CN103755971A - Method for extracting lignin of straws by acidic ionic liquid and organic solvent - Google Patents
Method for extracting lignin of straws by acidic ionic liquid and organic solvent Download PDFInfo
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- CN103755971A CN103755971A CN201310669507.1A CN201310669507A CN103755971A CN 103755971 A CN103755971 A CN 103755971A CN 201310669507 A CN201310669507 A CN 201310669507A CN 103755971 A CN103755971 A CN 103755971A
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- xylogen
- organic solvent
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- ionic liquid
- acidic ion
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to a method for extracting lignin of straws by an acidic ionic liquid and an organic solvent. The method realizes simultaneous lignin extraction and biomass liquefaction under the normal pressure by the acidic ionic liquid and the high-boiling point organic solvent. The method comprises the following steps of a, adding straws into the high-boiling point organic solvent and the acidic ionic liquid and carrying out a reaction process, b, after the reaction, adding acetone into the reaction product and carrying out filtration separation, and c, removing acetone in the filtrate, adding distilled water into the filtrate so that lignin is separated, and carrying out freeze drying. The method has simple processes, realizes the reaction under the normal pressure and is environmentally friendly.
Description
Technical field
The invention belongs to biomass comprehensive and utilize field, particularly a kind of method of utilizing acidic ion liquid to extract xylogen with high boiling organic solvent in stalk.
Background technology
Along with scientific-technical progress and social development, people improve constantly the understanding of environment and the energy.Xylogen is one of main component of the abundantest lignocellulose, it is a kind of renewable natural resources with aromatic nucleus, in the natural structure unit of xylogen, contain various active functional group, mainly contain alcoholic extract hydroxyl group, phenolic hydroxyl group, methoxyl group, aldehyde radical, ketone group, carboxyl etc., the response capacity of these active groups is very strong, the reactions such as energy be oxidized, reduction, sulfomethylation, alkoxide, alkylation, this has just improved xylogen in industrial adaptability greatly.China's stalk main application is papermaking, feed, goes back field and use as fuel, and the complete situation in high flow rate, high pollution, low output is very low to the utilization ratio of stalk.The main component of stalk is Mierocrystalline cellulose, hemicellulose and xylogen, and therefore the renewable resources of this rich content of development and utilization is of great immediate significance and vast potential for future development.
The method of extracting at present xylogen from biomass mainly contains: organic solvent extraction method, concentrated acid dissolves vegetable fibre extracting method and alkaline extraction method, but organic solvent extraction method adopts low boiling point organic solvent more, causes condition harshness, the problems such as boiling point is low, dangerous large.Acid extraction and alkaline extraction can cause problem of environmental pollution.Ionic liquid is a kind of compound of green safety, has higher thermostability, but it is higher easily to reclaim price, limited it and used on a large scale, and viscosity is large, is unfavorable for high efficiency extraction xylogen.
Summary of the invention
In order to solve the aforementioned problems in the prior, we have carried out a large amount of research, found that and can adopt acidic ion liquid to make catalyzer and high boiling organic solvent does the method that solvent extracts the xylogen in stalk, this method has not only solved the high problem of simple use ionic liquid cost, and reduction system viscosity, reduce problems such as equipment corrosions simultaneously, have that technique is simple, an environmental protection, last handling process is simple, lignin extraction rate is high feature.
Method provided by the invention is: take stalk as raw material, acidic ion liquid is catalyzer, and high boiling organic solvent is solvent, under normal pressure, in 110～160 ℃, reacts 0.5～6h.When the color of solution is from colourless while becoming brown, reaction stops.Add acetone and stir 30min, product vacuum filtration, insolubles carbohydrate is dried to constant weight at 105 ℃.Filtrate adding distil water is separated out xylogen, and standing for some time, vacuum filtration obtains xylogen, afterwards lyophilize.Ionic liquid can be by adding wherein acetonitrile/ethyl acetate to separate, then refine, and can realize the recycle of ionic liquid.
The mass ratio of described high boiling organic solvent and stalk is: 5:1～15:1, the mass ratio of acidic ion liquid and stalk is: 1.5:1～7.5:1.
Wherein described acidic ion liquid is functionalized ion liquid, and positively charged ion is monokaryon and the double-core nitrogenous compound that alkyl imidazole, alkyl pyridine etc. form, and negatively charged ion is HSO
4 -ionic liquid, high boiling organic solvent is N-Methyl pyrrolidone.
Described method, is used oil bath heating.
Described method, ionic liquid recycle can be by adding wherein acetonitrile/ethyl acetate to separate, then refine, and can realize the recycle of ionic liquid.
The present invention has the following advantages:
1. raw material sources are abundant, environmental protection;
2. this invention, in liquefying biomass, has been extracted xylogen;
3. the present invention uses functionalized ion liquid and high boiling organic solvent jointly to extract xylogen, has reduced extraction expense;
4. this invention mild condition can be extracted xylogen under normal pressure, little to equipment corrosion, has improved the extraction yield of xylogen;
5. technique simple possible of the present invention, functionalized ion liquid and high boiling organic solvent be recyclable and recycling all, environmentally safe;
6. method provided by the invention is easy to realize industrialization.
Embodiment
The present invention illustrates by following examples, but the present invention is not limited to following embodiment, and before and after not departing from, under the prerequisite of described aim, change is included in technical scope of the present invention.
