CN103233381A - High efficiency composite precipitating agent and method for extracting cellulose - Google Patents
High efficiency composite precipitating agent and method for extracting cellulose Download PDFInfo
- Publication number
- CN103233381A CN103233381A CN2013101271966A CN201310127196A CN103233381A CN 103233381 A CN103233381 A CN 103233381A CN 2013101271966 A CN2013101271966 A CN 2013101271966A CN 201310127196 A CN201310127196 A CN 201310127196A CN 103233381 A CN103233381 A CN 103233381A
- Authority
- CN
- China
- Prior art keywords
- ionic liquid
- allyl
- efficient compound
- compound precipitants
- methylimidazole
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides a high efficiency composite precipitating agent, which is composed of mixed acetone and waterless ethanol, and the volume ratio between the acetone and the waterless ethanol is 1:2-5; a method for extracting cellulose comprises the following steps: crushing straws into powder of 100 meshes, dissolving the straws with an ionic liquid 1-allyl-3-methylimidazolim chloride, adding a high efficiency composite precipitating agent, and extracting cellulose from the ionic liquid. The invention has the advantages that according to the invention a high efficiency composite precipitating agent is used for extracting cellulose which is dissolved in the ionic liquid, thereby realizing high efficiency regeneration of cellulose, and the high efficiency composite precipitating agent is easy to be separated from the ionic liquid; the invention improves the utilization efficiency of biomass resource, and improves the problem that the straw is hard to be degraded and reused with deep social meaning and economic value; the high efficiency composite precipitating agent is easy to be separated from the ionic liquid, thereby realizing high efficiency recovery and re-utilization of the ionic liquid and the precipitating agent.
Description
Technical field
The present invention relates to the biomass processes technology, especially a kind of efficient compound precipitants and be used for to extract cellulosic method.
Background technology
Along with the energy crisis that consumption and the whole world of traditional energies such as coal, oil faces, the development of sustainable energy and utilization have caused widely to be paid attention to.Cellulose is the living beings macromolecule that the occurring in nature distribution is the widest, reserves are maximum, and by β-1, the 4-glycosidic bond connects and the glucan of formation its structure by glucose molecule.Usually containing thousands of glucose units, is the main component of plant cell wall.Annual plant can produce 1,000 hundred million tons cellulose by photosynthesis, owing to plurality of advantages such as pollution-free, biocompatibility, readily degradable, wide material sources, is considered to be inexhaustible renewable resource simultaneously.
The research of ionic liquid aspect dissolving cellulos has at present had swift and violent development.The ionic liquid of discovering numerous species has solvability to cellulose.When utilizing ionic liquid extract cellulose/hemicellulose, precipitating agent is a key factor.Concerning fiber have the ionic liquid of fine solvability, can from ionic liquid, separate the cellulose that dissolves for those by selecting suitable precipitating agent such as acetone.For realizing cellulosic highly efficient regeneration, make up efficient compound precipitants, can reach with ionic liquid and form stronger active force, thereby realize cellulosic highly efficient regeneration.In addition, efficient compound precipitants is easy to separate with ionic liquid, thereby realizes high efficiente callback and the recycling of ionic liquid and precipitating agent.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of efficient compound precipitants is provided and is used for extracting cellulosic method, this method equipment needed thereby is simple, technology is easy, treatment temperature is low, mild condition, and can not cause additional environmental hazard, improve biomass resource utilization efficient.
Technical scheme of the present invention:
A kind of efficient compound precipitants is made up of acetone and absolute ethyl alcohol mixing, and the volume ratio of acetone and absolute ethyl alcohol is 1:2-5.
