CN105251418A - Method for preparing Pickering microemulsion gel from poly-o-phenylenediamine - Google Patents
Method for preparing Pickering microemulsion gel from poly-o-phenylenediamine Download PDFInfo
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- CN105251418A CN105251418A CN201510747796.1A CN201510747796A CN105251418A CN 105251418 A CN105251418 A CN 105251418A CN 201510747796 A CN201510747796 A CN 201510747796A CN 105251418 A CN105251418 A CN 105251418A
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Abstract
The invention discloses a method for preparing Pickering microemulsion gel from poly-o-phenylenediamine. The method comprises the steps: 1, adding 0.5ml of an oil-phase solvent into 1.0ml of a 0.15-0.2mol/L o-phenylenediamine aqueous solution to obtain a solution, oscillating the solution, and performing ultrasound operation under the frequency being 60-80Hz for 10-20min until the solution becomes a milky-state turbid liquid; and 2, adding 5mu L of a 0.4-0.55mol/L FeCl3 solution under an ultrasound condition until yellow-green sediment is generated in the solution, further performing ultrasound operation for 10-20m, standing for reaction for 8-12d to obtain a product distributed on an oil-water interface in a gel state, and removing superfluous water-phase and oil-phase solutions to obtain the Pickering microemulsion gel containing the stable poly-o-phenylenediamine. The method is simple, high in repeatability and the universality, and suitable for a plurality of oil phases; and all the steps can be performed under room temperature, and heating is not required.
Description
Technical field
The present invention relates to a kind of preparation method of Pickering microemulsion gel, particularly relate to a kind of method preparing the stable Pickering microemulsion of poly-o-phenylenediamine oligomer in metastable state liquid phase environment.
Background technology
The dispersion that emulsion is made up of two kinds of immiscible liquid phases, wherein one is scattered in another phase with the form of drop, there is larger oil/water interface in system, is a kind of thermodynamic unstable system.Emulsion to be in dynamic stabilization state to need in system, to add the third material, normally surfactant or nano particle.The stability that Pickering microemulsion is derives from solid particle and is adsorbed on oil/water interface, and forms the membranoid substance of individual layer or multilayer.Because the stability of Pickering microemulsion is strong, so have important using value in medicine, foods and cosmetics field.
Summary of the invention
The present invention relates to a kind of method utilizing poly-o-phenylenediamine to prepare Pickering microemulsion gel, in the metastable state environment that oil/water is formed, the oxidation of oxidized dose of o-phenylenediamine forms poly-o-phenylenediamine oligomer, poly-o-phenylenediamine oligomer is adsorbed on oil/water interface, thus defines the stable Pickering microemulsion of poly-o-phenylenediamine.Owing to there is non-covalent bond active force between poly-o-phenylenediamine oligomer, when oil phase is excessive, define the Pickering gel that poly-o-phenylenediamine is stable.
A kind of method utilizing poly-o-phenylenediamine to prepare Pickering microemulsion gel, utilize the research object that conducting polymer o-phenylenediamine is solid particle, in the liquid phase environment of inferior stable state, oxidant is utilized to produce poly-o-phenylenediamine oligomer, poly-o-phenylenediamine oligomer is adsorbed on oil/water interface, thus defines the stable Pickering microemulsion of poly-o-phenylenediamine oligomer.Concrete steps are as follows:
One, in 1.0ml, 0.15 ~ 0.2mol/L o-phenylenediamine aqueous solution, 0.5ml oil phase solvent (hexane, toluene, chlorobenzene, benzinum, ethyl acetate, decane etc.) is added, solution is vibrated, under the frequency of 60 ~ 80Hz ultrasonic 10 ~ 20 minutes, solution was milky suspension;
Two, under ultrasonic condition, in suspension, add the FeCl of 5 μ L, 0.4 ~ 0.55mol/L
3, there is a large amount of yellow-green precipitates in solution, after continuing ultrasonic 10 ~ 20 minutes in solution, leave standstill reaction 8 ~ 12 days, product is that gel is distributed on oil-water interfaces, removes unnecessary aqueous phase and oil-phase solution, obtains the Pickering microemulsion gel that poly-o-phenylenediamine is stable.
Tool of the present invention has the following advantages:
1, this technology utilization poly-o-phenylenediamine successfully achieves the stable of oil/water interface, has prepared Pickering microemulsion;
2, there is non-covalent bond active force between poly-o-phenylenediamine oligomer, after therefore defining Pickering microemulsion on oil/water interface, define spawn immediately;
3, in spawn containing a large amount of microemulsion ingredients, for the storage of microemulsion and release provide a kind of new method;
4, the method adopts FeCl
3for oxidant, substantially increase the speed of oxidation, the poly-o-phenylenediamine granule-morphology formed is homogeneous;
5, this preparation technology is simple to operate, and repeatability and universality are by force, all applicable to multiple oil phase solvent;
6, the institute of this technique carries out in steps all at ambient temperature, without the need to heating.
