CN103102501B - Nonionic reverse micelle system modified nano microcrystalline cellulose and modification method thereof - Google Patents
Nonionic reverse micelle system modified nano microcrystalline cellulose and modification method thereof Download PDFInfo
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Abstract
The invention relates to nonionic reverse micelle system modified nano microcrystalline cellulose and a modification method thereof. The nonionic reverse micelle system modified nano microcrystalline cellulose is characterized in that nano microcrystalline cellulose is wrapped in a polar core of a reverse micelle system, and a continuous organic phase is arranged on the outside of the nano microcrystalline cellulose, wherein the reverse micelle system is prepared from a nonionic surfactant, a cosurfactant and an organic solvent through ultrasonic treatment; and the organic solvent is a weak-polarity organic solvent or the combination of a weak-polarity organic solvent and a non-polar organic solvent. According to the invention, preparation raw materials are commonly used industrial raw materials, thereby being easy to obtain; and the obtained reverse micelle system is stable, large in solubilized water yield and controllable in particle size, and can well disperse the nano microcrystalline cellulose with good stability. The modification method is simple in operation, and does not change the original shapes of nanoparticles, thereby keeping the original properties of nanoparticles. The modified nano microcrystalline celluloses can be applied to the fields of materials, medicines, textiles, and the like.
Description
Technical field
The present invention relates to a kind of nano micro crystal cellulose and method of modifying thereof of Nonionic reverse micelle system modification, particularly relate to a kind of nonionic surface active agent that adopts and in weak polar solvent, make reverse micelle system to the nano micro crystal cellulose of the Nonionic reverse micelle system modification of nano micro crystal cellulose modification and method of modifying thereof.
Background technology
Due to nano micro crystal cellulose, dispersing property is poor in organic solvent, and its application is on the composite very restricted.
At present mainly chemical modification is passed through to the method for nano micro crystal cellulose modification, comprise esterification, etherificate, oxidation, silanization, graft polymerization reaction etc.But chemical modification method needs the original form strictly controlling to protect nano micro crystal cellulose to reaction conditions, to avoid any polymorphic transformation and to maintain the complete of crystal.In addition, conventional method of modifying needs to carry out drying to nano particle in advance, and drying process easily causes the irreversible reunion of nano particle, thus affects the performance of nano particle.
Reverse micelle, also known as reverse micelle, is a kind of aqueous polymerization body contrary with Normal micelles structure of surfactant-dispersed spontaneous formation in continuous print organic phase.Organic solvent adopts the low-pole/nonpolar mixed organic solvents of the non-polar organic solvents such as octane-iso, hexanaphthene, tetracol phenixin, benzene or chloroform/hexanaphthene usually, and what select is cats product when adopting mixed organic solvents.
In reverse micelle, inwardly, the glomerate polarity core of shape, can dissolve a certain amount of water in core to hydrophilic head, thus forms macroscopically transparent homogeneous, thermodynamically stable microemulsion, microcosmic is then nanoscale size " pond ".Reverse micelle film strength, size and increase-volume amount are all comparatively large, have been proved to be number of chemical reaction, as the perfect medium of enzyme catalysis, polymerization, organic synthesis, nanoparticle preparation feedback, have been called as " microreactor ".
Contrary with situation in aqueous, it is inside that tensio-active agent forms polar head in organic solvent, and the non-polar tail aggregate containing water molecules kernel outwardly, reverse micelle is that the modification of nano micro crystal cellulose provides a promising approach.
At present polar water soluble material dispersion method in organic solvent is mainly adopted the method for it being carried out to chemical modification or tensio-active agent.The shortcoming of chemical modification method is complicated, has requirement and the easy character changing material itself to reaction conditions; Surfactant-modified shortcoming is that tensio-active agent usage quantity is large, to environment.Adopt reverse micelle system to carry out modification to polar material, the organic solvent be applicable to can be selected as the external phase of system, the aqueous solution of polar material or aqueous dispersions directly wrapped in " pond " of reverse micelle system and do not change the original character of material.Reverse micelle technology both domestic and external is mainly used in the preparation of the separation of non-polar system Semi-polarity material, enzyme immobilizatio and nanoparticle, wherein lays particular emphasis on again the extracting and separating to biologically active substance (protein, amino acid, microbiotic, enzyme) to the research of the separation of non-polar system Semi-polarity material.In addition, send out preparation with inorganics or the polymkeric substance composite nano particle that is carrier and carry out to the nanoparticle organic dye generated the study hotspot that finishing etc. also becomes this field current with reverse micelle, but still do not report the modification being directly applied to polar material at present.
