CN101480609A - Method for preparing nano solid base catalyst with nucleocapsid structure for synthesizing biodiesel - Google Patents
Method for preparing nano solid base catalyst with nucleocapsid structure for synthesizing biodiesel Download PDFInfo
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- CN101480609A CN101480609A CNA2009100456526A CN200910045652A CN101480609A CN 101480609 A CN101480609 A CN 101480609A CN A2009100456526 A CNA2009100456526 A CN A2009100456526A CN 200910045652 A CN200910045652 A CN 200910045652A CN 101480609 A CN101480609 A CN 101480609A
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Abstract
The invention discloses a preparation method of a nanometer solid base catalyst with a nuclear shell structure for synthesizing biodiesel, comprising the following steps: (nanometer) oxide particles of which the particle diameter is smaller than 50nm are selected, a suspended disperse system is formed by the oxide particles, a dispersing agent and soluble aluminum salt in ethanol under the condition of ultrasonic oscillation, and then, the water solution of Ca(OH)2 is dropwise added to the disperse system until the pH value ranges from 6 to 8; the ultrasonic oscillation is continuously carried out for at least 30min to obtain suspending liquid, and then, the suspending liquid is filtered by suction, dried, milled and calcined to obtain the nanometer solid base catalyst with the nuclear shell structure, wherein the mass ratio of the (nanometer) oxide particles to the soluble aluminum salt to the dispersing agent is 1 : 0.2 to 0.8 : 0.1 to 0.3. The prepared catalyst has good catalytic effect on grease with a high acid value for synthesizing biodiesel; the preparation method simplifies the preliminary treatment processes of the grease with the high acid value for preparing the biodiesel, and reduces the operating cost.
Description
Technical field
The present invention relates to the solid catalytic material technical field, specifically a kind of preparation method of nano solid base catalyst with nucleocapsid structure of biodiesel synthesis.
Background technology
In recent years, the exploitation of solid base catalyst obtains remarkable progress, and catalyzed by solid base technology has obtained to use in production of biodiesel.Can predict, the solid catalysis technology will replace liquid acid base catalysis technology becomes one of mainstream technology.
In present production of biodiesel technology, the high-acid value grease that contains a large amount of free fatties for acidifying oil, trench wet goods, usually adopt esterification process to carry out preliminary treatment, its main component free fatty fully can be transformed, obtain higher product yield, but cost is to increase many loaded down with trivial details post-processing steps; When the relatively not high grease of preliminary treatment acid number,, transform so must carry out ester exchange because of most of triglycerides fails to change into biodiesel by esterification.Because solid base catalyst is relatively poor to the adaptability of high-acid value grease, cause preparing biological diesel fuel by high-acid-value grease technology all need select esterification technique to reduce acid value of oil and fat, will increase the technology cost undoubtedly.In recent years, nanometer technology is fast-developing and be used widely in the Preparation of Catalyst field, nanocatalyst embodies the property that many conventional yardstick catalyst particles are not had, as nanometer technology being applied in the middle of the preparation of solid base catalyst, then can obtain the solid base catalyst of anti-high-acid value grease, thereby reduce the pre-treating technology step of high-acid value grease, reduce the technology cost.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing nano solid base catalyst with nucleocapsid structure that is used for high-acid value grease raw material biodiesel synthesis, keeping the highly active while, simplify the pre-treating technology step of preparing biological diesel fuel by high-acid-value grease, and then reduce running cost.
