CN107913641A - A kind of preparation method of microemulsion - Google Patents
A kind of preparation method of microemulsion Download PDFInfo
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- CN107913641A CN107913641A CN201711254507.XA CN201711254507A CN107913641A CN 107913641 A CN107913641 A CN 107913641A CN 201711254507 A CN201711254507 A CN 201711254507A CN 107913641 A CN107913641 A CN 107913641A
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- microemulsion
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- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
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Abstract
The invention discloses a kind of preparation method of microemulsion.It is an object of the invention to for existing self-microemulsion technology there are the defects of, there is provided it is a kind of have extensively using property microemulsion prepare formula.The present invention obtains stable reverse micro emulsion by the ratio between control surface activating agent (Span 80, OP 10, Triton X 114), cosurfactant (isopropanol), oily (hexamethylene) and water (deionized water).Result of study is according to substantial amounts of experimental data, successfully obtain the component formula scope of transparent and stable microemulsion formulation, the three-phase diagram of ratio between each component is drawn in success, stable microemulsion can be obtained by being prepared in the proportion of the present invention, and the present invention provides experiment and theoretical foundation for the preparation of microemulsion.
Description
Technical field
The present invention relates to a kind of preparation method of microemulsion.
Background technology
Microemulsion due to huge surface area, ultralow interfacial tension, strong solubilising power and nano grade discontinuous phase and
With important application value, it is widely used in clean fuel, extraction, pharmaceutical carrier, microreactor, food additives, profit
Oil additive etc., it may also be used for coating and prepare nano-particle etc..
Reverse micro emulsion is a kind of w/o type (water-in-oil type) drop stablized by surfactant interface film.Wherein water
Core is prepares the microreactor of nano material, its water core dimension limitation particle diameter of particle, can rubbing by water and surfactant
Size of that than determining water core.Micro emulsion method is compared with other chemical methods, and particle prepared by micro emulsion method is not easy to reunite, and size is controllable,
Good dispersion, and preparation process, equipment are simple, the method for micro emulsion method preparation nano material receives the pole of domestic and international scientific research personnel
Big to pay attention to, its application has expanded to nano particle preparation, pharmacy, medicine transmission, enzyme reaction, electrochemical reaction and polymerisation
Deng.
Microemulsion is typically to be existed by four oil, surfactant, cosurfactant, water (or electrolyte aqueous solution) components
Stable homogeneous, isotropism, appearance transparent or the almost transparent dispersion spontaneously formed under suitable ratio.Microemulsion
It can be prepared by two kinds of technical methods, first, being completed by accurately mixing one step of each component, second, using emulsifying device such as height
Pressure homogenizer etc. carries out emulsification completion, and second method prepares complexity, need to could be obtained by certain mechanical means stable
Microemulsion.The first technical method process equipment is simple, is the preferred option for preparing microemulsion.
The successful preparation of microemulsion has the matching ratio of each component strict demand, and selects and design microemulsion composition
It is complicated, time-consuming, and unpredictable, it is most of to be only specific to one kind currently in the numerous and relevant patent document of micro emulsion
The specific molten product of oil, produce a certain specific microemulsion product, do not have it is forward-looking and guiding can be commonly used
Each recipe ingredient matching ratio.
It is an object of the invention to for existing self-microemulsion technology there are the defects of, there is provided it is a series of have extensively should
Formula is prepared with the microemulsion of property.By substantial amounts of experimental data, the micro emulsion formula of liquid of searching system rule, is selected not the present invention
Same surfactant, research obtain stabilization by the ratio between control surface activating agent, cosurfactant, oil, water
Reverse micro emulsion.Result of study successfully obtains the proportion of transparent and stable microemulsion formulation, successfully draws ratio between each component
Three-phase diagram, prepare in the weight range of the present invention and can obtain stable microemulsion, the present invention matching somebody with somebody for microemulsion
System provides experiment and theoretical foundation.
The content of the invention
It is Span-80 (sorbitan fatty acids that this research, which prepares the surfactant that stable microemulsion is selected,
Ester), OP-10 (alkylphenol polyoxyethylene ether -10) and Triton X-114 (polyoxyethylene octane alkylphenol ether), help surface-active
Agent is isopropanol, and oil phase is hexamethylene, and water is mutually deionized water.The invention comprises the following steps：
A. by a certain amount of surfactant, help surface-active, oil phase form mixed solution, magneton stirring under will go from
Sub- water is instilled in mixed solution dropwise, and the moment solution that deionized water adds can become cloudy, as stirring can horse back bleach；Such as
After fruit instills deionized water, agitating solution cannot horse back bleach, stand 30min, liquid becomes clarification again, then continue to be added dropwise again
Deionized water 0.05mL；If liquid does not return to clarification, the water at this moment added can be considered the maximum appearance under the conditions of this
Water.Obtain preparing one group of component formula of microemulsion.
