CN103263865A - Ionic liquid microemulsion and its preparation method and use - Google Patents
Ionic liquid microemulsion and its preparation method and use Download PDFInfo
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- CN103263865A CN103263865A CN2013101413219A CN201310141321A CN103263865A CN 103263865 A CN103263865 A CN 103263865A CN 2013101413219 A CN2013101413219 A CN 2013101413219A CN 201310141321 A CN201310141321 A CN 201310141321A CN 103263865 A CN103263865 A CN 103263865A
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Abstract
The invention discloses an ionic liquid microemulsion and its preparation method and use. The ionic liquid microemulsion is a [BMIM]PF6/[BMIM]Cl type ionic liquid microemulsion composed of a hydrophilic ionic liquid [BMIM]Cl as a main body, a lipophilic ionic liquid [BMIM]PF6 as a core, and a cationic surface active agent CTAB and a cosurfactant n-butanol as a mixed interfacial film. The preparation method comprises the following steps of adding the four components of the microemulsion into a reaction container, after adding a magnetic stirrer, putting the container into a magnetic stirring constant-temperature water bath kettle, keeping the temperature between 40 and 60 DEG C, and carrying out stirring until the system is clear and transparent and is not layered after being centrifugation at a high rate of 30000r/min for 5min. The ionic liquid microemulsion can be used for pre-treatment on wood fiber biomass. The ionic liquid microemulsion can reduce ionic liquid system viscosity and improves permeability and accessibility of drugs into a biomass raw material.
Description
Technical field
The present invention relates to a kind of novel ion liquid microemulsion, particularly relate to the preparation method of ion liquid microemulsion and the application in the wood fiber biomass preliminary treatment.
Background technology
The exhaustion of petroleum-based energy and ecological deterioration subsequently serious, people demand urgently reducing it to the negative effect of environment when seeking the alternative energy of a kind of green.Wood fiber biomass is renewable resource abundant, the most cheap on the earth, and the gross annual output amount can be up to 1 * 10
10Mt, thus bio-ethanol produce the lasting attention that more and more is subjected to Chinese scholars and enterpriser.But because the complex structure of living beings own and densification, the technology of Wooden Biomass ethanol production still exists expensive and problem such as poor efficiency, one of immature bottleneck that becomes restriction Wooden Biomass higher value application of wherein pretreatment of raw material technology.The combination of traditional preconditioning technique such as acid system, alkaline process, steam explosion, oxidation etc. and several method, treatment effect is better, but the processing cost height is seriously polluted; Though bioanalysis is handled cleaning, the cycle is long, treatment effeciency is low, cost is high, also is difficult to reach industrialization demands.
Ionic liquid is cellulosic direct solvent as a kind of green solvent.Can be used as the preliminary treatment solvent and tentatively open the internal structure of lignocellulose raw material, but because the ionic liquid viscosity is higher, the problem that the accessibility of existence and fibrous raw material and permeability are lower.
Summary of the invention
The object of the invention is to overcome the full-bodied shortcoming of simple ionic liquid, and a kind of ultra-small grain size is provided, and superpower infiltrative carrier-microemulsion effectively reduces the viscosity of ion liquid system, increases permeability and the accessibility of medicine.
Another object of the present invention is to provide the preparation method of above-mentioned ion liquid microemulsion system.
The present invention also has a purpose to be to provide the application of above-mentioned ion liquid microemulsion system in woody living beings.
The object of the invention is achieved through the following technical solutions:
The present invention selects for use hydrophily and lipophile ionic liquid to replace water and oil phase in traditional microemulsion respectively, with hydrophilic ionic-liquid [BMIM] Cl as main body, lipophile ionic liquid [BMIM] PF
6As nuclear, select for use cationic surfactant CTAB and cosurfactant n-butanol as mixed interfacial film simultaneously, constitute [BMIM] PF
6/ [BMIM] Cl type ion liquid microemulsion.This system can be used as the preliminary treatment solvent of biological material, changes the internal structure of raw material, increases hole area and contact gear ratio surface area, increases permeability and the accessibility of follow-up medicine, for solid foundation is established in the preparation of biomass energy.
Preferably, according to mass ratio, Biao Mian Huo Ji ︰ Zhu Biao Mian Huo Ji ︰ hydrophily Li Ye Ti ︰ lipophile ionic liquid=1:(6-14): (8-12): (4-8).
Preferably, according to mass ratio, Biao Mian Huo Ji ︰ Zhu Biao Mian Huo Ji ︰ hydrophily Li Ye Ti ︰ lipophile ionic liquid=1:(8～12): (10～12): (4～6).