A kind of described efficient compound precipitants is used for extracting cellulosic method, and step is as follows:
1) rice straw was ground into 100 order rice straw powder;
2) the rice straw powder is mixed with ionic liquid 1-allyl-3-methylimidazole villaumite (AMIMCl), in 60 ℃ of water-bath mechanical agitation reaction 6h, obtain reactant;
3) with above-mentioned reactant with the centrifugal 10min of 12000r/min rotating speed, Separation of Solid and Liquid is got supernatant;
4) add efficient compound precipitants in the supernatant that above-mentioned separation obtains, mechanical agitation 30-60min under the room temperature obtains containing sedimentary mixed liquor, behind the suction filtration sediment oven dry that obtains is preserved, and is the target product cellulose, and the filtrate behind the suction filtration is reclaimed;
5) ionic liquid 1-allyl-3-methylimidazole acetate, repetitive cycling utilization are reclaimed in filtrate decompression distillation under 70 ℃ of water bath condition of Rotary Evaporators of reclaiming.
Described ionic liquid 1-allyl-3-methylimidazole villaumite (AMIMCl) is to be synthesized with the mass ratio of 1.0:1.2 by N-methylimidazole, allyl chloride, and its preparation method is: at N
2Protection mixes with allyl chloride the N-methylimidazole down with mass ratio 1.0:1.2; In 40 ℃ of water-baths, add hot reflux 12h then, after the removal of impurity, can make 1-allyl-3-methylimidazole villaumite.
The mass ratio of described rice straw powder and ionic liquid 1-allyl-3-methylimidazole villaumite is 1:20.
Described supernatant is 1:5-10 with the volume ratio of efficient compound precipitants.
Advantage of the present invention and beneficial effect are:
1) adopt 1-allyl-3-methylimidazole villaumite dissolving cellulos, it is strong and be easy to reclaim, can not volatilize to cellulosic solvability, can dissolve the cellulose in the rice straw effectively, and can not cause the resource excess waste;
2) use efficient compound precipitants to extract the cellulose that is dissolved in the ionic liquid, can realize cellulosic highly efficient regeneration, and efficient compound precipitants is easy to separate with ionic liquid;
3) this method equipment needed thereby is simple, technology is easy, treatment temperature is low, mild condition and can not cause additional environmental hazard, realized the high-efficiency pretreatment of rice straw, improve biomass resource utilization efficient, solved that rice straw is difficult to degrade, the difficult problem of recycling, had extremely far-reaching social effect and an economic worth.
The specific embodiment
The present invention is described in further detail by following examples, but the technology contents that present embodiment is narrated is illustrative, rather than determinate, should not limit to protection scope of the present invention according to this.
Embodiment 1:
A kind of efficient compound precipitants is used for extracting cellulosic method, and step is as follows:
1) rice straw was ground into 100 order rice straw powder;
2) be that 1:20 mix with ionic liquid 1-allyl-3-methylimidazole villaumite according to mass ratio with the rice straw powder, in 60 ℃ of water-bath mechanical agitation reaction 6h, obtain reactant;
3) with above-mentioned reactant with the centrifugal 10min of 12000r/min rotating speed, Separation of Solid and Liquid is got supernatant;
4) in the supernatant that above-mentioned separation obtains, add efficient compound precipitants, efficient compound precipitants is made up of acetone and absolute ethyl alcohol, its volume ratio is 1:5, supernatant is 1:5 with the volume ratio of efficient compound precipitants, mechanical agitation 60min under the room temperature obtains containing sedimentary mixed liquor, behind the suction filtration sediment oven dry that obtains is preserved, be the target product cellulose, the filtrate behind the suction filtration is reclaimed;
5) ionic liquid 1-allyl-3-methylimidazole acetate, repetitive cycling utilization are reclaimed in filtrate decompression distillation under 70 ℃ of water bath condition of Rotary Evaporators of reclaiming.
The used ionic liquid 1-allyl of this method-3-methylimidazole villaumite system is synthetic with the mass ratio of 1.0:1.2 by N-methylimidazole, allyl chloride, and its preparation method is: at N
2Protection mixes with allyl chloride the N-methylimidazole down with mass ratio 1.0:1.2; In 40 ℃ of water-baths, add hot reflux 12h then, after the removal of impurity, can make 1-allyl-3-methylimidazole villaumite.
