CN104525066A - Preparation method for monodisperse consolidation micelle particulate - Google Patents
Preparation method for monodisperse consolidation micelle particulate Download PDFInfo
- Publication number
- CN104525066A CN104525066A CN201510009162.6A CN201510009162A CN104525066A CN 104525066 A CN104525066 A CN 104525066A CN 201510009162 A CN201510009162 A CN 201510009162A CN 104525066 A CN104525066 A CN 104525066A
- Authority
- CN
- China
- Prior art keywords
- consolidation
- alkane chain
- preparation
- surfactant
- deionized water
- 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.)
- Granted
Links
Classifications
-
- 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 invention relates to a preparation method for monodisperse consolidation micelle particulates. The preparation method comprises the following steps that water-insoluble long alkane chain surfactants, short alkane chain surfactants and styrene are used as raw materials, the long alkane chain surfactants are dissolved in a cosolvent, the short alkane chain surfactants and the styrene are added into the cosolvent, and the mixture is stirred fully and evenly; deionized water is dropped into the mixture to drive the mixture to gather and a micelle solubilizing the styrene is formed, and the deionized water is continuously added until the deionized water is excessive; styrene polymerization is triggered to form monodisperse and consolidation spherical micelle particulates with different particle sizes. The monodisperse consolidation micelle particulates can act as units of novel colloidal crystal lattice arrangement, and novel colloidal crystal function materials are further prepared.
Description
Technical field
The invention belongs to technical field of function materials, relate to a kind of preparation method of single dispersing consolidation micellar particles.
Background technology
Colloidal crystal is by the inorganic or polymeric colloid microballoon of diameter at sub-micron or Nano grade, size monodisperse, under the effects such as gravity, electrostatic force or capillary force, the aggregation of the two dimension that self assembly is formed or three-dimensional close stacked arrangement (respect by fourth, Deng, chemical progress, 2004,16,321 ~ 326.; Xia, Y.;
et al.
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 (de Villeneuve, V.;
et al.
science2005,309,1231 ~ 1233.; Alsayed, A.;
et al.
science2005,309,1207 ~ 1210.; Pham, K.;
et al.
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, can be developed to important nonlinear optical material thus.Colloidal crystal can be used as photonic crystal to use, 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 apparatus synthesis template, can the nanoparticle of inducing function in self assembly above, object (Yang, the S. of practical function implementation; Lei, Y.
nanoscale2011,3,2768 ~ 2782.).
Prepare colloidal crystal requirement particulate unit and there is good monodispersity, therefore silica, polystyrene and polyacrylamide microsphere is depended on so far, and inorganic nano-particle, the size of these microballoons or particulate in hundreds of nanometer until micron, or below 10 nanometers, in the middle of lacking, the particulate of dimension, which has limited colloidal crystal in development to a greater extent.
Summary of the invention
The object of this invention is to provide a kind of preparation method of single dispersing consolidation micellar particles.The present invention breaches Traditional Thinking, utilize surfactant 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 micellar particles, make it the new unit becoming preparation new colloidal crystal lattice.
In order to reach the object of the invention, adopt following technical scheme:
A kind of preparation method of single dispersing consolidation micellar particles: with molten long alkane chain surfactant, short alkane chain surfactant and the styrene of shipwreck for raw material, first by long alkane chain surfactant dissolves in cosolvent, add short alkane chain surfactant and styrene again, stir; Then drip deionized water, order about surfactant and be gathered into the cinnamic micella of solubilising, 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 carbon number of the long alkane chain surfactant that described shipwreck is molten is 20 ~ 28, and the alkane chain carbon number of short alkane chain surfactant is 10 ~ 18.
Described long alkane chain surfactant and the mol ratio of short alkane chain surfactant are 1:1 ~ 1:6.
The cinnamic concentration of solubilising and the ratio of surfactant total concentration are between 0.1:1 to 6:1.
Described cosolvent is methyl alcohol, ethanol, propyl alcohol, or the one in the mixture of methyl alcohol, ethanol, propyl alcohol and DMF.
Wherein, the addition of deionized water with deionized water in total solvent the mass fraction of (deionized water and cosolvent) reach more than 80wt% and be as the criterion.
Preparation method of the present invention is different from the preparation of neat polymer particulate, but the single dispersing micella directly utilizing surfactant self-organizing to be formed.The object that solubilized styrene is also polymerized is in order to consolidation micella and regulation and control size.This method can obtain very little organic fine particles, also eliminates numerous and diverse formality of removing surfactant templates in the preparation of neat polymer particulate.