The above-mentioned preparation method who states ion liquid microemulsion, four kinds of components of microemulsion are added in the reaction vessel, add after the magnetic stir bar container as in the magnetic agitation thermostat water bath, constant temperature 40-60 ℃, stirring is until the system clear, and not stratified under 30000r/min high speed centrifugation 5min condition, namely make ion liquid microemulsion.
Preferably, the rotating speed of described stirring is 300-400r/min, and the time is 20-25min.
The application of described ion liquid microemulsion in the wood fiber biomass preliminary treatment.Use this ionic liquid microemulsion system in needlebush, leaf wood and other biomass fiber raw material can reduce the pollution of environment when fully changing fibre structure, whole reduce to produce drop into, biomass energy is developed to the direction of green high-efficient more.Preferred applying step is as follows:
(1) in wood powder by the over dry quality, ion liquid microemulsion is mixed according to liquid-solid ratio 15-35ml/g with wood powder, at temperature 70-120 ℃, in water-bath or oil bath, react 6h at least under the condition of magnetic agitation rotating speed 400r/min, leave standstill and be cooled to room temperature;
(2) carry out the step-down suction filtration to reacting the back wood powder, the distilled water washing, oven dry at last gets final product.Filter cake oven dry is placed on and is used for next step enzymatic saccharification in the sealing bag, and gained filtrate can be directly used in down the preliminary treatment of criticizing wood powder through high speed centrifugation 15min after further removing the granulated slag that does not filter out behind the suction filtration.
Preferably, the liquid-solid ratio of described ion liquid microemulsion and wood powder is 20-30ml/g.
Preferably, described reaction temperature is 80-100 ℃.
Preferably, described wood powder is the powder of wood fiber biomass such as masson pine, larch, Eucalyptus or poplar.
Have following advantage and beneficial effect with respect to the prior art invention:
(1) the present invention is by the characteristic of ultra-small grain size and the superpower solubilising power of microemulsion, selects for use hydrophily and lipophile ionic liquid to replace water and oil phase in traditional microemulsion respectively, makes ion liquid microemulsion.This system not only has ionic liquid to the dissolubility of fibrous raw material, and has strong permeability, the characteristics of low-viscosity.Adopt the crystallization property of the woody biomass fiber raw material after this ion liquid microemulsion is handled to change, surface texture generation significant change simultaneously, hole area increases, and permeability and the accessibility of medicine increase thereupon, improve preliminary treatment efficient, be conducive to the raising of follow-up enzymatic saccharification efficient.
(2) the present invention can give full play to the advantage separately of ionic liquid and microemulsion, and under the situation that guarantees pretreating effect, selected medicine can carry out circulating and recovering, and the recyclability of ionic liquid has effectively reduced production cost, and to the environment green non-pollution.
(3) technology of the present invention is simple, and it is comparatively cheap that selected ionic liquid is price, and at the widely used medicine in other field, process for preparation requires lower to instrument and equipment.
Description of drawings
Fig. 1 is the influence curve figure of four kinds of different components of ion liquid microemulsion of the present invention to the system electrical conductivity.
Fig. 2 is that the different solvents system is to the permeance property comparative graph of woody biomass material.
Fig. 3 handles preceding wood powder apparent structure figure for ion liquid microemulsion.
Fig. 4 is ion liquid microemulsion of the present invention wood powder surface texture figure after handling.
The specific embodiment
The invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited thereto.
Embodiment 1
With hydrophilic ionic-liquid [BMIM] Cl as main body, lipophile ionic liquid [BMIM] PF
6As nuclear, use cationic surfactant CTAB(softex kw simultaneously) and the cosurfactant n-butanol as mixed interfacial film, constitute [BMIM] PF
6/ [BMIM] Cl type ion liquid microemulsion, its preparation method is as follows:
(((hydrophilic ionic-liquid) ︰ m (lipophile ionic liquid)=1:6:8:4 adds in the clear glass reaction vessel cosurfactant) ︰ m surfactant) ︰ m according to mass ratio m with four components of microemulsion, add after the magnetic stir bar container as in the magnetic agitation thermostat water bath, 40 ℃ of constant temperatures are stirring 20min until system clear and not stratified under 30000r/min high speed centrifugation 5min condition under the condition of rotating speed 300r/min.Making ion liquid microemulsion is placed in the port grinding bottle standby.Electrical conductivity performance and wood permeability at the configuration ion liquid microemulsion can characterize detection simultaneously.
