CN103159622A - Preparation method of acetin - Google Patents
Preparation method of acetin Download PDFInfo
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- CN103159622A CN103159622A CN 201110425564 CN201110425564A CN103159622A CN 103159622 A CN103159622 A CN 103159622A CN 201110425564 CN201110425564 CN 201110425564 CN 201110425564 A CN201110425564 A CN 201110425564A CN 103159622 A CN103159622 A CN 103159622A
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- glycerol acetate
- acetin
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Abstract
The invention relates to a preparation method of acetin. The acetin prepared through the preparation method can be used as an additive of biodiesel to improve the cryogenic property of the biodiesel and the like. The preparation method of the acetin comprises the steps: mixing glycerol and acetic acid together according to certain molar ratio, heating and stirring the mixture under the function of a carbon based solid acid catalyst, separating and generating water from the mixture, filtering and removing the catalyst after the mixture reacts for certain period of time, performing distillation or reduced pressure distillation, and obtaining the acetin. The preparation method of the acetin has the advantages of being simple to operate, simple in catalyst separation, high in product yield, light in tincture, free from extraneous odor and convenient for industrialization implementation and the like. Further the preparation method of the acetin provides a new path for the development and utilization of biodiesel by-product glycerol.
Description
Technical field
The present invention relates to a kind of method for preparing glycerol acetate by glycerine and acetic acid esterified reaction, belong to the technical field for preparing glycerol acetate.
Background technology
All can produce by-product glycerin in the production process of biofuel, along with the large-scale development of biofuel, the reasonable utilization of by-product glycerin becomes one of key issue of Biodiesel development.The additive that is transformation of glycerol useful chemical, biofuel and biofuel has caused attention (J.A.Melero, et.al, the Energy ﹠amp of height; Fuels 2007,21,1782-1791; J.A.Melero, et.al, Green Chem., 2009,11,1285-1308; Liao, X.-Y, et.al, Fuel Processing Technology, 2009,90,988-993).Anhydrated by glycerine and acetic acid esterified and can obtain glycerol acetate, the additive that can be used for biofuel improves low-temperature performance of biofuel etc.
The preparation glycerol acetate needs an acidic catalyst: traditionally, tosic acid can be used as catalyzer; Also can use other an acidic catalyst, as catalyzer (Maria-Isabel Galan, et.al, Bioresource Technology, 2009,100,3775-3778 such as sulfuric acid, hydrochloric acid, phosphoric acid or various acidic ion liquids; Wu Lu equality, chemistry and biotechnology, 2009,26 (11): 27-29).Although use these catalyzer, all can obtain higher reaction yield, the main problem that exists is that catalyzer is to corrosion and the recovery problem of equipment.
Charcoal base solid sulfoacid is a kind of Multifunction material that has potentiality that development in recent years is got up.Be with a wide range of applications at aspects such as ion-exchange, absorption, catalysis, proton conductives.But, come catalyzing glycerol and acetic acid to prepare glycerol acetate and yet there are no report as catalyzer by the charcoal base solid sulfoacid of waste polystyrene foam and phenylcarbinol preparation.
Summary of the invention
For the deficiencies in the prior art, technical problem to be solved by this invention is that a kind of preparation method of glycerol acetate is provided.Method provided by the invention is: get a certain amount of glycerine, acetic acid, catalyzer and put into reactor, carry out dehydration reaction under heated and stirred.After reaction finishes, obtain glycerol acetate through simple separation.That this preparation method has is simple to operate, catalyst separating is simple, product yield is high, lighter color, free from extraneous odour, is convenient to the characteristics such as industrializing implementation.
