CN104525066B - The preparation method of a kind of single dispersing consolidation micella particulate - Google Patents
The preparation method of a kind of single dispersing consolidation micella particulate Download PDFInfo
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- CN104525066B CN104525066B CN201510009162.6A CN201510009162A CN104525066B CN 104525066 B CN104525066 B CN 104525066B CN 201510009162 A CN201510009162 A CN 201510009162A CN 104525066 B CN104525066 B CN 104525066B
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- active agent
- micella
- consolidation
- alkane chain
- tensio
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
Abstract
The present invention relates to the preparation method of a kind of single dispersing consolidation micella particulate. Taking the molten long alkane chain tensio-active agent of shipwreck, short alkane chain tensio-active agent and vinylbenzene as raw material, first by long alkane chain surfactant dissolves in cosolvent, then add short alkane chain tensio-active agent and vinylbenzene, stir; Then drip the micella being gathered into solubilising vinylbenzene adding deionized water and ordering about, continue to add deionized water until excessive; Then cause styrene polymerization, form the single dispersing of different-grain diameter and the globular micelle particulate of consolidation. This single dispersing consolidation micella particulate can be used as the unit of new colloidal crystal lattice arrangement, and then preparation new colloidal crystal functional materials.
Description
Technical field
The invention belongs to technical field of function materials, it relates to the preparation method of a kind of single dispersing consolidation micella particulate.
Background technology
Colloidal crystal is that under the effects such as gravity, electrostatic force or capillary force, the aggregate of the two dimension that self-assembly is formed or three-dimensional close packing arrangement (respect by fourth by the inorganic or polymeric colloid microballoon of diameter at submicron or Nano grade, size single dispersing, Deng, chemical progress, 2004,16,321 ~ 326.; Xia, Y.; Etal.Adv.Mater.2000,12,693 ~ 713.). Colloidal crystal is just shown great attention to from birth, this is because (1) it can study growth and the fusing of crystal as model system, there is important scientific meaning (deVilleneuve, V.; Etal.Science2005,309,1231 ~ 1233.; Alsayed, A.; Etal.Science2005,309,1207 ~ 1210.; Pham, K.; Etal.Science2002,296,104 ~ 106.; Zhang, K.; Liu, X.Y.Nature2004,429,739 ~ 743.). (2) colloidal crystal has energy gap due to periodic structure, therefore has specific optical diffraction and optical band gap character, thus can be developed to important nonlinear optical material. Colloidal crystal can be used as photonic crystal and uses, and special light property makes colloidal crystal be expected to for the transporting of modulated electromagnetic wave (Li Hang, etc., chemical progress, 2011,23,1060 ~ 1068). (3) two-dimensional colloidal crystal is good nanometer of apparatus synthesis template, it is possible to the nanoparticle of inducing function is in self-assembly above, it is achieved object (Yang, the S. of function apparatus; Lei, Y.Nanoscale2011,3,2768 ~ 2782.).
Prepare colloidal crystal requirement particulate unit and there is good monodispersity, therefore silicon-dioxide, polystyrene and polyacrylamide microsphere is depended on so far, and inorganic nano-particle, the size of these microballoons or particulate at hundreds of nanometers until micron, or less than 10 nanometers, in the middle of lacking, the particulate of dimension degree, which has limited colloidal crystal development to a greater extent.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of single dispersing consolidation micella particulate. The present invention breaches tradition thinking, utilizing tensio-active agent to organize themselves into the feature of high degree of monodispersity micella, innovation preparation method, introduces curing mechanism, thus achieve the preparation of single dispersing consolidation micella particulate, make it to become the new unit of preparation new colloidal crystal lattice.
In order to reach the object of the invention, adopt following technical scheme:
The preparation method of a kind of single dispersing consolidation micella particulate: taking the molten long alkane chain tensio-active agent of shipwreck, short alkane chain tensio-active agent and vinylbenzene as raw material, first by long alkane chain surfactant dissolves in cosolvent, add short alkane chain tensio-active agent and vinylbenzene again, stir; Then drip and add deionized water, order about the micella that tensio-active agent is gathered into solubilising vinylbenzene, continue to add deionized water until greatly excessive; Finally cause styrene polymerization, form the single dispersing of different-grain diameter and the globular micelle particulate of consolidation.