Summary of the invention
The object of this invention is to provide a kind of nano micro crystal cellulose and method of modifying thereof of Nonionic reverse micelle system modification, particularly provide a kind of nonionic surface active agent that adopts in weak polar solvent, to make reverse micelle system to the nano micro crystal cellulose of the Nonionic reverse micelle system modification of nano micro crystal cellulose modification and method of modifying thereof.
When tensio-active agent concentration is in aqueous greater than its micelle-forming concentration, its polar group contacts with water outwardly, and form Normal micelles, hydrophobic group forms the kernel being similar to liquid hydrocarbon inwards, mainly contains spherical, spheroid, bar-shaped and stratiform etc.Contrary with situation in aqueous, it is inside that tensio-active agent forms polar head in organic solvent, and the non-polar tail aggregate containing water molecules kernel outwardly, is called reverse micelle.The polarity environment of reverse micelle inside makes it can Solubilization of Water, the aqueous solution and other polar material and form expansion reverse micelle.A kind of Nonionic reverse micelle system of the present invention is clear transparent solutions, described nonionic reverse micelle system, cosurfactant and organic solvent obtain through ultrasonication, and described organic solvent is the combination of weakly polar organic solvent or weakly polar organic solvent and non-polar organic solvent.Modified nano micro crystal cellulose is clear transparent solutions.
As preferred technical scheme:
A kind of Nonionic reverse micelle system as above, described nonionic surface active agent is fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene or polyol ester Soxylat A 25-7; The concentration of described nonionic surface active agent in described reverse micelle system is 0.01 ~ 0.20g/mL.
A kind of Nonionic reverse micelle system as above, described cosurfactant is n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-Octanol or isooctyl alcohol; The mass percent of described cosurfactant and described nonionic surface active agent is: 12.5% ~ 200%.The effect of cosurfactant can improve the efficiency of tensio-active agent.
A kind of Nonionic reverse micelle system as above, described weakly polar organic solvent is that polarity is greater than 0.1 and is less than or equal to the organic solvent of 4.5, is methylene dichloride, chloroform, ethylene dichloride or toluene; Described weakly polar organic solvent and the combination of non-polar organic solvent refer to the combination that described weakly polar organic solvent and polarity are less than or equal to the non-polar organic solvent of 0.1, described non-polar organic solvent is iso-pentane, Skellysolve A, normal hexane, hexanaphthene or octane-iso, and the mass percent of wherein said weakly polar organic solvent and non-polar organic solvent is: 100% ~ 200%.Weakly polar organic solvent replaces traditional non-polar organic solvent, can expand the range of application of reverse micelle system.
Present invention also offers a kind of preparation method of Nonionic reverse micelle system, nonionic surface active agent, cosurfactant and organic solvent are mixed with working fluid at a certain temperature; Then by described working fluid through ultrasonication, obtain stable reverse micelle system; Described organic solvent is the combination of weakly polar organic solvent or weakly polar organic solvent and non-polar organic solvent.
The preparation method of a kind of Nonionic reverse micelle system as above, described ultrasonication refers to ultrasonic power 600 ~ 1000W, and the treatment time is 5 ~ 30min; Described certain temperature is 25 ~ 30 DEG C; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 5000 ~ 8000r/min, time 20 ~ 30min, solution is not muddy, is stabilising system.Reverse micelle system size distribution after the process of excusing from death ripple is homogeneous.