The technical scheme that the present invention solves described glycerol acetate preparation method technical problem is, use the charcoal base solid sulfoacid of unbodied bulk as an acidic catalyst, the carbon material that this catalyzer uses is waste polystyrene foam and phenylcarbinol, and making catalyzer, to have sour density value be 0.3～2.0mmol/g.The preparation technology of this charcoal base solid sulfoacid is: a certain amount of waste polystyrene foam is dissolved in appropriate phenylcarbinol, under agitation adds the appropriate vitriol oil, 160～220 ℃ of reactions of heated and stirred 1～3 hour.Suction filtration, it is neutral washing to filtrate, filtration cakes torrefaction dewaters, and can obtain the charcoal base solid sulfoacid of unbodied bulk.
The technical scheme that the present invention solves described glycerol acetate preparation method technical problem is, design a kind of method that glycerine and acetic acid prepare glycerol acetate, this preparation method is applicable to glycerol acetate of the present invention, concrete technology is: glycerine is mixed by 1: 4～1.6 mol ratio mutually with acetic acid, take glycerine as standard substance, add the solid acid catalyst less than qualities of glycerin 10%, heated and stirred, keep 90～170 ℃ of temperature, separate the water that generates, react after 1～6 hour, remove by filter catalyzer, distillation or underpressure distillation can obtain glycerol acetate.
Compare with the glycerol acetate preparation method of prior art, the present invention is to provide a kind of novel preparation method.Water insoluble and the organic solvent of the catalyzer that uses easily separates with reaction system, can Reusability.The preparation glycerol acetate reaction times is short, productive rate is high, lighter color, free from extraneous odour.Preparation technology is simple simultaneously, and catalyzer is little to equipment corrosion, suitable large-scale industrial production.
Embodiment
Further narrate the present invention below in conjunction with embodiment.Specific embodiment does not limit claim of the present invention.
Glycerol acetate preparation method technical scheme of the present invention is to use the charcoal base solid sulfoacid of the amorphous bulk that is prepared by waste polystyrene foam and phenylcarbinol as an acidic catalyst.
Glycerol acetate preparation method technical scheme of the present invention is, adopt glycerine and acetic acid to prepare glycerol acetate, this preparation method is applicable to glycerol acetate of the present invention, concrete technology is: glycerine is mixed by 1: 4～1.6 mol ratio mutually with acetic acid, under the charcoal base solid sulfoacid less than qualities of glycerin 10% exists, heated and stirred, keep 130～150 ℃ of temperature, with the water of taking generation with aqua out of or fractionation water storage, react after 2～4 hours, remove by filter catalyzer, distillation or underpressure distillation can obtain glycerol acetate.
Glycerol acetate of the present invention, main component is Vanay, can be used for the additive of biofuel.Prepared glycerol acetate is colourless transparent liquid.The present invention is owing to having adopted the charcoal base solid sulfoacid that is prepared by waste polystyrene foam and phenylcarbinol as catalyzer, in the scope of applicant's retrieval, there are no using the method to prepare the bibliographical information of glycerol acetate.Be easy to obtain on market and the glycerine of less expensive is synthesis material because glycerol acetate of the present invention adopts again, have the advantage that cost is low, be easy to industrialization and practical application.Development and utilization for biological diesel oil byproduct glycerin simultaneously provides a kind of new approach.
The present invention does not address part and is applicable to prior art.
Embodiment 1:
The 5g waste polystyrene foam is dissolved in the 10mL phenylcarbinol, under agitation adds the vitriol oil of 10mL98%, 160～220 ℃ of reactions of heated and stirred 3 hours.Suction filtration, it is neutral washing to filtrate, filtration cakes torrefaction dewaters, and can obtain the charcoal base solid sulfoacid catalyzer of unbodied bulk.Acid density 1.50mmol/g.
Embodiment 2
On the 100mL three-necked flask, electric stirring is installed, thermometer and minute water reflux add 10.4g glycerine, 32.3g acetic acid, 20mL benzene, and the catalyzer of preparation in 0.5g embodiment 1,130 ℃ of heated and stirred, reflux dewatering reaction 6 hours.Directly pour out reaction solution, after Distillation recovery benzene and unreacted acetic acid, obtain glycerol acetate, products collection efficiency 87.1%.Product contains 97.5% TG acid through the makings analysis, and all the other are glyceryl diacetate.
