CN102728252B - Method for preparing multiple emulsions from layered active particles - Google Patents
Method for preparing multiple emulsions from layered active particles Download PDFInfo
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- CN102728252B CN102728252B CN201110082231.8A CN201110082231A CN102728252B CN 102728252 B CN102728252 B CN 102728252B CN 201110082231 A CN201110082231 A CN 201110082231A CN 102728252 B CN102728252 B CN 102728252B
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Abstract
A method for preparing multiple emulsions from layered active particles comprises steps of: preparing a surfactant oily solution, a water-in-oil emulsion and a layered active particle water dispersion system and further preparing a water-in-oil-in-water multiple emulsion. The preparation technology comprises the following steps of: (A) preparing the surfactant oily solution with the mass concentration of 1.0-4.0%; (B) gradually adding clear water into the surfactant oily solution at the stirring rate of 800-1200 r/s to obtain the water-in-oil emulsion; (C) preparing the layered active particle water dispersion system with the mass concentration of 0.5-1.5%; and (D) gradually adding the water-in-oil emulsion into the layered active particle water dispersion system at the high stirring rate of 3000-5000 r/s to obtain the oil-in-water water-covering multiple emulsions. The method provided by the invention has characteristics of long stabilization time, small amount of the surfactant, low cost, safety, environmental protection, no toxic and side effect and the like, and is widely applied in petroleum exploitation technologies.
Description
Technical field
The preparation method who the present invention relates to the multiple-phase emulsion that profile control aspect, oil exploitation stratum is applied to, particularly stratiform active particle is prepared the method for multiple-phase emulsion.
Background technology
Tradition is prepared the method for multiple-phase emulsion, generally to utilize two kinds of surfactants to be prepared, although this preparation method has prepared the multiple-phase emulsion of profile control aspect, oil field application, for the profile control technology of oilfield exploitation has been made contribution, but it exists following shortcoming or deficiency simultaneously: 1. stabilization time is short, surfactant forms rapidly mixed micelle, thereby breakdown of emulsion becomes simple oil-in-water or water-in-oil emulsion; 2. chemical agent large usage quantity, causes expensive; 3. the application of a large amount of chemical agents makes it have certain toxic and side effect.
Summary of the invention
The object of this invention is to provide a kind of stratiform active particle and prepare the method for multiple-phase emulsion, adopt hydrophily stratiform active particle and a small amount of composite multiple-phase emulsion of preparing of oil soluble surfactant, the shortcoming or the deficiency that effectively overcome or avoid existing in above-mentioned prior art.
Stratiform active particle of the present invention is prepared the method for multiple-phase emulsion, comprise preparation table surface-active agent oil solution, prepare water-in-oil emulsion, preparation stratiform active particle aqueous dispersion and then prepare the multiple-phase emulsion of W/O/W, its step of preparation process is as follows:
(A) the surfactant oil solution that preparation quality concentration is 1.0%～4.0%;
(B) clear water is progressively added in surfactant oil solution under the mixing speed of 800-1200 revolutions per second, obtain water-in-oil emulsion;
(C) the stratiform active particle aqueous dispersion that preparation quality concentration is 0.5%～1.5%;
(D) by water-in-oil emulsion progressively to add in stratiform active particle aqueous dispersion under 3000-5000 revolutions per second of high-speed stirred, obtain the multiple-phase emulsion of W/O/W.
Wherein, the preparation of described surfactant oil solution is that 1.0-4.0 part surfactant is positioned in 100 parts of nonpolar paraffin oils, stirs 20-40s obtain with the speed of 3000-5000 revolutions per second.Surfactant in described surfactant oil solution is lipophile Span class surfactant.Described lipophile Span class surfactant is Span20, Span40, Span60 or Span80.In described water-in-oil emulsion, the volume ratio of clear water and surfactant oil solution is 3-7:7-3.The preparation of layered active particle aqueous dispersion is that the stratiform active particle of 0.5-1.5 part is positioned in clear water, to stir under the speed of 3000-5000 revolutions per second after 5-15 min, places and obtains for three days.Layered active particle is magnalium positive colloid laminate granular or montmorillonite layered particle or hectorite laminate granular.In the multiple-phase emulsion of described W/O/W, the volume ratio of water-in-oil emulsion and stratiform active particle aqueous dispersion is 2-5:8-5.
The present invention compared with prior art tool has the following advantages:
1, stabilization time long, in general half a year, there is not demulsifying phenomenon;
2, slow releasing function is obvious, and the time that is converted into simple O/W or O/W emulsion is 5～7 days
3, with hydrophilic active nano particle, replace hydrophilic surfactant active, reduce dosage of surfactant, reduce cost;
4, safety and environmental protection, has no side effect.
The specific embodiment
Stratiform active particle is prepared a method for multiple-phase emulsion, comprises preparation table surface-active agent oil solution, prepares water-in-oil emulsion, preparation stratiform active particle aqueous dispersion and then prepare the multiple-phase emulsion of W/O/W, and its step of preparation process is as follows:
(A) the surfactant oil solution that preparation quality concentration is 1.0%～4.0%;
(B) clear water is progressively added in surfactant oil solution under the mixing speed of 800-1200 revolutions per second, obtain water-in-oil emulsion;
(C) the stratiform active particle aqueous dispersion that preparation quality concentration is 0.5%～1.5%;
(D) by water-in-oil emulsion progressively to add stratiform active particle under 3000-5000 revolutions per second of high-speed stirred
In aqueous dispersion, obtain the multiple-phase emulsion of W/O/W.