The alkane chain carbonatoms of the long alkane chain tensio-active agent that described shipwreck is molten is 20 ~ 28, and the alkane chain carbonatoms of short alkane chain tensio-active agent is 10 ~ 18.
Described long alkane chain tensio-active agent and the mol ratio of short alkane chain tensio-active agent are 1:1 ~ 1:6.
The concentration of the vinylbenzene of solubilising and the ratio of tensio-active agent total concn are between 0.1:1 to 6:1.
Described cosolvent is methyl alcohol, ethanol, propyl alcohol, or methyl alcohol, ethanol, propyl alcohol and N, the one in the mixture of dinethylformamide.
Wherein, the add-on of deionized water with deionized water in total solvent the massfraction of (deionized water and cosolvent) reach more than 80wt% and be as the criterion.
The preparation method of the present invention is different from the preparation of simple polymer particles, but directly utilizes the single dispersing micella that tensio-active agent self-organization is formed. Solubilized styrene and the object be polymerized is in order to consolidation micella and regulation and control size. This kind of method can obtain very little organic fine particles, also eliminates in prepared by simple polymer particles the numerous and diverse formality removing surfactant templates.
The remarkable advantage of the present invention is:
1, the present invention first allows the molten long alkane chain tensio-active agent of shipwreck dissolve in cosolvent, under short alkane chain tensio-active agent coordinates, relies on the realization that adds of poor solvent water to organize themselves into as single dispersing micella; The method breaches a long-term difficult problem for the molten long alkane chain tensio-active agent investigation and application of shipwreck, and its research of expansion and practical application is significant;
2, synchronously having added in the micelle formation process of single dispersing vinylbenzene molten, recycling adds the polymerization of molten vinylbenzene to realize the consolidation of micella particulate, simultaneously by adding molten quantity to regulate and control the size of micella particulate, kills two birds with one stone.
Figure of description
Fig. 1 is the single dispersing of embodiment 1 preparation and the transmission electron microscope photo of the spherical micelle particulate of consolidation.
Embodiment
Embodiment 1
1. styrene monomer is washed with the sodium hydroxide solution of 10%, after removing stopper, wash excessive alkali lye with deionized water again, by pH detection paper after the aobvious neutrality of solution, add anhydrous sodium sulphate standing and drying 5h;
2. under the heating condition of 20torr pressure and 40 �� of C, dried styrene monomer being carried out underpressure distillation process, the styrene monomer after purifying is stored in the camera bellows of 10 DEG C for subsequent use;
3. take 0.04g docosyl trimethylammonium bromide (C22TABr), 0.07g cetyl trimethylammonium bromide (C16TABr), 0.08g vinylbenzene in 1mL ethanolic soln, under 30 DEG C of constant temperature agitation conditions, in solution, drip the �� L deionized water that adds 150 with blue lattice TJ-1A type micro-injection pump, drip speed and be set to 20 �� L/min, after solution fully dissolves, continue constant temperature stir 2h;
4., under 30 DEG C of constant temperature agitation conditions, continuing to drip the massfraction adding water to deionized water in total solvent is 80wt%, and the solution prepared is put into after dripping 70 DEG C of baking oven preheating 1h;
5., under nitrogen atmosphere protection, in preheated solution, add the K that consumption is styrene monomer quality 1%2S2O4, under 70 DEG C of heating condition, cause styrene monomer polymerization, stop after reaction 2h;
As shown in Figure 1, size is about 30nm to the spherical micelle particulate of gained single dispersing and consolidation, and dispersity index is 0.10.
Embodiment 2
1. styrene monomer treatment process is the same;
2. take 0.04gC22TABr��0.07gC16TABr, 0.06g vinylbenzene, in 1mLEtOH solution, under 30 DEG C of constant temperature agitation conditions, drips the �� L deionized water that adds 150 in solution, drips speed and be set to 20 �� L/min, continue constant temperature and stir 2h after solution fully dissolves with blue lattice TJ-1A type micro-injection pump;
3., under 30 DEG C of constant temperature agitation conditions, continuing to drip the massfraction adding water to deionized water in total solvent is 85wt%, and the solution prepared is put into after dripping 70 DEG C of baking oven preheating 1h;
4., under nitrogen atmosphere protection, in preheated solution, add the K of styrene monomer quality 1%2S2O4, under 70 DEG C of heating condition, cause styrene monomer polymerization, stop after reaction 2h.