Invention further provides a kind of method of Nonionic reverse micelle system modified Nano Microcrystalline Cellulose, comprise the following steps:
(1) nonionic surface active agent, cosurfactant and organic solvent are mixed with working fluid at a certain temperature;
(2) then by described working fluid through ultrasonication, obtain stable reverse micelle system;
(3) certain density nano micro crystal cellulose is added in reverse micelle system, ultrasonication, obtain nano micro crystal cellulose stable dispersions in organic solvent, namely complete the modification to nano micro crystal cellulose;
Described organic solvent is the combination of weakly polar organic solvent or weakly polar organic solvent and non-polar organic solvent.
The method of Nonionic reverse micelle system modified polar material as above, described certain temperature is 25 ~ 30 DEG C; Ultrasonication in described step (2) refers to ultrasonic power 600 ~ 1000W, and the treatment time is 5 ~ 30min; Ultrasonication in described step (3) refers to ultrasonic power 600 ~ 1000W, and the treatment time is 5 ~ 30min.
The method of Nonionic reverse micelle system modified Nano Microcrystalline Cellulose as above, described finite concentration refers to that the mass percent that nano micro crystal cellulose accounts for nano micro crystal cellulose stable dispersions is in organic solvent 0.01% ~ 10%.
The method of Nonionic reverse micelle system modified Nano Microcrystalline Cellulose as above, described stable reverse micelle system is reverse micelle system solution, clear, and place one month, solution is not muddy, is stabilising system.
The modified polar material that the method for a kind of Nonionic reverse micelle system modified polar material of the present invention obtains, described modified polar material is the stable dispersions of polar water soluble material in reverse micelle system, and described nonionic reverse micelle system, cosurfactant and organic solvent obtain through ultrasonication; Described organic solvent is the combination of weakly polar organic solvent or weakly polar organic solvent and non-polar organic solvent.
Beneficial effect:
(1) the present invention adopts common non-ionic surfactant, cosurfactant and non-polar organic solvent to prepare reverse micelle system, and by using assistant concentration, burden control water solubilization size.
(2) the present invention utilizes ultrasonic wave to prepare reverse micelle system, is stablized, uniform reverse micelle system, and the present invention adopts supersonic treatment, prepares that inverse micelle method is simple, simple operation, and application is simple.
(3) utilize ultrasonic wave to carry out pre-treatment to the nano micro crystal cellulose of polar water soluble, polar water soluble material is scattered in the middle of system better.
(4) the present invention adopts non-ionic type reverse micelle modified Nano Microcrystalline Cellulose, such that polar water soluble nano micro crystal cellulose is uniform and stable to be scattered in non-polar organic solvent, can be applicable to react between water-soluble substances and nonpolar organic matter matter.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent fatty alcohol-polyoxyethylene ether AEO-9, cosurfactant n-propyl alcohol and organic solvent dichloromethane are mixed with working fluid at 25 DEG C; Then by described working fluid through ultrasonication, ultrasonic power 600W, the treatment time is 30min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 5000r/min, time 30min, solution is not muddy, is stabilising system.Wherein, the concentration of fatty alcohol-polyoxyethylene ether in described reverse micelle system is 0.01g/mL, and the mass percent of n-propyl alcohol and fatty alcohol-polyoxyethylene ether is 12.5%.The nano micro crystal cellulose aqueous dispersions of 0.5% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 2
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent alkylphenol polyoxyethylene OP-7, cosurfactant propyl carbinol and organic solvent trichloromethane are mixed with working fluid at 25 DEG C; Then by described working fluid through ultrasonication, ultrasonic power 1000W, the treatment time is 5min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 8000r/min, time 20min, solution is not muddy, is stabilising system.Wherein, the concentration of alkylphenol polyoxyethylene OP-7 in described reverse micelle system is 0.05g/mL, and propyl carbinol and alkylphenol polyoxyethylene OP-7 mass percent are 150%.The nano micro crystal cellulose aqueous dispersions of 0.5% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 3
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent fatty alcohol-polyoxyethylene ether AEO-11, cosurfactant n-Octanol and mixed organic solvents toluene and normal hexane are mixed with working fluid at 25 DEG C, and the mass percent of toluene and normal hexane is 200%; Then by described working fluid through ultrasonication, ultrasonic power 800W, the treatment time is 25min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 8000r/min, time 20min, solution is not muddy, is stabilising system.Wherein, the concentration of fatty alcohol-polyoxyethylene ether AEO-11 in described reverse micelle system is 0.12g/mL, and the mass percent of n-Octanol and fatty alcohol-polyoxyethylene ether AEO-11 is 50%.The nano micro crystal cellulose aqueous dispersions of 1.5% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 4