Accompanying drawing explanation
The Pickering microemulsion light microscope shape appearance figure that the poly-o-phenylenediamine of Fig. 1 prepared by embodiment 1 is stable;
The Pickering microemulsion light microscope shape appearance figure that the poly-o-phenylenediamine of Fig. 2 prepared by embodiment 2 is stable.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
embodiment 1:
In the poly-o-phenylenediamine aqueous solution that 1.0ml, 0.2mol/L newly configure, add 0.5ml toluene, vibrated by solution, under the frequency of 70Hz ultrasonic 15 minutes, solution was milky suspension.In suspension, the FeCl of 5 μ L, 0.5mol/L is added under ultrasonic condition
3, there is a large amount of yellow-green precipitates in solution, after continuing ultrasonic 15 minutes in solution, leave standstill reaction 10 days, product is that gel is distributed on oil-water interfaces, removes unnecessary aqueous phase and oil-phase solution, obtains the Pickering microemulsion gel (Fig. 1) that poly-o-phenylenediamine is stable.
embodiment 2:
In the poly-o-phenylenediamine aqueous solution that 1.0ml, 0.18mol/L newly configure, add 0.5ml decane, vibrated by solution, under the frequency of 70Hz ultrasonic 15 minutes, solution was milky suspension.In suspension, the FeCl of 5 μ L, 0.5mol/L is added under ultrasonic condition
3, there is a large amount of yellow-green precipitates in solution, after continuing ultrasonic 15 minutes in solution, leave standstill reaction 10 days, product is that gel is distributed on oil-water interfaces, removes unnecessary aqueous phase and oil-phase solution, obtains the Pickering microemulsion gel (Fig. 2) that poly-o-phenylenediamine is stable.
Claims (2)
1. utilize poly-o-phenylenediamine to prepare a method for Pickering microemulsion gel, it is characterized in that described method step is as follows:
One, in 1.0ml, 0.15 ~ 0.2mol/L o-phenylenediamine aqueous solution, add 0.5ml oil phase solvent, vibrated by solution, under the frequency of 60 ~ 80Hz ultrasonic 10 ~ 20 minutes, solution was milky suspension;
Two, under ultrasonic condition, in suspension, add the FeCl of 5 μ L, 0.4 ~ 0.55mol/L
3, there is yellow-green precipitate in solution in solution, after continuing ultrasonic 10 ~ 20 minutes, leave standstill reaction 8 ~ 12 days, product is that gel is distributed on oil-water interfaces, removes unnecessary aqueous phase and oil-phase solution, obtains the Pickering microemulsion gel that poly-o-phenylenediamine is stable.
2. the method utilizing poly-o-phenylenediamine to prepare Pickering microemulsion gel according to claim 1, is characterized in that described oil phase solvent is hexane, toluene, chlorobenzene, benzinum, ethyl acetate or decane.
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| CN201510747796.1A CN105251418B (en) | 2015-11-06 | 2015-11-06 | Method for preparing Pickering microemulsion gel from poly-o-phenylenediamine |
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| CN201510747796.1A CN105251418B (en) | 2015-11-06 | 2015-11-06 | Method for preparing Pickering microemulsion gel from poly-o-phenylenediamine |
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| CN105251418A true CN105251418A (en) | 2016-01-20 |
| CN105251418B CN105251418B (en) | 2017-04-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511397A (en) * | 2019-09-02 | 2019-11-29 | 哈尔滨工业大学 | A method of Pickering lotion is prepared based on oil-water interfaces oxidative polymerization method fabricated in situ poly-o-phenylenediamine fiber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1369478A (en) * | 2001-02-16 | 2002-09-18 | 中国科学院长春应用化学研究所 | Process for synthesizing oligomer of phenylamine |
| CN104231179A (en) * | 2014-08-29 | 2014-12-24 | 江苏科技大学 | Preparation method of polymethyl methacrylate macroporous microsphere adsorbent |
| CN104892833A (en) * | 2015-05-21 | 2015-09-09 | 安徽大学 | Preparation method of polyacrylic acid hollow microgel |
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2015
- 2015-11-06 CN CN201510747796.1A patent/CN105251418B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1369478A (en) * | 2001-02-16 | 2002-09-18 | 中国科学院长春应用化学研究所 | Process for synthesizing oligomer of phenylamine |
| CN104231179A (en) * | 2014-08-29 | 2014-12-24 | 江苏科技大学 | Preparation method of polymethyl methacrylate macroporous microsphere adsorbent |
| CN104892833A (en) * | 2015-05-21 | 2015-09-09 | 安徽大学 | Preparation method of polyacrylic acid hollow microgel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511397A (en) * | 2019-09-02 | 2019-11-29 | 哈尔滨工业大学 | A method of Pickering lotion is prepared based on oil-water interfaces oxidative polymerization method fabricated in situ poly-o-phenylenediamine fiber |
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