The ion liquid microemulsion and the 80 order masson pine wood powders (water content 7%) that make are had in the round-bottomed flask of condenser system according to liquid-solid ratio 20:1ml/g (wood powder is calculated by the over dry quality) adding, 80 ℃ of temperature, in oil bath pan, react the 7h time under the condition of magnetic agitation rotating speed 400r/min, take off round-bottomed flask, be cooled to room temperature.
Carry out the step-down suction filtration to reacting the back wood powder, the distilled water washing, 105 ℃ of oven dry are handled.Filter cake oven dry is placed on and is used for next step enzymatic saccharification in the sealing bag, gained filtrate high speed centrifugation 15min behind the suction filtration, further remove can be directly used in behind the granulated slag that does not filter out recycling.
To carry out the enzymatic saccharification reaction through pretreated wood powder and cellulase, cellulase is selected sigmaC-1184 for use, enzyme dosage is 60PFU/g, time 24h, 50 ℃ of temperature, ph value 4.8, liquid-solid ratio 25:1ml/g, rotating speed 150rpm. reaction selects for use the method for chromatography of ions to carry out reducing sugar test after finishing, and the reduced sugar yield is not pass through 2.27 times of pretreated wood powder reduced sugar yield under the similarity condition.
Embodiment 2
(((hydrophilic ionic-liquid) ︰ m (lipophile ionic liquid)=1:10:12:4 adds in the clear glass reaction vessel cosurfactant) ︰ m surfactant) ︰ m according to mass ratio m with four components of microemulsion, add after the magnetic stir bar container as in the magnetic agitation thermostat water bath, 50 ℃ of constant temperatures are stirring 20min until system clear and not stratified under 30000r/min high speed centrifugation 5min condition under the condition of rotating speed 300r/min.Making ion liquid microemulsion is placed in the port grinding bottle standby.Electrical conductivity performance and wood permeability at the configuration ion liquid microemulsion can characterize detection simultaneously.
The ion liquid microemulsion and the 80 order masson pine wood powders (water content 7%) that make are had in the round-bottomed flask of condenser system according to liquid-solid ratio 30:1ml/g (wood powder is calculated by the over dry quality) adding, 100 ℃ of temperature, in oil bath pan, react the 7h time under the condition of magnetic agitation rotating speed 400r/min, take off round-bottomed flask, be cooled to room temperature.
Carry out the step-down suction filtration to reacting the back wood powder, the distilled water washing, 105 ℃ of oven dry are handled.Filter cake oven dry is placed on and is used for next step enzymatic saccharification in the sealing bag, gained filtrate high speed centrifugation 15min behind the suction filtration, further remove can be directly used in behind the granulated slag that does not filter out recycling.
To carry out the enzymatic saccharification reaction through pretreated wood powder and cellulase, cellulase is selected sigmaC-1184 for use, enzyme dosage is 60PFU/g, time 24h, 50 ℃ of temperature, ph value 4.8, liquid-solid ratio 25:1ml/g, rotating speed 150rpm. reaction selects for use the method for chromatography of ions to carry out reducing sugar test after finishing, and the reduced sugar yield is not pass through 2.53 times of pretreated wood powder reduced sugar yield under the similarity condition.
Embodiment 3
(((hydrophilic ionic-liquid) ︰ m (lipophile ionic liquid)=1:14:12:6 adds in the clear glass reaction vessel cosurfactant) ︰ m surfactant) ︰ m according to mass ratio m with four components of microemulsion, add after the magnetic stir bar container as in the magnetic agitation thermostat water bath, 50 ℃ of constant temperatures are stirring 20min until system clear and not stratified under 30000r/min high speed centrifugation 5min condition under the condition of rotating speed 300r/min.Making ion liquid microemulsion is placed in the port grinding bottle standby.Electrical conductivity performance and wood permeability at the configuration ion liquid microemulsion can characterize detection simultaneously.
The ion liquid microemulsion and the 80 order masson pine wood powders (water content 7%) that make are had in the round-bottomed flask of condenser system according to liquid-solid ratio 25:1ml/g (wood powder is calculated by the over dry quality) adding, 90 ℃ of temperature, in oil bath pan, react the 7h time under the condition of magnetic agitation rotating speed 400r/min, take off round-bottomed flask.