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent fatty alcohol-polyoxyethylene ether AEO-7, cosurfactant Virahol and organic solvent toluene are mixed with working fluid at 25 DEG C; Then by described working fluid through ultrasonication, ultrasonic power 1000W, the treatment time is 5min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 8000r/min, time 20min, solution is not muddy, is stabilising system.Wherein, the concentration of fatty alcohol-polyoxyethylene ether AEO-7 in described reverse micelle system is 0.10g/mL, and the mass percent of Virahol and fatty alcohol-polyoxyethylene ether AEO-7 is 200%.The nano micro crystal cellulose aqueous dispersions of 2.0% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 5
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent fatty alcohol-polyoxyethylene ether AEO-9, cosurfactant isopropylcarbinol and organic solvent dichloromethane are mixed with working fluid at 25 DEG C; Then by described working fluid through ultrasonication, ultrasonic power 600W, the treatment time is 30min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 5000r/min, time 30min, solution is not muddy, is stabilising system.Wherein, the concentration of fatty alcohol-polyoxyethylene ether AEO-9 in described reverse micelle system is 0.08g/mL, and the mass percent of isopropylcarbinol and fatty alcohol-polyoxyethylene ether AEO-9 is 100%.The nano micro crystal cellulose aqueous dispersions of 1.5% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 6
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent alkylphenol polyoxyethylene OP-7, cosurfactant Pentyl alcohol and mixed organic solvents chloroform and iso-pentane are mixed with working fluid at 25 DEG C, and the mass percent of chloroform and iso-pentane is 100%; Then by described working fluid through ultrasonication, ultrasonic power 800W, the treatment time is 25min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 8000r/min, time 20min, solution is not muddy, is stabilising system.Wherein, the concentration of alkylphenol polyoxyethylene OP-7 in described reverse micelle system is 0.10g/mL, and the mass percent of Pentyl alcohol and alkylphenol polyoxyethylene OP-7 is 120%.The nano micro crystal cellulose aqueous dispersions of 5% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 7
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent alkylphenol polyoxyethylene OP-10, cosurfactant primary isoamyl alcohol and mixed organic solvents methylene dichloride and hexanaphthene are mixed with working fluid at 25 DEG C, and methylene dichloride and hexanaphthene mass percent are 120%; Then by described working fluid through ultrasonication, ultrasonic power 1000W, the treatment time is 5min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 8000r/min, time 20min, solution is not muddy, is stabilising system.Wherein, the concentration of alkylphenol polyoxyethylene OP-10 in described reverse micelle system is 0.14g/mL, and the mass percent of primary isoamyl alcohol and alkylphenol polyoxyethylene OP-10 is 80%.The nano micro crystal cellulose aqueous dispersions of 5% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 8
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent polyol ester Soxylat A 25-7 Tween-40, cosurfactant isooctyl alcohol and mixed organic solvents ethylene dichloride and Skellysolve A are mixed with working fluid at 25 DEG C, and ethylene dichloride and Skellysolve A mass percent are 150%; Then by described working fluid through ultrasonication, ultrasonic power 800W, the treatment time is 20min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 6000r/min, time 25min, solution is not muddy, is stabilising system.Wherein, the concentration of polyol ester Soxylat A 25-7 Tween-40 in described reverse micelle system is 0.20g/mL, and the mass percent of isooctyl alcohol and polyol ester Soxylat A 25-7 Tween-40 is 20%.The nano micro crystal cellulose aqueous dispersions of 4% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Embodiment 9
Nonionic reverse micelle system modified Nano Microcrystalline Cellulose:
Nonionic surface active agent polyol ester Soxylat A 25-7 Tween-20, cosurfactant propyl carbinol and mixed organic solvents chloroform and octane-iso are mixed with working fluid at 25 DEG C, and chloroform and octane-iso mass percent are 150%; Then by described working fluid through ultrasonication, ultrasonic power 1000W, the treatment time is 5min, obtains stable reverse micelle system; Described reverse micelle system stabilizes to clear transparent solutions, and through whizzer high speed centrifugation, rotating speed 6000r/min, time 25min, solution is not muddy, is stabilising system.Wherein, the concentration of polyol ester Soxylat A 25-7 Tween-20 in described reverse micelle system is 0.20g/mL, and the mass percent of n-Octanol and polyol ester Soxylat A 25-7 Tween-20 is 50%.The nano micro crystal cellulose aqueous dispersions of 6% is added in above reverse micelle system, ultrasonication 5min, obtain the dispersion liquid that nano micro crystal cellulose is stable in trichloromethane.