The concrete technical scheme that realizes the object of the invention is as follows:
A kind of method for preparing nano solid base catalyst with nucleocapsid structure of biodiesel synthesis, it comprises following concrete steps:
A), choose particle diameter (nanometer) oxide particle below 50nm, add to stir in ethanol or the methyl alcohol and make it form suspension system;
B), in resulting suspension system, add dispersant, and vibration is uniformly dispersed it in ultrasonic wave, forms dispersion;
C), get in the dispersion that aluminum soluble salt is dissolved into step, then with Ca (OH)
2The aqueous solution dropwise adds wherein, reaches 6～8 until pH value, continues sonic oscillation 30min at least, obtains suspension suction filtration, drying, grinding, calcining and obtains nano solid base catalyst with nucleocapsid structure;
Wherein: nano-oxide particles: aluminum soluble salt: the mass ratio of dispersant is 1: 0.2～0.8: 0.1～0.3; Described oxide particle is selected from one or more mixing in the oxide of magnesium, calcium, silicon or aluminium; Described aluminum soluble salt comprises Al
2(SO
4)
3, Al (NO
3)
3, AlCl
3Described dispersant is selected from one or more mixing in poly glycol monomethyl ether, polyethylene glycol (molecular weight 2000～20000), lauryl sodium sulfate, the sldium lauryl sulfate.
The nano core-shell structure solid base catalyst grain graininess of the present invention's preparation has good catalytic activity to high-acid value grease about 80nm.
The specific embodiment
Embodiment 1
Choose the alumina particle 10g of particle diameter below 50nm, add in the 100ml ethanol and stirring, make it form suspension system, add 1g polyethylene glycol (molecular weight 2000), and vibration is uniformly dispersed it in ultrasonic wave; With 2g Al
2(SO
4)
3Be dissolved into dispersion, with Ca (OH)
2The aqueous solution dropwise adds, and measures pH value and stops by 7.0 o'clock dripping, and continues sonic oscillation 30min, obtains suspension suction filtration, drying, grinding, calcining and obtains nano solid base catalyst with nucleocapsid structure.
Embodiment 2
Choose the calcium oxide particle 50g of particle diameter below 50nm, add in the 100ml methyl alcohol and stirring, make it form suspension system, add the 10g lauryl sodium sulfate, and vibration is uniformly dispersed it in ultrasonic wave; With 35g Al (NO
3)
3Be dissolved into dispersion, with Ca (OH)
2The aqueous solution dropwise adds, and measures pH value and stops by 8.0 o'clock dripping, and continues sonic oscillation 30min, obtains suspension suction filtration, drying, grinding, calcining and obtains nano solid base catalyst with nucleocapsid structure.
Embodiment 3
Choose the calcium oxide particle 50g of particle diameter below 50nm, add in the 100ml methyl alcohol and stirring, make it form suspension system, add the 10g poly glycol monomethyl ether, and vibration is uniformly dispersed it in ultrasonic wave; With 35g AlCl
3Be dissolved into dispersion, with Ca (OH)
2The aqueous solution dropwise adds, and measures pH value and stops by 8.0 o'clock dripping, and continues sonic oscillation 30min, obtains suspension suction filtration, drying, grinding, calcining and obtains nano solid base catalyst with nucleocapsid structure.
Embodiment 4
Choose the alumina particle 10g of particle diameter below 50nm, add in the 100ml ethanol and stirring, make it form suspension system, add 1g polyethylene glycol (molecular weight 20000), and vibration is uniformly dispersed it in ultrasonic wave; With 2g Al
2(SO
4)
3Be dissolved into dispersion, with Ca (OH)
2The aqueous solution dropwise adds, and measures pH value and stops by 7.0 o'clock dripping, and continues sonic oscillation 30min, obtains suspension suction filtration, drying, grinding, calcining and obtains nano solid base catalyst with nucleocapsid structure.
Embodiment 5
Choose the alumina particle 10g of particle diameter below 50nm, add in the 100ml ethanol and stirring, make it form suspension system, add the 1g sldium lauryl sulfate, and vibration is uniformly dispersed it in ultrasonic wave; With 2g Al (NO
4)
3Be dissolved into dispersion, with Ca (OH)
2The aqueous solution dropwise adds, and measures pH value and stops by 7.0 o'clock dripping, and continues sonic oscillation 30min, obtains suspension suction filtration, drying, grinding, calcining and obtains nano solid base catalyst with nucleocapsid structure.