Carry out the step-down suction filtration to reacting the back wood powder, the distilled water washing, 105 ℃ of oven dry are handled.Filter cake oven dry is placed on and is used for next step enzymatic saccharification in the sealing bag, gained filtrate high speed centrifugation 15min behind the suction filtration, further remove can be directly used in behind the granulated slag that does not filter out recycling.To being untreated wood powder and handled wood powder and carried out the SEM scanning electron microscope observation.When being untreated, as shown in Figure 3, the wood powder microscopic surface texture compacts smoothly, the pit bottom closure, and chemicals is difficult for infiltration; Through preliminary treatment, as shown in Figure 4, the dissolved destruction of surface texture, compactness reduces, and especially the pit foot passage is opened, and medicine permeability and accessibility all can be increased dramatically.
To carry out the enzymatic saccharification reaction through pretreated wood powder and cellulase, cellulase is selected sigmaC-1184 for use, enzyme dosage is 60PFU/g, time 24h, 50 ℃ of temperature, ph value 4.8, liquid-solid ratio 25:1ml/g, rotating speed 150rpm. reaction selects for use the method for chromatography of ions to carry out reducing sugar test after finishing, and the reduced sugar yield is not pass through 2.35 times of pretreated wood powder reduced sugar yield under the similarity condition.
The comparative example
The preparation of oil-in-water microemulsion:
(((deionized water) ︰ m (cyclohexane)=1:5:4:2 adds in the clear glass reaction vessel n-butanol) ︰ m CTAB) ︰ m according to mass ratio m with four components of microemulsion, add after the magnetic stir bar container as in the magnetic agitation thermostat water bath, 40 ℃ of constant temperatures are stirring 20min until system clear and not stratified under 30000r/min high speed centrifugation 5min condition under the condition of rotating speed 300r/min.Making water oil-packaging type micro-emulsion liquid is placed in the port grinding bottle standby.Electrical conductivity performance and wood permeability at configuration water oil-packaging type micro-emulsion liquid can characterize detection simultaneously.
The oil-in-water microemulsion and the 80 order masson pine wood powders (water content 7%) that make are had in the round-bottomed flask of condenser system according to liquid-solid ratio 25:1ml/g (wood powder is calculated by the over dry quality) adding, 80 ℃ of temperature, in oil bath pan, react the 7h time under the condition of magnetic agitation rotating speed 400r/min, take off round-bottomed flask.
Carry out the step-down suction filtration to reacting the back wood powder, the distilled water washing, 105 ℃ of oven dry are handled.Filter cake oven dry is placed on and is used for next step enzymatic saccharification in the sealing bag, gained filtrate high speed centrifugation 15min behind the suction filtration, further remove can be directly used in behind the granulated slag that does not filter out recycling.
To carry out the enzymatic saccharification reaction through pretreated wood powder and cellulase, cellulase is selected sigmaC-1184 for use, and enzyme dosage is 60PFU/g, time 24h, 50 ℃ of temperature, ph value 4.8, liquid-solid ratio 25:1ml
/ g, rotating speed 150rpm.Select for use the method for chromatography of ions to carry out reducing sugar test after reaction finishes, the reduced sugar yield is not pass through 1.31 times of pretreated wood powder reduced sugar yield under the similarity condition.
Claims (10)
1. an ion liquid microemulsion is characterized in that, with hydrophilic ionic-liquid [BMIM] Cl as main body, lipophile ionic liquid [BMIM] PF
6As nuclear, use cationic surfactant CTAB and cosurfactant n-butanol as mixed interfacial film simultaneously, constitute [BMIM] PF
6/ [BMIM] Cl type ion liquid microemulsion.
2. ion liquid microemulsion according to claim 1 is characterized in that, according to mass ratio, and Biao Mian Huo Ji ︰ Zhu Biao Mian Huo Ji ︰ hydrophily Li Ye Ti ︰ lipophile ionic liquid=1:(6-14): (8-12): (4-8).
3. ion liquid microemulsion according to claim 2 is characterized in that, according to mass ratio, and Biao Mian Huo Ji ︰ Zhu Biao Mian Huo Ji ︰ hydrophily Li Ye Ti ︰ lipophile ionic liquid=1:(8～12): (10～12): (4～6).
4. the preparation method of claim 1 or 2 or 3 described ion liquid microemulsions, it is characterized in that, four kinds of components of microemulsion are added in the reaction vessel, add after the magnetic stir bar container as in the magnetic agitation thermostat water bath, constant temperature 40-60 ℃, stirring is until the system clear, and not stratified under 30000r/min high speed centrifugation 5min condition, namely makes ion liquid microemulsion.