B. change the ratio of surfactant, cosurfactant and oil, repeat experimental procedure above, obtain preparing steady
Determine the series formula of microemulsion.Formula three-phase diagram is done according to the weight that each component adds, obtains the formula range of microemulsion.
C. different surfactants is selected, repeat step a, b, obtains different surfaces activating agent and prepare microemulsion
Series formula and three-phase diagram.
Brief description of the drawings
The proportioning three-phase diagram of each component when Fig. 1 surfactants are Span-80.
The proportioning three-phase diagram of each component when Fig. 2 surfactants are OP-10.
The proportioning three-phase diagram of each component when Fig. 3 surfactants are Triton X-114.
Embodiment
The present invention is further elaborated for application example below：
Embodiment 1
1st, at room temperature, surfactant Span-80 2.037g, cosurfactant isopropanol 6.004g, oil phase ring are weighed
Hexane 8.072g adds magneton stirring in beaker 1；
2nd, a clean beaker 2 separately is taken, pours into deionized water, weigh up the gross weight of beaker 2 and deionized water, and record
Lower gravimetric value, is denoted as m1=135.761g；
3rd, the deionized water in beaker 2 is taken with dropper, is added drop-wise to dropwise in beaker 1, the moment solution that deionized water adds
It can become cloudy, as stirring can horse back bleach；After deionized water is instilled, agitating solution cannot horse back bleach, stand
30min, liquid become clarification again again, then deionized water 0.05mL is added dropwise, and stand 30min, and liquid returns to clarification；Be added dropwise again from
Sub- water 0.05mL, stands 30min, and liquid does not return to clarification, stops that deionized water is added dropwise, and weighs the weight of beaker 2 at this time, remembers
For m2=134.580g；
4th, microemulsion can add maximum m (water)=m of deionized water at this time1-m2=1.181g, with surfactant
Weight is 1, and conversion each component ratio is m (table work): m (helps table): m (oil): m (water)=1: 2.947: 3.963: 0.580
5th, final each component ratio and weight percentage data are summarized in table 1, the data of embodiment 1 be tilted in table plus under
Line institute column data.
6th, three-phase diagram is done according to 1 each component ratio data of table, obtains attached drawing 1, each component when surfactant is Span80
Proportioning three-phase diagram.The region I that solid line includes in three-phase diagram is Span-80 when being surfactant, can prepare stablize it is anti-phase
The component formula scope of microemulsion.The data of embodiment 1 are the point of square in three-phase diagram.
The each group distribution ratio of microemulsion is prepared when 1 surfactant of table is Span-80
Embodiment 2
1st, at room temperature, OP-10 surfactants 2.033g, cosurfactant isopropanol 2.091g, oil phase hexamethylene are weighed
Alkane 4.045g adds magneton stirring in beaker 1；
2nd, a clean beaker 2 separately is taken, pours into deionized water, weigh up the gross weight of beaker 2 and deionized water, and record
Lower gravimetric value, is denoted as m1=112.021g；
3rd, the deionized water in beaker 2 is taken with dropper, is added drop-wise to dropwise in beaker 1, the moment solution that deionized water adds
It can become cloudy, as stirring can horse back bleach；After instilling deionized water, agitating solution cannot horse back bleach, stand
30min, liquid become clarification again again, then deionized water 0.05mL is added dropwise, and stand 30min liquid and do not return to clarification, stop being added dropwise
Deionized water, and the weight of beaker 2 is weighed, it is denoted as m2=110.715g；
4th, microemulsion can add maximum m (water)=m of deionized water at this time1-m2=1.306g, with surfactant
Weight is 1, and conversion each component ratio is m (table work): m (helps table): m (oil): m (water)=1: 1.029: 1.990: 0.642；
5th, final each component ratio and weight percentage data are summarized in table 2, the data of embodiment 2 be tilted in table plus under
Line institute column data.
6th, three-phase diagram is done according to 2 each component ratio data of table, obtains attached drawing 2, each component when surfactant is OP-10
Match three-phase diagram.The region I that solid line includes in three-phase diagram is OP-10 when being surfactant, can prepare stable reverse microemulsion
The component formula scope of liquid.The data of embodiment 2 are the point of square in three-phase diagram.
