassium silicate, sodium metasilicate, nano Co 2O 3, the soybean oil that comes unstuck, methyl alcohol;
Take by weighing 10g potassium silicate and sodium metasilicate respectively, it is dissolved in 50 ℃ the 50g water, the mol ratio of pressing Si and Co adds magnetic nuclear Co at 3: 1 2O 3, under 40 ℃, ultrasonic operating frequency 45KHz, ultrasonic power 75W condition, carry out ultrasonic wave and disperse 30min, make the magnetic matrix surface coat the silicate active material, 50 ℃ of vacuum drying 1h then, 350 ℃ of calcining 3h.Cooled catalyst grinds and sieves, and gets particle diameter 60 purpose magnetic solid base catalysts.
By weight 200g soya-bean oil and 60g methyl alcohol are added in the 500mL fluidized bed body, add the magnetic solid catalyst of the above-mentioned preparation of 20g again, outside magnetic field intensity is that 0.03T and flow rate of liquid are 5.6 * 10 -2Under the condition of m/s, reacted 2 hours, and after reaction finishes, catalyst absorption was reclaimed with external magnetic field, tell upper phase, standing demix obtains coarse biodiesel and crude glycerine, and methyl alcohol is removed in decompression distillation, obtain the 199.8g biodiesel, yield 99.9% obtains glycerine 19.7g, and the biodiesel conversion ratio that adopts gas Chromatographic Determination to obtain is 96.7%.
Continue to add the come unstuck soybean oil and the methyl alcohol of same amount in fluid bed, carry out the next batch reaction, step is the same, and after catalyst used 15 times so repeatedly, its catalytic activity was still more than 96%.
The assay method and the measurement result that obtain every quality index of biodiesel product see Table 2, and GB/T 20828-2007 all is up to state standards.
Embodiment 4:
Raw material: potassium silicate, nanometer Ni 2O 3, palm oil, methyl alcohol;
Take by weighing the 20g potassium silicate, it is dissolved in 50 ℃ the 30g water, the mol ratio of pressing Si and Ni adds magnetic nuclear Ni at 3.5: 1 2O 3, carrying out the churned mechanically while at 40 ℃, 200r/min, the ultrasonic wave that carries out frequency 45KHz, power 75W disperses, and jitter time 40min makes the magnetic matrix surface coat the silicate active material, 50 ℃ of vacuum drying 1h then, 200 ℃ of calcining 3h.Cooled catalyst grinds and sieves, and gets particle diameter 40 purpose magnetic solid base catalysts.
By weight 200g palm oil and 60g methyl alcohol are added in the 500mL there-necked flask, add the above-mentioned magnetic solid catalyst of 10g again, be heated to 70 ℃, under the stirring and refluxing condition, reacted 1 hour, stop reaction, with Nd-Fe-B permanent magnet catalyst absorption is reclaimed, tell upper phase, standing separation obtains coarse biodiesel and crude glycerine, decompression distillation is removed methyl alcohol and is obtained the 198.9g biodiesel, yield 99.5% obtains glycerine 19.7g, and the biodiesel conversion ratio that adopts gas Chromatographic Determination to obtain is 96.7%.
Continue to add the palm oil and the methyl alcohol of same amount in there-necked flask, carry out the next batch reaction, step is the same, and after catalyst used 13 times so repeatedly, its catalytic activity was still more than 96%.
The assay method and the measurement result that obtain every quality index of biodiesel product see Table 2, and GB/T 20828-2007 all is up to state standards.
Each raw material biodiesel quality index that table 2 is measured with reference to standard GB/T 20828-2007

Claims (9)