Claims (8)
1. a nano micro crystal cellulose for Nonionic reverse micelle system modification, is characterized in that: the nano micro crystal cellulose of described Nonionic reverse micelle system modification, and described nano micro crystal cellulose wraps in the polarity core of reverse micelle, and outside is continuous print organic phase; Described nonionic reverse micelle system, cosurfactant and organic solvent obtain through ultrasonication; Described organic solvent is the combination of weakly polar organic solvent or weakly polar organic solvent and non-polar organic solvent; The combination of wherein said weakly polar organic solvent and non-polar organic solvent, the mass percent of weakly polar organic solvent and non-polar organic solvent is: 100% ~ 200%; The concentration of described nonionic surface active agent in described reverse micelle system is 0.01 ~ 0.20g/mL.
2. the nano micro crystal cellulose of a kind of Nonionic reverse micelle system modification according to claim 1, is characterized in that, described nonionic surface active agent is fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene or polyol ester Soxylat A 25-7.
3. the nano micro crystal cellulose of a kind of Nonionic reverse micelle system modification according to claim 1, is characterized in that, described cosurfactant is n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-Octanol or isooctyl alcohol; The mass percent of described cosurfactant and described nonionic surface active agent is: 12.5% ~ 200%.
4. the nano micro crystal cellulose of a kind of Nonionic reverse micelle system modification according to claim 1, it is characterized in that, described weakly polar organic solvent is that polarity is greater than 0.1 and is less than or equal to the organic solvent of 4.5, is methylene dichloride, chloroform, ethylene dichloride or toluene; Described weakly polar organic solvent and the combination of non-polar organic solvent refer to the combination that described weakly polar organic solvent and polarity are less than or equal to the non-polar organic solvent of 0.1, and described non-polar organic solvent is iso-pentane, Skellysolve A, normal hexane, hexanaphthene or octane-iso.
5. the nano micro crystal cellulose of a kind of Nonionic reverse micelle system modification according to claim 1, is characterized in that, described nano micro crystal cellulose is the rod-like nano particle that can be dispersed in water, long 100 ~ 200nm, wide 7 ~ 15nm.
6. the method for modifying of the nano micro crystal cellulose of the Nonionic reverse micelle system modification according to any one of Claims 1 to 5, is characterized in that comprising the following steps:
(1) nonionic surface active agent, cosurfactant and organic solvent are mixed with working fluid at a certain temperature;
(2) then by described working fluid through ultrasonication, obtain stable reverse micelle system;
(3) nano micro crystal cellulose aqueous dispersions is added in reverse micelle system, ultrasonication, obtain nano micro crystal cellulose stable dispersions in organic solvent, namely complete the modification to nano micro crystal cellulose;
Described organic solvent is the combination of weakly polar organic solvent or weakly polar organic solvent and non-polar organic solvent.
7. method of modifying according to claim 6, is characterized in that, described certain temperature is 25 ~ 30 DEG C; Ultrasonication in described step (2) refers to ultrasonic power 600 ~ 1000W, and the treatment time is 5 ~ 30min; Ultrasonication in described step (3) refers to ultrasonic power 600 ~ 1000W, and the treatment time is 5 ~ 30min.
8. method of modifying according to claim 6, is characterized in that, described stable reverse micelle system is reverse micelle system solution, clear, and place one month, solution is not muddy, is stabilising system.
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