Remarkable advantage of the present invention is:
1, the present invention first allows the molten long alkane chain surfactant of shipwreck dissolve in cosolvent, under short alkane chain surfactant coordinates, relies on the realization that adds of poor solvent water to organize themselves into as single dispersing micella; The method breaches the long standing difficulty of the molten long alkane chain surfactant investigation and application of shipwreck, to expansion its research and practical application significant;
2, synchronous solubilization styrene in single dispersing micelle forma-tion process, the cinnamic polymerization of recycling solubilization realizes the consolidation of micellar particles, regulates and controls the size of micellar particles simultaneously, kill two birds with one stone by solubilization quantity.
figure of description
Fig. 1 be embodiment 1 prepare single dispersing and the transmission electron microscope photo of the spherical micelle particulate of consolidation.
Detailed description of the invention
embodiment 1
1., by the styrene monomer sodium hydroxide solution washing of 10%, wash away excessive alkali lye by deionized water again after removing polymerization inhibitor, show after neutrality by pH detection paper until solution, add anhydrous sodium sulfate standing and drying 5h;
2., under the heating condition of 20 torr pressure and 40 ° of C, carry out decompression distillation process to dried styrene monomer, the styrene monomer after purifying is stored in the camera bellows of 10 DEG C for subsequent use;
3. take 0.04g behenyl ammonium bromide (C
22tABr), 0.07g softex kw (C
16tABr), 0.08g styrene is in 1mL ethanolic solution, under 30 DEG C of constant temperature stirring conditions, in solution, drip 150 μ L deionized waters with Lange TJ-1A type micro-injection pump, drip speed and be set to 20 μ L/min, after solution fully dissolves, continue constant temperature stir 2h;
4., under 30 DEG C of constant temperature stirring conditions, continuing to drip the mass fraction adding water to deionized water in total solvent is 80wt%, the solution prepared is put into 70 DEG C of baking oven preheating 1h after dripping;
5., under nitrogen atmosphere protection, in preheated solution, add the K that consumption is styrene monomer quality 1%
2s
2o
4, under 70 DEG C of heating condition, cause styrene monomer polymerization, stop after reaction 2h;
As shown in Figure 1, size is about 30nm, and decentralization index is 0.10 for gained single dispersing and the spherical micelle particulate of consolidation.
embodiment 2
1. styrene monomer processing method is the same;
2. take 0.04g C
22tABr, 0.07g C
16tABr, 0.06g styrene, in 1mL EtOH solution, under 30 DEG C of constant temperature stirring conditions, drips 150 μ L deionized waters with Lange TJ-1A type micro-injection pump in solution, drips speed and is set to 20 μ L/min, continues constant temperature and stir 2h after solution fully dissolves;
3., under 30 DEG C of constant temperature stirring conditions, continuing to drip the mass fraction adding water to deionized water in total solvent is 85wt%, the solution prepared is put into 70 DEG C of baking oven preheating 1h after dripping;
4., under nitrogen atmosphere protection, in preheated solution, add the K of styrene monomer quality 1%
2s
2o
4, 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 decentralization index is 0.10.
embodiment 3
1. styrene monomer processing method is the same;
2. take 0.04g C
22tABr, 0.07g C
16tABr, 0.04g styrene, in 1mL EtOH solution, under 30 DEG C of constant temperature stirring conditions, drips 150 μ L deionized waters with Lange TJ-1A type micro-injection pump in solution, drips speed and is set to 20 μ L/min, continues constant temperature and stir 2h after solution fully dissolves;
3., under 30 DEG C of constant temperature stirring conditions, continuing to drip the mass fraction adding water to deionized water in total solvent is 90wt%, the solution prepared is put into 70 DEG C of baking oven preheating 1h after dripping;
4., under nitrogen atmosphere protection, in preheated solution, add the K of styrene monomer quality 1%
2s
2o
4, 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 decentralization index is 0.10.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (6)
1. the preparation method of a single dispersing consolidation micellar particles, it is characterized in that: with molten long alkane chain surfactant, short alkane chain surfactant and the styrene of shipwreck for raw material, first by long alkane chain surfactant dissolves in cosolvent, add short alkane chain surfactant and styrene again, stir; Then drip poor solvent deionized water, order about surfactant and be gathered into the cinnamic micella of solubilising, 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 micellar particles according to claim 1, it is characterized in that: the alkane chain carbon number of the long alkane chain surfactant that described shipwreck is molten is 20 ~ 28, and the alkane chain carbon number of short alkane chain surfactant is 10 ~ 18.
3. the preparation method of single dispersing consolidation micellar particles according to claim 1, is characterized in that: described long alkane chain surfactant and the mol ratio of short alkane chain surfactant are 1:1 ~ 1:6.
4. the preparation method of single dispersing consolidation micellar particles according to claim 1, is characterized in that: the cinnamic concentration of solubilising and the ratio of surfactant total concentration are 0.1:1 ~ 6:1.