1. a magnetic solid base catalyst that is used for production of biodiesel is characterized in that by the magnetic matrix and is coated on the outer silicate clad of magnetic matrix forming, and described magnetic matrix comprises carbonyl iron dust, Fe 3O 4Powder, Ni 2O 3Powder or Co 2O 3Powder; Described silicate comprises the mixture of sodium metasilicate, potassium silicate or both arbitrary proportions; Described magnetic solid base catalyst is prepared from by following method: silicate is dissolved in 10～100 ℃, accounts in the water of silicate quality 100～900%, form colloidal sol, the mol ratio of pressing metallic element Fe in Si and the magnetic matrix or Ni or Co added the magnetic matrix in 1: 1～10: 1, carrying out magnetic nuclear disperses, make the magnetic matrix surface coat the silicate clad, then with it under 30～100 ℃ of conditions, behind vacuum drying 0.5～2h, again through 150～800 ℃ of calcining 0.5～5h, cooled catalyst grinds and sieves, and promptly gets particle diameter 20～100 purpose magnetic solid base catalysts.
2. the magnetic solid base catalyst that is used for production of biodiesel according to claim 1 is characterized in that described Fe 3O 4, Ni 2O 3, Co 2O 3Powder magnetic matrix is a nano particle.
3. the magnetic solid base catalyst that is used for production of biodiesel according to claim 1 and 2, the particle diameter that it is characterized in that described catalyst is 20～100 orders, described Fe 3O 4, Ni 2O 3, Co 2O 3The particle diameter of powder magnetic matrix is less than or equal to 20nm.
4. described magnetic solid base catalyst preparation method who is used for production of biodiesel of claim 1, it is characterized in that silicate is dissolved in 10～100 ℃, account in the water of silicate quality 100～900%, form colloidal sol, the mol ratio of pressing metallic element Fe in Si and the magnetic matrix or Ni or Co added the magnetic matrix in 1: 1～10: 1, carrying out magnetic nuclear disperses, make the magnetic matrix surface coat the silicate clad, then with it under 30～100 ℃ of conditions, behind vacuum drying 0.5～2h, again through 150～800 ℃ of calcining 0.5～5h, cooled catalyst grinds and sieves, and promptly gets particle diameter 20～100 purpose magnetic solid base catalysts.
5. the magnetic solid base catalyst preparation method who is used for production of biodiesel according to claim 4 is characterized in that the dispersion of described magnetic nuclear adopts mechanical agitation to disperse and/or ultrasonic wave disperses, perhaps mechanical dispersed with stirring ultrasonic wave dispersion more earlier.
6. the magnetic solid base catalyst preparation method who is used for production of biodiesel according to claim 5 is characterized in that condition that mechanical agitation is disperseed is to carry out mechanical agitation and disperse 10～120min at 20～100 ℃, 100～900r/min; The condition that ultrasonic wave disperses is to carry out ultrasonic wave and disperse 10～180min at 20～100 ℃, ultrasonic operating frequency 20～100KHz, ultrasonic power 20～1000W.
7. the application of the described magnetic solid base catalyst of claim 1 in production of biodiesel, it is characterized in that prepared magnetic solid base catalyst and grease, low-carbon alcohols added in the reflux condensate device that band stirs or in magnetic field fluidized bed in proportion and react, after reaction finishes, with permanent magnet or magnetic field magnetic catalyst absorption is reclaimed, tell the upper phase product; With upper phase product standing demix, obtain coarse biodiesel and glycerine mutually, coarse biodiesel is distilled out low-carbon alcohols respectively mutually with glycerine, promptly obtain neutral biodiesel and glycerine.
8. the application of magnetic solid base catalyst according to claim 7 in production of biodiesel, it is characterized in that the reaction condition that described grease and low-carbon alcohols, magnetic solid base catalyst react in the reflux condensate device that band stirs is: low-carbon alcohols and grease mol ratio are 3～30: 1, the magnetic solid base catalyst addition is an oil quality 1～20%, 40～100 ℃ of reaction temperatures, stir speed (S.S.) 100～800r/min, reaction time 0.5～5h.
9. the application of magnetic solid base catalyst according to claim 7 in production of biodiesel, it is characterized in that the reaction condition that described grease and low-carbon alcohols, magnetic solid base catalyst react in the fluid bed of band externally-applied magnetic field is: external magnetic field intensity 0.01T～0.05T, flow rate of liquid are 1～10 * 10 -2M/s, 20～100 ℃ of reaction temperatures, reaction time 1～5h, low-carbon alcohols and grease mol ratio are 3～30: 1, the magnetic solid base catalyst addition is 1～20% of an oil quality.
CN200810047999XA 2008-06-12 2008-06-12 Magnetic solid base catalyst for biological diesel oil production and method for producing the same Expired - Fee Related CN101293205B (en)

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CN104388195B (en) * 2014-08-08 2017-02-01 内蒙古科技大学 Method for synthesizing fatty acid methyl ester by using magnetic solid base to catalyze in-situ transesterification of navicula sp.
CN104492436B (en) * 2014-12-12 2016-09-07 中国科学院西双版纳热带植物园 A kind of carbon back magnetic solid base catalyst and application thereof
CN105199982B (en) * 2015-09-18 2018-09-28 天津大学 It is a kind of magnetism whole-cell catalyst and preparation method and production biodiesel method
CN106601417B (en) * 2016-12-26 2019-02-05 安徽工业大学 A kind of core-shell structure iron silicon soft magnetism composite iron core and preparation method thereof
CN107469852A (en) * 2017-08-07 2017-12-15 江南大学 A kind of carbon-based magnetic solid base catalyst of biodiesel synthesis and preparation method thereof

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