5. preparation method according to claim 4 is characterized in that, the rotating speed of described stirring is 300-400r/min, and the time is 20-25min.
6. claim 1 or 2 or 3 application of described ion liquid microemulsion in the wood fiber biomass preliminary treatment.
7. application according to claim 6 is characterized in that, comprises the steps:
(1) in wood powder by the over dry quality, ion liquid microemulsion is mixed according to liquid-solid ratio 15-35ml/g with wood powder, at temperature 70-120 ℃, in water-bath or oil bath, react 6h at least under the condition of magnetic agitation rotating speed 400r/min, leave standstill and be cooled to room temperature;
(2) carry out the step-down suction filtration to reacting the back wood powder, the distilled water washing, oven dry at last gets final product.
8. application according to claim 7 is characterized in that, the liquid-solid ratio of described ion liquid microemulsion and wood powder is 20-30ml/g.
9. application according to claim 7 is characterized in that, described reaction temperature is 80-100 ℃.
10. application according to claim 7 is characterized in that, described wood powder is the powder of masson pine, larch, Eucalyptus or poplar.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106420610A (en) * | 2016-10-21 | 2017-02-22 | 昆明理工大学 | Ionic liquid microemulsion and application thereof |
| CN107216508A (en) * | 2017-06-20 | 2017-09-29 | 广西师范学院 | Sisal hemp enhancing rubber tyre and preparation method thereof |
| CN109912413A (en) * | 2019-03-27 | 2019-06-21 | 华南理工大学 | A kind of method that oleic acid base ion liquid microemulsion catalyzes and synthesizes butyl oleate |
| CN110387245A (en) * | 2019-08-28 | 2019-10-29 | 浙江海洋大学 | A kind of diesel fuel contaminated soil restorative procedure based on conductivity |
| CN110550650A (en) * | 2019-07-18 | 2019-12-10 | 华南理工大学 | Flower-shaped CuS submicron sphere and thermal synthesis method of ionic liquid microemulsion thereof |
| CN115058239A (en) * | 2022-06-22 | 2022-09-16 | 中国石油大学(华东) | Ionic liquid microemulsion thickened oil modifying viscosity reducer and preparation method thereof |
| CN115231562A (en) * | 2022-07-28 | 2022-10-25 | 国网湖南省电力有限公司 | Method for preparing MXene based on ionic liquid microemulsion stripping |
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| CN106420610A (en) * | 2016-10-21 | 2017-02-22 | 昆明理工大学 | Ionic liquid microemulsion and application thereof |
| CN106420610B (en) * | 2016-10-21 | 2019-06-11 | 昆明理工大学 | A kind of ionic liquid micro emulsion and its application |
| CN107216508A (en) * | 2017-06-20 | 2017-09-29 | 广西师范学院 | Sisal hemp enhancing rubber tyre and preparation method thereof |
| CN107216508B (en) * | 2017-06-20 | 2018-10-16 | 广西师范学院 | Sisal hemp enhances rubber tyre and preparation method thereof |
| CN109912413A (en) * | 2019-03-27 | 2019-06-21 | 华南理工大学 | A kind of method that oleic acid base ion liquid microemulsion catalyzes and synthesizes butyl oleate |
| CN110550650A (en) * | 2019-07-18 | 2019-12-10 | 华南理工大学 | Flower-shaped CuS submicron sphere and thermal synthesis method of ionic liquid microemulsion thereof |
| CN110550650B (en) * | 2019-07-18 | 2022-02-15 | 华南理工大学 | Flower-shaped CuS submicron sphere and thermal synthesis method of ionic liquid microemulsion thereof |
| CN110387245A (en) * | 2019-08-28 | 2019-10-29 | 浙江海洋大学 | A kind of diesel fuel contaminated soil restorative procedure based on conductivity |
| CN110387245B (en) * | 2019-08-28 | 2021-06-08 | 浙江海洋大学 | Diesel oil contaminated soil remediation method based on conductivity |
| CN115058239A (en) * | 2022-06-22 | 2022-09-16 | 中国石油大学(华东) | Ionic liquid microemulsion thickened oil modifying viscosity reducer and preparation method thereof |
| CN115231562A (en) * | 2022-07-28 | 2022-10-25 | 国网湖南省电力有限公司 | Method for preparing MXene based on ionic liquid microemulsion stripping |
| CN115231562B (en) * | 2022-07-28 | 2023-10-27 | 国网湖南省电力有限公司 | Method for preparing MXene based on ionic liquid microemulsion stripping |
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