Embodiment 3
On the 100mL three-necked flask, electric stirring is installed, thermometer and minute water reflux add 5.0g glycerine, 19.2g acetic acid, 20mL benzene, and the catalyzer of preparation in 0.4g embodiment 1,130 ℃ of heated and stirred, back flow reaction 4 hours.Directly pour out reaction solution, after Distillation recovery benzene and unreacted acetic acid, obtain glycerol acetate, products collection efficiency 96.4%.Product contains 98.2% TG acid through the makings analysis, and all the other are glyceryl diacetate.
Embodiment 4
On the 100mL three-necked flask, electric stirring is installed, thermometer and fractionation plant add 5.0g glycerine, 19.2g acetic acid, and the catalyzer of preparation in 0.5g embodiment 1,120-150 ℃ of heated and stirred, fractionation reaction 2 hours.After the unreacted acetic acid of Distillation recovery, obtain glycerol acetate, productive rate 91.5%.Product contains 95.2% TG acid through the makings analysis, and all the other are glyceryl diacetate.
Claims (5)
1. the preparation method of a glycerol acetate, it is characterized in that method provided by the invention is: glycerine is mixed by 1: 4～1.6 mol ratio mutually with acetic acid, take glycerine as standard substance, add the solid acid catalyst less than qualities of glycerin 10%, heated and stirred, keep 90～170 ℃ of temperature, separate the water that generates, react after 1～6 hour, remove by filter catalyzer, distillation or underpressure distillation can obtain glycerol acetate, and its main component is Vanay.
A kind of glycerol acetate according to claim 1 the preparation method, it is characterized in that described catalyzer is to use the charcoal base solid sulfoacid of unbodied bulk as an acidic catalyst, the carbon material that this catalyzer uses is waste polystyrene foam and phenylcarbinol, and making catalyzer, to have sour density value be 0.3～2.0mmol/g.
3. the preparation method of a kind of glycerol acetate according to claim 1, is characterized in that described temperature of reaction is 90～170 ℃, and more suitable temperature is 110～160 ℃, and most suitable temperature is 130～150 ℃.
4. the preparation method of a kind of glycerol acetate according to claim 1, is characterized in that the described reaction times is 1～6 hour, and the more suitable time is 1.5～4 hours.
5. the preparation method of a kind of glycerol acetate according to claim 1, it is characterized in that to separate in described reacting by heating process the water of generation, can dewater to realize by band aqua or fractionation, can be sherwood oil, hexanaphthene, heptane, toluene or the benzene of 60-90 ℃ with aqua.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110425564 CN103159622A (en) | 2011-12-19 | 2011-12-19 | Preparation method of acetin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110425564 CN103159622A (en) | 2011-12-19 | 2011-12-19 | Preparation method of acetin |
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| CN103159622A true CN103159622A (en) | 2013-06-19 |
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| CN 201110425564 Pending CN103159622A (en) | 2011-12-19 | 2011-12-19 | Preparation method of acetin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032999A (en) * | 2017-05-22 | 2017-08-11 | 山东岩海建设资源有限公司 | A kind of method that utilization biological diesel oil byproduct glycerin produces triacetyl glycerine |
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2011
- 2011-12-19 CN CN 201110425564 patent/CN103159622A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032999A (en) * | 2017-05-22 | 2017-08-11 | 山东岩海建设资源有限公司 | A kind of method that utilization biological diesel oil byproduct glycerin produces triacetyl glycerine |
| CN107032999B (en) * | 2017-05-22 | 2019-12-17 | 山东岩海建设资源有限公司 | Method for producing glycerol triacetate by using biodiesel byproduct glycerol |
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Application publication date: 20130619 |