Application examples 1
Get the Jatropha curcas oil 100g of acid number 2.0, according to 1: 15 (oil: mol ratio methyl alcohol) of industrial methanol, at 75 ℃, under the normal pressure, prepare nano solid base catalyst with nucleocapsid structure among the embodiment 1 of adding vegetable oil quality 3%, react 4 hours afterproducts and separate, obtain the decompression distillation of biodiesel phase and remove methyl alcohol, obtain the biodiesel product.Fatty acid methyl ester is 95.6% in the employing gas chromatography mensuration biodiesel.
Application examples 2
Get the Jatropha curcas oil 100g of acid number 4.0, according to 1: 15 (oil: mol ratio methyl alcohol) of industrial methanol, at 75 ℃, under the normal pressure, prepare nano solid base catalyst with nucleocapsid structure among the embodiment 2 of adding vegetable oil quality 3%, react 4 hours afterproducts and separate, obtain the decompression distillation of biodiesel phase and remove methyl alcohol, obtain the biodiesel product.Fatty acid methyl ester is 98.2% in the employing gas chromatography mensuration biodiesel.
Claims (1)
1, a kind of method for preparing nano solid base catalyst with nucleocapsid structure of biodiesel synthesis is characterized in that this method comprises following concrete steps:
A), choose particle diameter (nanometer) oxide particle below 50nm, add to stir in ethanol or the methyl alcohol and make it form suspension system;
B), in resulting suspension system, add dispersant, and vibration is uniformly dispersed it in ultrasonic wave, forms dispersion;
C), get in the dispersion that aluminum soluble salt is dissolved into step, then with Ca (OH)
2The aqueous solution dropwise adds wherein, reaches 6～8 until pH value, continues sonic oscillation 30min at least, obtains suspension suction filtration, drying, grinding, calcining and obtains nano solid base catalyst with nucleocapsid structure;
Wherein: nano-oxide particles: aluminum soluble salt: the mass ratio of dispersant is 1: 0.2～0.8: 0.1～0.3; Described oxide particle is selected from one or more mixing in the oxide of magnesium, calcium, silicon or aluminium; Described aluminum soluble salt comprises Al
2(SO
4)
3, Al (NO
3)
3, AlCl
3Described dispersant is selected from one or more mixing in poly glycol monomethyl ether, polyethylene glycol (molecular weight 2000～20000), lauryl sodium sulfate, the sldium lauryl sulfate.
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|---|---|---|---|
| CN2009100456526A CN101480609B (en) | 2009-01-21 | 2009-01-21 | Method for preparing nano solid base catalyst with nucleocapsid structure for synthesizing biodiesel |
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|---|---|---|---|
| CN2009100456526A CN101480609B (en) | 2009-01-21 | 2009-01-21 | Method for preparing nano solid base catalyst with nucleocapsid structure for synthesizing biodiesel |
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| CN101480609B CN101480609B (en) | 2010-08-11 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289236A (en) * | 2014-09-28 | 2015-01-21 | 佛山市天晟隆油脂化工有限公司 | Preparation method of solid base catalyst |
| CN108697149A (en) * | 2016-03-02 | 2018-10-23 | 巴斯夫欧洲公司 | Vibrate droplet formation |
-
2009
- 2009-01-21 CN CN2009100456526A patent/CN101480609B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289236A (en) * | 2014-09-28 | 2015-01-21 | 佛山市天晟隆油脂化工有限公司 | Preparation method of solid base catalyst |
| CN108697149A (en) * | 2016-03-02 | 2018-10-23 | 巴斯夫欧洲公司 | Vibrate droplet formation |
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Denomination of invention: Method for preparing nano solid base catalyst with nucleocapsid structure for synthesizing biodiesel Effective date of registration: 20101008 Granted publication date: 20100811 Pledgee: Shanghai, Xuhui, Company limited by guarantee Pledgor: Shanghai Sanrui Polymer Material Co., Ltd. Registration number: 2010990000907 |
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