Testing result shows: extract through efficient compound precipitants, the cellulosic recovery rate of gained is 95%, and described recovery rate is for adding the ratio of separating out the cellulose quality of dissolving in cellulose quality and the ionic liquid behind the efficient compound precipitants.
Embodiment 2:
A kind of efficient compound precipitants is used for extracting cellulosic method, and step is as follows:
1) rice straw was ground into 100 order rice straw powder;
2) be that 1:20 mix with ionic liquid 1-allyl-3-methylimidazole villaumite according to mass ratio with the rice straw powder, in 60 ℃ of water-bath mechanical agitation reaction 6h, obtain reactant;
3) with above-mentioned reactant with the centrifugal 10min of 12000r/min rotating speed, Separation of Solid and Liquid is got supernatant;
4) in the supernatant that above-mentioned separation obtains, add efficient compound precipitants, efficient compound precipitants is made up of acetone and absolute ethyl alcohol, its volume ratio is 1:3, supernatant is 1:8 with the volume ratio of efficient compound precipitants, mechanical agitation 40min under the room temperature obtains containing sedimentary mixed liquor, behind the suction filtration sediment oven dry that obtains is preserved, be the target product cellulose, the filtrate behind the suction filtration is reclaimed;
5) ionic liquid 1-allyl-3-methylimidazole acetate, repetitive cycling utilization are reclaimed in filtrate decompression distillation under 70 ℃ of water bath condition of Rotary Evaporators of reclaiming.
The preparation method of the used ionic liquid 1-allyl of this method-3-methylimidazole villaumite is identical with embodiment 1.
Testing result shows: extract through efficient compound precipitants, the cellulosic recovery rate of gained is 99%, and described recovery rate is for adding the ratio of separating out the cellulose quality of dissolving in cellulose quality and the ionic liquid behind the efficient compound precipitants.
Embodiment 3:
A kind of efficient compound precipitants is used for extracting cellulosic method, and step is as follows:
1) rice straw was ground into 100 order rice straw powder;
2) be that 1:20 mix with ionic liquid 1-allyl-3-methylimidazole villaumite (AMIMCl) according to mass ratio with the rice straw powder, in 60 ℃ of water-bath mechanical agitation reaction 6h, obtain reactant;
3) with above-mentioned reactant with the centrifugal 10min of 12000r/min rotating speed, Separation of Solid and Liquid is got supernatant;
4) in the supernatant that above-mentioned separation obtains, add efficient compound precipitants, efficient compound precipitants is made up of acetone and absolute ethyl alcohol, its volume ratio is 1:2, supernatant is 1:10 with the volume ratio of efficient compound precipitants, mechanical agitation 30min under the room temperature obtains containing sedimentary mixed liquor, behind the suction filtration sediment oven dry that obtains is preserved, be the target product cellulose, the filtrate behind the suction filtration is reclaimed;
5) ionic liquid 1-allyl-3-methylimidazole acetate, repetitive cycling utilization are reclaimed in filtrate decompression distillation under 70 ℃ of water bath condition of Rotary Evaporators of reclaiming.
The preparation method of the used ionic liquid 1-allyl of this method-3-methylimidazole villaumite is identical with embodiment 1.
Testing result shows: extract through efficient compound precipitants, the cellulosic recovery rate of gained is 98%, and described recovery rate is for adding the ratio of separating out the cellulose quality of dissolving in cellulose quality and the ionic liquid behind the efficient compound precipitants.
Claims (5)
1. efficient compound precipitants is characterized in that: mixed by acetone and absolute ethyl alcohol and form, the volume ratio of acetone and absolute ethyl alcohol is 1:2-5.