5. the preparation method of single dispersing consolidation micellar particles according to claim 1, is characterized in that: described cosolvent is methyl alcohol, ethanol, propyl alcohol, or the one in the mixture of methyl alcohol, ethanol, propyl alcohol and DMF.
6. the preparation method of single dispersing consolidation micellar particles according to claim 1, is characterized in that: the addition of deionized water reaches more than 80wt% with the mass fraction of deionized water in total solvent and is as the criterion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510009162.6A CN104525066B (en) | 2015-01-09 | 2015-01-09 | The preparation method of a kind of single dispersing consolidation micella particulate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510009162.6A CN104525066B (en) | 2015-01-09 | 2015-01-09 | The preparation method of a kind of single dispersing consolidation micella particulate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104525066A true CN104525066A (en) | 2015-04-22 |
| CN104525066B CN104525066B (en) | 2016-06-01 |
Family
ID=52840799
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510009162.6A Expired - Fee Related CN104525066B (en) | 2015-01-09 | 2015-01-09 | The preparation method of a kind of single dispersing consolidation micella particulate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104525066B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542045A (en) * | 2016-01-15 | 2016-05-04 | 福州大学 | Method for preparing rodlike micelle with consolidated structure |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040012105A1 (en) * | 2000-09-21 | 2004-01-22 | Holger Deppe | Polystyrene microspheres and a method for their production |
| 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 |
-
2015
- 2015-01-09 CN CN201510009162.6A patent/CN104525066B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040012105A1 (en) * | 2000-09-21 | 2004-01-22 | Holger Deppe | Polystyrene microspheres and a method for their production |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542045A (en) * | 2016-01-15 | 2016-05-04 | 福州大学 | Method for preparing rodlike micelle with consolidated structure |
| CN105542045B (en) * | 2016-01-15 | 2018-01-12 | 福州大学 | A kind of preparation method of the rod-shaped micelle of structure consolidation |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104525066B (en) | 2016-06-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Nandiyanto et al. | Synthesis of additive-free cationic polystyrene particles with controllable size for hollow template applications | |
| Oliveira et al. | Controlled precipitation of zinc oxide particles at room temperature | |
| Li et al. | Fabrication of industrial-level polymer photonic crystal films at ambient temperature Based on uniform core/shell colloidal particles | |
| Zhang et al. | Microfluidic‐Spinning‐Directed Microreactors Toward Generation of Multiple Nanocrystals Loaded Anisotropic Fluorescent Microfibers | |
| Duan et al. | Synthesis and characterization of poly (N-isopropylacrylamide)/silica composite microspheres via inverse Pickering suspension polymerization | |
| WO2014154148A1 (en) | Preparation method and use of color saturation variable photonic crystal material | |
| Zhang et al. | Construction of silver tungstate multilevel sphere clusters by controlling the energy distribution on the crystal surface | |
| CN105273190A (en) | Polysulfide rubber nanoparticles and preparing method and application thereof | |
| CN101468817B (en) | Mesoporous nanocrystalline assembled porous bengala microsphere and preparation thereof | |
| CN104028775A (en) | Preparation method for monodisperse uniform-particle-size silver nanoparticles | |
| Wang et al. | Synthesis of monodisperse hollow silver spheres using phase-transformable emulsions as templates | |
| CN102515245A (en) | Method for controllably synthesizing nano zinc oxide based on solvent heat | |
| Zhang et al. | A facile route to mono-dispersed CeO2 nanocubes and their enhanced photocatalytic properties | |
| CN108726554A (en) | One kind efficiently preparing evengranular nano barium sulfate method | |
| Liu et al. | Magnetic field induced formation of visually structural colored fiber in micro-space | |
| CN104549374B (en) | Cadmium selenide flower-like microsphere being made up of nanometer sheet with water-wetted surface and its preparation method and application | |
| Tian et al. | Rapid visualized hydrophobic-force-driving self-assembly towards brilliant photonic crystals | |
| CN104692454A (en) | Method for preparing lead sulfide nano-particles through reflux precipitation | |
| CN104525066B (en) | The preparation method of a kind of single dispersing consolidation micella particulate | |
| CN102492300B (en) | Preparation method of monodispersing fibroin particles and preparation method of photonic crystal | |
| Guo et al. | Carbon spheres surface modification and dispersion in polymer matrix | |
| Yu et al. | Patternable structural color prepared by using photonic crystal paints with high solid content | |
| Wang et al. | Preparation of high efficiency hollow TiO2 nanospheres for electrophoretic displays | |
| Li et al. | A microfluidics‐dispensing‐printing strategy for Janus photonic crystal microspheres towards smart patterned displays | |
| CN103214340B (en) | Triptycene organic nano-material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160601 Termination date: 20190109 |