CN105542045B - A kind of preparation method of the rod-shaped micelle of structure consolidation - Google Patents
A kind of preparation method of the rod-shaped micelle of structure consolidation Download PDFInfo
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- CN105542045B CN105542045B CN201610025941.XA CN201610025941A CN105542045B CN 105542045 B CN105542045 B CN 105542045B CN 201610025941 A CN201610025941 A CN 201610025941A CN 105542045 B CN105542045 B CN 105542045B
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- rod
- styrene
- shaped micelle
- surfactant
- preparation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/06—Organic solvent
- C08F2/08—Organic solvent with the aid of dispersing agents for the polymer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/07—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Colloid Chemistry (AREA)
Abstract
The present invention relates to a kind of preparation method of the rod-shaped micelle of structure consolidation.Using long chain alkyl ammonium salt surfactant, organic salt conditioning agent and styrene as raw material, first long chain alkyl ammonium salt surfactant, organic salt conditioning agent and styrene are dissolved in cosolvent, stirred；Then poor solvent deionized water is added dropwise, the rod-shaped micelle for driving surfactant to be gathered into solubilized styrene, continues plus deionized water is up to excess；Finally trigger styrene polymerization, form the single dispersing of different-grain diameter and the rod-shaped micelle particulate of consolidation.The unit that single dispersing consolidation micellar particles can arrange as new colloidal crystal lattice, and then prepare new colloidal crystal functional material.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of preparation method of the rod-shaped micelle of structure consolidation.
Background technology
Colloidal crystal be by diameter in sub-micron or Nano grade, the inorganic or polymeric colloid particulate of size monodisperse,
Under the effect such as gravity, electrostatic force or capillary force, the two dimension or the aggregation of three-dimensional close stacked arrangement that are self-assembly of（Ding Jing
Deng, chemical progress, 2004,16,321 ~ 326.；Xia, Y.;et al. Adv. Mater. 2000, 12, 693~
713.）.Colloidal crystal has important science and application value：（1）It can as model system research crystal growth and
Fusing（de Villeneuve, V.;et al. Science2005, 309, 1231~1233.；Alsayed, A.;et al. Science2005, 309, 1207~1210.；Pham, K.;et al. Science 2002, 296, 104~
106.；Zhang, K.; Liu, X. Y.Nature2004, 429, 739~743.）；（2）Colloidal crystal is due to periodically
Structure and there is energy gap, therefore there is specific optical diffraction and optical band gap property, it is possible thereby to develop into important non-linear
Optical material.Colloidal crystal can be used as photonic crystal to use, and special light property makes colloidal crystal be expected to be used for modulated electromagnetic
Ripple transports（Li Hang, etc., chemical progress, 2011,23,1060 ~ 1068）；（3）Two-dimensional colloidal crystal is good nanometer device
Tool synthesizes template, can realize the purpose of function implementation with the nanoparticle of inducing function in self assembly above（Yang,
S.; Lei, Y. Nanoscale2011, 3, 2768~2782.）.
Preparing colloidal crystal requirement particulate unit has good monodispersity, so far dependent on silica, polyphenyl second
The size of alkene and polyacrylamide microsphere, and inorganic nano-particle, these microballoons or particulate at hundreds of nanometers until micron, or
Below 10 nanometers of person, lack the particulate of middle dimension, also lack the pattern different from ball, these limit colloidal crystal bigger
Development in degree.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the rod-shaped micelle of structure consolidation.The present invention passes through organic salt
Conditioning agent regulates and controls aggregation pattern into bar-shaped, is re-introduced into curing mechanism, it is achieved thereby that single dispersing consolidation rod-shaped micelle particulate
Prepare, make the new unit for preparing new colloidal crystal lattice.
In order to reach the object of the invention, adopt the following technical scheme that：
A kind of preparation method of the rod-shaped micelle of structure consolidation：Adjusted with long chain alkyl ammonium salt surfactant, organic salt
It is raw material to save agent and styrene, is first dissolved in long chain alkyl ammonium salt surfactant, organic salt conditioning agent and styrene altogether
In solvent, stir；Then poor solvent deionized water is added dropwise, drives surfactant to be gathered into styrene solubilized
Rod-shaped micelle, continue plus deionized water be until excess；Finally trigger styrene polymerization, form the single dispersing of different-grain diameter and consolidate
The rod-shaped micelle particulate of knot.
The long alkane chain carbon number of described long chain alkyl ammonium salt surfactant is 16 ~ 20.
Described organic salt conditioning agent is benzene sulfonate or naphthalene sulfonate.
The ratio of the mass concentration of the styrene of solubilising and the mass concentration of surfactant is 1:1~8:1.
Described cosolvent includes one kind in methanol, ethanol or propyl alcohol.
Wherein, the addition of deionized water with deionized water in total solvent（Deionized water and cosolvent）Mass fraction
Reach more than 85wt% to be defined.
The preparation method of the present invention is different from the preparation of neat polymer particulate, but directly utilizes surfactant from group
Knit the single dispersing micella to be formed.Solubilized styrene and the purpose being polymerize are to consolidate micella.This method can obtain very
Small organic fine particles, also eliminate numerous and diverse formality that surfactant templates are removed in prepared by neat polymer particulate.