One kind according to claim 1 efficient compound precipitants be used for extracting cellulosic method, it is characterized in that step is as follows:
1) rice straw was ground into 100 order rice straw powder;
2) the rice straw powder is mixed with ionic liquid 1-allyl-3-methylimidazole villaumite (AMIMCl), in 60 ℃ of water-bath mechanical agitation reaction 6h, obtain reactant;
3) with above-mentioned reactant with the centrifugal 10min of 12000r/min rotating speed, Separation of Solid and Liquid is got supernatant;
4) add efficient compound precipitants in the supernatant that above-mentioned separation obtains, mechanical agitation 30-60min under the room temperature obtains containing sedimentary mixed liquor, behind the suction filtration sediment oven dry that obtains is preserved, and is the target product cellulose, and the filtrate behind the suction filtration is reclaimed;
5) ionic liquid 1-allyl-3-methylimidazole acetate, repetitive cycling utilization are reclaimed in filtrate decompression distillation under 70 ℃ of water bath condition of Rotary Evaporators of reclaiming.
3. be used for extracting cellulosic method according to the described efficient compound precipitants of claim 2, it is characterized in that: described ionic liquid 1-allyl-3-methylimidazole villaumite (AMIMCl) is to be synthesized with the mass ratio of 1.0:1.2 by N-methylimidazole, allyl chloride, and its preparation method is: at N
2Protection mixes with allyl chloride the N-methylimidazole down with mass ratio 1.0:1.2; In 40 ℃ of water-baths, add hot reflux 12h then, after the removal of impurity, can make 1-allyl-3-methylimidazole villaumite.
4. be used for extracting cellulosic method according to the described efficient compound precipitants of claim 2, it is characterized in that: the mass ratio of described rice straw powder and ionic liquid 1-allyl-3-methylimidazole villaumite is 1:20.
5. be used for extracting cellulosic method according to the described efficient compound precipitants of claim 2, it is characterized in that: described supernatant is 1:5-10 with the volume ratio of efficient compound precipitants.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101271966A CN103233381A (en) | 2013-04-12 | 2013-04-12 | High efficiency composite precipitating agent and method for extracting cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101271966A CN103233381A (en) | 2013-04-12 | 2013-04-12 | High efficiency composite precipitating agent and method for extracting cellulose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103233381A true CN103233381A (en) | 2013-08-07 |
Family
ID=48881445
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101271966A Pending CN103233381A (en) | 2013-04-12 | 2013-04-12 | High efficiency composite precipitating agent and method for extracting cellulose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103233381A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525461A (en) * | 2015-01-16 | 2015-04-22 | 南开大学 | Method for achieving material insulation and magnetism isolation through spraying load technology |
| CN105203372A (en) * | 2014-05-26 | 2015-12-30 | 中国科学院大连化学物理研究所 | Method for removing ionic liquid in sample solution |
| CN109880131A (en) * | 2019-01-25 | 2019-06-14 | 华中科技大学 | A kind of ionic liquid plasticized fibre element clean method for preparing |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005017001A1 (en) * | 2003-08-15 | 2005-02-24 | Kemira Oyj | Dissolution method for lignocellulosic materials |
| CN102101915A (en) * | 2010-11-11 | 2011-06-22 | 华南理工大学 | Separation method for agriculture and forestry biomass components |
| CN102504285A (en) * | 2011-11-03 | 2012-06-20 | 中国科技开发院广西分院 | Regenerated cellulose microspheres and preparation method thereof |
| CN102733224A (en) * | 2012-06-20 | 2012-10-17 | 合肥工业大学 | Method for separating corncob cellulose by using ionic liquid |
| CN102797187A (en) * | 2012-09-07 | 2012-11-28 | 南开大学 | Method for extracting cellulose in biomass raw material by utilizing ionic liquid |