The spherical micelle particle size of gained consolidation is about 25nm, and dispersity index is 0.10.
Embodiment 3
1. styrene monomer treatment process is the same;
2. take 0.04gC22TABr��0.07gC16TABr, 0.04g vinylbenzene, in 1mLEtOH solution, under 30 DEG C of constant temperature agitation conditions, drips the �� L deionized water that adds 150 in solution, drips speed and be set to 20 �� L/min, continue constant temperature and stir 2h after solution fully dissolves with blue lattice TJ-1A type micro-injection pump;
3., under 30 DEG C of constant temperature agitation conditions, continuing to drip the massfraction adding water to deionized water in total solvent is 90wt%, and the solution prepared is put into after dripping 70 DEG C of baking oven preheating 1h;
4., under nitrogen atmosphere protection, in preheated solution, add the K of styrene monomer quality 1%2S2O4, under 70 DEG C of heating condition, cause styrene monomer polymerization, stop after reaction 2h.
The spherical micelle particle size of gained consolidation is about 20nm, and dispersity index is 0.10.
The foregoing is only the better embodiment of the present invention, all impartial changes done according to the present patent application patent scope, with modifying, all should belong to the covering scope of the present invention.
Claims (6)
1. the preparation method of a single dispersing consolidation micella particulate, it is characterized in that: taking the molten long alkane chain tensio-active agent of shipwreck, short alkane chain tensio-active agent and vinylbenzene as raw material, first by long alkane chain surfactant dissolves in cosolvent, add short alkane chain tensio-active agent and vinylbenzene again, stir; Then drip and add poor solvent deionized water, order about the micella that tensio-active agent is gathered into solubilising vinylbenzene, continue to add deionized water until excessive; Finally cause styrene polymerization, form the single dispersing of different-grain diameter and the globular micelle particulate of consolidation.
2. the preparation method of single dispersing consolidation micella particulate according to claim 1, it is characterized in that: the alkane chain carbonatoms of the long alkane chain tensio-active agent that described shipwreck is molten is 20 ~ 28, and the alkane chain carbonatoms of short alkane chain tensio-active agent is 10 ~ 18.
3. the preparation method of single dispersing consolidation micella particulate according to claim 1, it is characterised in that: described long alkane chain tensio-active agent and the mol ratio of short alkane chain tensio-active agent are 1:1 ~ 1:6.
4. the preparation method of single dispersing consolidation micella particulate according to claim 1, it is characterised in that: the concentration of the vinylbenzene of solubilising and the ratio of tensio-active agent total concn are 0.1:1 ~ 6:1.
5. the preparation method of single dispersing consolidation micella particulate according to claim 1, it is characterised in that: described cosolvent is methyl alcohol, ethanol, propyl alcohol, or methyl alcohol, ethanol, propyl alcohol and N, the one in the mixture of dinethylformamide.
6. the preparation method of single dispersing consolidation micella particulate according to claim 1, it is characterised in that: the add-on of deionized water reaches more than 80wt% with the massfraction of deionized water in total solvent and is as the criterion.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1516893A1 (en) * | 2002-06-03 | 2005-03-23 | Sanyo Chemical Industries, Ltd. | Micelle-containing organic polymer, organic polymer porous material and porous carbon material |
| CN101343254A (en) * | 2008-07-09 | 2009-01-14 | 中北大学 | Gemini surfactant containing triazine ring |
| CN103739122A (en) * | 2014-01-24 | 2014-04-23 | 福州大学 | Method for removing micro organic pollutants from tap water through Pluronic block copolymers |
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| KR20030051653A (en) * | 2000-09-21 | 2003-06-25 | 메르크 파텐트 게엠베하 | Polystyrene microspheres and a method for their production |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1516893A1 (en) * | 2002-06-03 | 2005-03-23 | Sanyo Chemical Industries, Ltd. | Micelle-containing organic polymer, organic polymer porous material and porous carbon material |
| CN101343254A (en) * | 2008-07-09 | 2009-01-14 | 中北大学 | Gemini surfactant containing triazine ring |
| CN103739122A (en) * | 2014-01-24 | 2014-04-23 | 福州大学 | Method for removing micro organic pollutants from tap water through Pluronic block copolymers |
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