The present invention remarkable advantage be：
1st, the present invention first allows long chain alkyl ammonium salt surfactant to be dissolved in cosolvent, in organic salt adjustment control
Under, realize and organized themselves into as monodispersed rod-shaped micelle by the addition of poor solvent water；The preparation method breaches long alkane
The problem that based quaternary ammonium salt surfactant not readily dissolves, it is significant to expanding its research and practical application；
2nd, synchronous solubilization styrene during single dispersing micelle forma-tion, the polymerization of solubilization styrene is recycled to realize glue
The consolidation of beam particulate.
Figure of description
Fig. 1 is the transmission electron microscope photo of single dispersing prepared by embodiment 1 and the rod-shaped micelle particulate of consolidation.
Embodiment
The present invention further illustrates the present invention with the following example, but protection scope of the present invention is not limited to following reality
Apply example.
Embodiment 1
A kind of preparation method of rod-shaped micelle：
1）Styrene monomer is washed with 10 wt% sodium hydroxide solutions, was washed with deionized water again after removing polymerization inhibitor
The alkali lye of amount, with the detection of pH test paper after the aobvious neutrality of solution, add the h of anhydrous sodium sulfate standing and drying 5；In 20 torr pressure and
Under 40 DEG C of heating condition, vacuum distillation processing is carried out to dried styrene monomer, styrene monomer storage after purification
It is standby in 10 DEG C of camera bellows；
2）Weigh 0.0943 g Cetyltrimethylammonium bromides（C18TABr）, 0.0277 g sodium naphthalene sulfonates（SNphs）、
0.16 g styrene is in 1 mL ethanol solutions, under 30 DEG C of constant temperature stirring conditions, with Lange TJ-1A types micro-injection pump to
150 μ L deionized waters are added dropwise in solution, drop speed is arranged to 20 μ L/min, continues constant temperature after solution fully dissolves and stirs 2 h；
3）Under 30 DEG C of constant temperature stirring conditions, it is 90 to continue to drip the mass fraction for adding water to deionized water in total solvent
Wt%, the solution prepared is put into 70 DEG C of baking ovens after dripping and preheats 1h；
4）Under nitrogen atmosphere protection, it is the wt%'s of styrene monomer quality 1 that dosage is added into preheated solution
K2S2O4, trigger styrene monomer polymerization under 70 DEG C of heating conditions, stop after reacting 2 h；
Gained single dispersing and the rod-shaped micelle particulate of consolidation disperse as shown in figure 1, length about 70 nm, diameter 8-10 nm
It is 0.12 to spend index.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (5)
- A kind of 1. preparation method of the rod-shaped micelle of structure consolidation, it is characterised in that：With long chain alkyl ammonium salt surfactant, Organic salt conditioning agent and styrene are raw material, first by long chain alkyl ammonium salt surfactant, organic salt conditioning agent and styrene It is dissolved in cosolvent, stirs；Then poor solvent deionized water is added dropwise, drives surfactant to be gathered into solubilising The rod-shaped micelle of styrene, continues plus deionized water is until excess；Finally trigger styrene polymerization, form the list of different-grain diameter Scattered and consolidation rod-shaped micelle particulate；The long alkane chain carbon number of described long chain alkyl ammonium salt surfactant is 16 ~ 20；Described organic salt conditioning agent is benzene sulfonate or naphthalene sulfonate.
- 2. the preparation method of the rod-shaped micelle of structure consolidation according to claim 1, it is characterised in that：Described long alkane The mol ratio of based quaternary ammonium salt surfactant and organic salt conditioning agent is 1:0.1~1:6.
- 3. the preparation method of the rod-shaped micelle of structure consolidation according to claim 1, it is characterised in that：The styrene of solubilising Mass concentration and surfactant mass concentration ratio be 1:1~8:1.
- 4. the preparation method of the rod-shaped micelle of structure consolidation according to claim 1, it is characterised in that：Described cosolvent Including one kind in methanol, ethanol or propyl alcohol.
- 5. the preparation method of the rod-shaped micelle of structure consolidation according to claim 1, it is characterised in that：Deionized water adds Enter mass fraction of the amount by deionized water in total solvent and reach more than 85wt% to be defined.
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| CN201610025941.XA CN105542045B (en) | 2016-01-15 | 2016-01-15 | A kind of preparation method of the rod-shaped micelle of structure consolidation |
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| CN105542045B true CN105542045B (en) | 2018-01-12 |
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Citations (4)
| 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 |
| CN104525066A (en) * | 2015-01-09 | 2015-04-22 | 福州大学 | Preparation method for monodisperse consolidation micelle particulate |
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2016
- 2016-01-15 CN CN201610025941.XA patent/CN105542045B/en not_active Expired - Fee Related
Patent Citations (4)
| 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 |
| CN104525066A (en) * | 2015-01-09 | 2015-04-22 | 福州大学 | Preparation method for monodisperse consolidation micelle particulate |
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