Embodiment 1
Ionic liquid used is 1-methyl-3-N-morpholinopropanesulfonic acid base imidazole bisulfate ([C
3h
6sO
3hmin] HSO
4)
Implementation method is: 20mlN-methyl-2-pyrrolidone (NMP) is added in the three neck round-bottomed flasks of 50ml, round-bottomed flask is placed in to the oil bath pan of 160 ℃, add afterwards 1-methyl-3-N-morpholinopropanesulfonic acid base imidazole bisulfate ([C
3h
6sO
3hmin] HSO
4) 1.81g and 2g stalk be added in there-necked flask, at N
2lower stirring oil bath is heated to 160 ℃, reaction 2h, and stopped reaction, is cooled to room temperature, adds acetone, stirring at room 30min, by mixture suction filtration, filtrate is steamed and is removed acetone at Rotary Evaporators backspin, adds distilled water and separates out precipitation xylogen.Xylogen lyophilize is to constant weight, and calculating lignin extraction rate is 81.31%.
Embodiment 2～4
Implementation method is: according to the experimental procedure identical with embodiment 1, but use different ionic liquid/stalk mass ratio, shown in result table 1.
The stalk of table 1 different mass extracts the result of xylogen in ionic liquid
Claims (8)
1. an acidic ion liquid and organic solvent extract the method for xylogen in stalk, it is characterized in that: take stalk as raw material, acidic ion liquid makees catalyzer and high boiling organic solvent is solvent, under normal pressure, in 120～160 ℃, react 0.5～6h, when the color of solution is from colourless while becoming brown, reaction stops, add acetone and stir 30min, product vacuum filtration, insolubles carbohydrate is dried to constant weight at 105 ℃, and filtrate adding distil water is separated out xylogen, standing for some time, vacuum filtration obtains xylogen, and lyophilize obtains xylogen
Wherein R is for extracting xylogen rate, W
0for the xylogen initial mass in stalk, W
1for extracting the quality of xylogen.
2. a kind of acidic ion liquid according to claim 1 and organic solvent extract the method for xylogen in stalk, and stalk is preferably the Powdered stalk pulverizing and sieving.
3. a kind of acidic ion liquid according to claim 1 and organic solvent extract the method for xylogen in stalk, the mass ratio that it is characterized in that high boiling organic solvent and stalk is: 5:1～15:1, the mass ratio of acidic ion liquid and stalk is: 1.5:1～7.5:1.
4. a kind of acidic ion liquid according to claim 1 and organic solvent extract the method for xylogen in stalk, it is characterized in that, described acidic ion liquid is sulfonate functional ionic liquid, and positively charged ion is imidazoles organic cation, and negatively charged ion is HSO
4 -ionic liquid.
5. a kind of acidic ion liquid according to claim 1 and organic solvent extract the method for xylogen in stalk, it is characterized in that, described high boiling organic solvent is N-Methyl pyrrolidone.
6. acidic ion liquid and organic solvent are the method for solvent extraction xylogen according to claim 1, use oil bath heating.
7. the method for liquefying straws by ionic liquid according to claim 1, vacuum filtration temperature is temperature of reaction or slightly lower than temperature of reaction.
8. the method for liquefying straws by ionic liquid according to claim 1, ionic liquid can be separation by adding wherein acetonitrile/ethyl acetate to carry out with liquefied product, then refine, and can realize the recycle of ionic liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310669507.1A CN103755971A (en) | 2013-12-10 | 2013-12-10 | Method for extracting lignin of straws by acidic ionic liquid and organic solvent |
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|---|---|---|---|
| CN201310669507.1A CN103755971A (en) | 2013-12-10 | 2013-12-10 | Method for extracting lignin of straws by acidic ionic liquid and organic solvent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448339A (en) * | 2014-12-04 | 2015-03-25 | 江南大学 | Method for extracting lignin from straws by oxalic acid combined with ionic liquid and organic solvent |
| CN106188568A (en) * | 2016-07-20 | 2016-12-07 | 昆明理工大学 | The method of pyridine analogs carboxylic acid separating biomass lignin |
| CN106698581A (en) * | 2017-01-17 | 2017-05-24 | 河北工业大学 | Adsorption treatment method for cationic dye |
| CN113999269A (en) * | 2021-12-09 | 2022-02-01 | 中国矿业大学 | Method for promoting extraction of lignin in straws and catalytic preparation of levulinic acid and ethyl ester thereof by using ammonium-based Bronsted acidic ionic liquid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448339A (en) * | 2014-12-04 | 2015-03-25 | 江南大学 | Method for extracting lignin from straws by oxalic acid combined with ionic liquid and organic solvent |
| CN106188568A (en) * | 2016-07-20 | 2016-12-07 | 昆明理工大学 | The method of pyridine analogs carboxylic acid separating biomass lignin |
| CN106698581A (en) * | 2017-01-17 | 2017-05-24 | 河北工业大学 | Adsorption treatment method for cationic dye |
| CN106698581B (en) * | 2017-01-17 | 2020-05-05 | 河北工业大学 | Adsorption treatment method of cationic dye |
| CN113999269A (en) * | 2021-12-09 | 2022-02-01 | 中国矿业大学 | Method for promoting extraction of lignin in straws and catalytic preparation of levulinic acid and ethyl ester thereof by using ammonium-based Bronsted acidic ionic liquid |
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Application publication date: 20140430 |