The each group distribution ratio of microemulsion is prepared when 2 surfactant of table is OP-10
Embodiment 3
1st, at room temperature, weigh surfactant Triton X-1142.032g, cosurfactant isopropanol 14.031g,
Oil phase hexamethylene 12.005g adds magneton stirring in beaker 1；
2nd, a clean beaker 2 separately is taken, pours into deionized water, weigh up the gross weight of beaker 2 and deionized water, and record
Lower gravimetric value, is denoted as m1=84.488g；
3rd, the deionized water in beaker 2 is taken with dropper, is added drop-wise to dropwise in beaker 1, the moment solution that deionized water adds
It can become cloudy, as stirring can horse back bleach；After instilling deionized water, agitating solution cannot horse back bleach, stand
30min, liquid become clarification again again, then deionized water 0.05mL is added dropwise, and stand 30min liquid and do not return to clarification, stop being added dropwise
Deionized water, and the weight of beaker 2 at this time is weighed, it is denoted as m2=79.479g；
4th, microemulsion can add maximum m (water)=m of deionized water at this time1-m2=5.009g, with surfactant
Weight is 1, and conversion each component ratio is m (table work): m (helps table): m (oil): m (water)=1: 6.905: 5.908: 2.465
5th, final each component ratio and weight percentage data are summarized in table 3, the data of embodiment 3 be tilted in table plus under
Line institute column data.
6th, three-phase diagram is done according to 3 each component ratio data of table, attached drawing 3 is obtained, when surfactant is Triton X-114
The proportioning three-phase diagram of each component.The region I that solid line includes in three-phase diagram is Triton X-114 when being surfactant, Neng Goupei
System stablizes the component formula scope of reverse micro emulsion.The data of embodiment 3 are the point of square in three-phase diagram.
The each group distribution ratio of microemulsion is prepared when 3 surfactant of table is Triton X-114
Claims (4)
1. a kind of preparation method of microemulsion, it is characterised in that including step in detail below：
(1) by a certain amount of surfactant (Span-80, OP-10, Triton X-114), cosurfactant (isopropanol),
Oily (hexamethylene) composition mixed solution, instills deionized water in mixed solution under magneton stirring dropwise；
(2) the moment solution that deionized water adds can become cloudy, as stirring can horse back bleach；If instill deionized water
Afterwards, agitating solution cannot horse back bleach, stand 30min, liquid becomes clarification again again, then continues dropwise addition deionized water
0.05mL；If liquid does not return to clarification, the water at this moment added can be considered the maximum moisture capacity under the conditions of this.Obtain
Prepare one group of component formula of microemulsion.
(3) change the addition of surfactant, cosurfactant and oil, repeat experimental procedure (1) (2), obtain preparing steady
Determine the series of components formula of microemulsion.The proportioning three-phase diagram of microemulsion is drawn according to each component ratio.
2. the preparation method of a kind of microemulsion according to claim 1, it is characterised in that surfactant is
During Span-80, surfactant percentage by weight is 3.13%-30.34%, and cosurfactant percentage by weight is
19.43%-54.73%, weight of oil percentage are 18.29%-69.11%, and water percentage by weight is 3.05%-18.93%.
A kind of 3. preparation method of microemulsion according to claim 1, it is characterised in that surfactant OP-
When 10, surfactant percentage by weight is 3.88%-21.45%, and cosurfactant percentage by weight is 18.60%-
59.13%, weight of oil percentage is 23.79%-63.01%, and water percentage by weight is 5.40%-22.50%.
4. the preparation method of a kind of microemulsion according to claim 1, it is characterised in that surfactant is
During Triton X-114, surfactant percentage by weight is 4.42%-14.25%, and cosurfactant percentage by weight is
23.65%-60.75%, weight of oil percentage are 24.80%-61.83%, and water percentage by weight is 5.90%-20.84%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110052736A (en) * | 2019-05-23 | 2019-07-26 | 中国计量大学 | A kind of preparation method of low-melting-point nano Tin Silver Copper Alloy |
| CN114804181A (en) * | 2022-04-18 | 2022-07-29 | 佛山集美精化科技有限公司 | Preparation process of barium sulfate |
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| CN114804181A (en) * | 2022-04-18 | 2022-07-29 | 佛山集美精化科技有限公司 | Preparation process of barium sulfate |
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Application publication date: 20180417 |