| CN102926251A (en) * | 2012-11-23 | 2013-02-13 | 南开大学 | Method for extracting cellulose from straw by adopting ionic liquid |
-
2013
- 2013-04-12 CN CN2013101271966A patent/CN103233381A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005017001A1 (en) * | 2003-08-15 | 2005-02-24 | Kemira Oyj | Dissolution method for lignocellulosic materials |
| CN102101915A (en) * | 2010-11-11 | 2011-06-22 | 华南理工大学 | Separation method for agriculture and forestry biomass components |
| CN102504285A (en) * | 2011-11-03 | 2012-06-20 | 中国科技开发院广西分院 | Regenerated cellulose microspheres and preparation method thereof |
| CN102733224A (en) * | 2012-06-20 | 2012-10-17 | 合肥工业大学 | Method for separating corncob cellulose by using ionic liquid |
| CN102797187A (en) * | 2012-09-07 | 2012-11-28 | 南开大学 | Method for extracting cellulose in biomass raw material by utilizing ionic liquid |
| CN102926251A (en) * | 2012-11-23 | 2013-02-13 | 南开大学 | Method for extracting cellulose from straw by adopting ionic liquid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203372A (en) * | 2014-05-26 | 2015-12-30 | 中国科学院大连化学物理研究所 | Method for removing ionic liquid in sample solution |
| CN104525461A (en) * | 2015-01-16 | 2015-04-22 | 南开大学 | Method for achieving material insulation and magnetism isolation through spraying load technology |
| CN109880131A (en) * | 2019-01-25 | 2019-06-14 | 华中科技大学 | A kind of ionic liquid plasticized fibre element clean method for preparing |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110540508B (en) | Eutectic solvent and application thereof in extracting lignin | |
| CN102926251B (en) | Method for extracting cellulose from straw by adopting ionic liquid | |
| CN103194924A (en) | Method for extracting cellulose from straw stalk by using imidazole ion liquid | |
| CN106008730A (en) | Enzymolysis method for simultaneously extracting fucoidin, alginic acid, mannitol and seaweed dietary fiber | |
| CN103088692B (en) | Selective Separation lignin and cellulosic method from lignocellulose-like biomass | |
| CN102199483B (en) | Method for extracting lipid from Chlorella sorokiniana CS-01 | |
| CN108641102B (en) | High-efficiency cellulose solvent system and application thereof | |
| CN103480627A (en) | Novel recycling comprehensive utilization technology for agricultural and forestry waste | |
| CN105544265A (en) | Method for separating and extracting cellulose and lignin from bamboo wood | |
| CN102493246B (en) | Method for extracting and separating cellulose from biomass solid waste | |
| CN104341534A (en) | Method for preparing sodium alginate and organic fertilizer from gulfweed | |
| CN103497343A (en) | Kitchen waste fermentation product fulvic acid and preparation method thereof | |
| CN103233381A (en) | High efficiency composite precipitating agent and method for extracting cellulose | |
| CN102153443B (en) | Method for degrading polyethylene terephthalate | |
| CN104164801A (en) | Method for separating and recycling cellulose, semicellulose and lignin in lignocellulosic biomass at one time | |
| CN106832041A (en) | A kind of method that biologic enzymolysis method extracts fucoidin | |
| CN103031762B (en) | Method for preparing material rich in cellulose in degradable ionic liquid solvent | |
| CN104448365A (en) | Method for preparing epoxy vegetable oil toughened epoxy resin/cellulose composite membrane | |
| CN102268827A (en) | Method for extracting celluloses from tobaccos based on ferric chloride pretreatment | |
| CN103524571B (en) | Walnut slag reclaims the method preparing Weibull | |
| CN102849910A (en) | Method for recovering humic acid from sludge and improving anaerobic digestion of sludge | |
| CN102887957A (en) | Method for preparing sodium carboxymethyl cellulose from furfural slag | |
| CN102796048A (en) | Preparation method of ionic liquid for efficiently extracting cellulose and application thereof | |
| CN114808510A (en) | Method for extracting high-purity cellulose material from xylitol residues by using ionic liquid | |
| KR102385644B1 (en) | Method of preparing a nanocellulose |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130807 |