The preparation of surfactant oil solution is that 1.0-4.0 part surfactant is positioned in 100 parts of nonpolar paraffin oils, stirs 20-40s obtain with the speed of 3000-5000 revolutions per second.Surfactant in surfactant oil solution is lipophile Span class surfactant.Lipophile Span class surfactant is Span20, Span40, Span60 or Span80.In water-in-oil emulsion, the volume ratio of clear water and surfactant oil solution is 3-7:7-3.The preparation of stratiform active particle aqueous dispersion is that the stratiform active particle of 0.5-1.5 part is positioned in clear water, to stir under the speed of 3000-5000 revolutions per second after 5-15 min, places and obtains for three days.Stratiform active particle is magnalium positive colloid laminate granular or montmorillonite layered particle or hectorite laminate granular.In the multiple-phase emulsion of W/O/W, the volume ratio of water-in-oil emulsion and stratiform active particle aqueous dispersion is 2-5:8-5.Provide specific embodiment below:
Embodiment 1
(A) the surfactant oil solution that preparation quality concentration is 1.0%;
(B) clear water is progressively added under the mixing speed of 800 revolutions per seconds in surfactant oil solution,
Obtain water-in-oil emulsion;
(C) the stratiform active particle aqueous dispersion that preparation quality concentration is 0.5%;
(D) by water-in-oil emulsion progressively to add stratiform active particle under 3000 revolutions per seconds of high-speed stirred
In aqueous dispersion, obtain the multiple-phase emulsion of W/O/W.
The preparation of surfactant oil solution is that 1.0 parts of surfactants are positioned in 100 parts of nonpolar paraffin oils, stirs 20-40s obtain with the speed of 3000 revolutions per seconds.Surfactant in surfactant oil solution is lipophile Span20.In water-in-oil emulsion, the volume ratio of clear water and surfactant oil solution is 3:7.The preparation of stratiform active particle aqueous dispersion is that the stratiform active particle of 0.5 part is positioned in clear water, to stir under the speed of 3000 revolutions per seconds after 5 min, places and obtains for three days.Stratiform active particle is magnalium positive colloid laminate granular.In the multiple-phase emulsion of W/O/W, the volume ratio of water-in-oil emulsion and stratiform active particle aqueous dispersion is 2:8.The multiple-phase emulsion performance of preparation: apparently present even milky, have certain viscosity, mobility is better, and particle diameter is 10 microns, places and does not occur layering demulsifying phenomenon half a year.The time that is converted into simple O/W emulsion is five days.
Embodiment 2
(A) the surfactant oil solution that preparation quality concentration is 3.0%;
(B) clear water is progressively added under the mixing speed of 1000 revolutions per seconds in surfactant oil solution,
Obtain water-in-oil emulsion;
(C) the stratiform active particle aqueous dispersion that preparation quality concentration is 0.75%;
(D) by water-in-oil emulsion progressively to add stratiform active particle under 4000 revolutions per seconds of high-speed stirred
In aqueous dispersion, obtain the multiple-phase emulsion of W/O/W.
The preparation of surfactant oil solution is that 3.0 parts of surfactants are positioned in 100 parts of nonpolar paraffin oils, stirs 30s obtain with the speed of 4000 revolutions per seconds.Surfactant in surfactant oil solution is lipophile Span40.In water-in-oil emulsion, the volume ratio of clear water and surfactant oil solution is 5:5.The preparation of stratiform active particle aqueous dispersion is that the stratiform active particle of 1.0 parts is positioned in clear water, to stir under the speed of 4000 revolutions per seconds after 10 min, places and obtains for three days.Stratiform active particle is the montmorillonite layered particle of magnalium.Water-in-oil emulsion and the aqueous dispersion of stratiform active particle in the multiple-phase emulsion of W/O/W
The volume ratio of system is 3:7.Prepared multiple-phase emulsion performance: apparently present even milky, have certain viscosity, mobility is better, and particle diameter is 16 microns, places and does not occur layering demulsifying phenomenon half a year, and the time that is converted into simple O/W emulsion is five days.
Embodiment 3
(A) the surfactant oil solution that preparation quality concentration is 4.0%;
(B) clear water is progressively added under the mixing speed of 1200 revolutions per seconds in surfactant oil solution,
Obtain water-in-oil emulsion;
(C) the stratiform active particle aqueous dispersion that preparation quality concentration is 1.5%;
(D) by water-in-oil emulsion progressively to add stratiform active particle under 5000 revolutions per seconds of high-speed stirred
In aqueous dispersion, obtain the multiple-phase emulsion of W/O/W.
The preparation of surfactant oil solution is that 4.0 parts of surfactants are positioned in 100 parts of nonpolar paraffin oils, stirs 40s obtain with the speed of 5000 revolutions per seconds.Surfactant in surfactant oil solution is lipophile Span80.In water-in-oil emulsion, the volume ratio of clear water and surfactant oil solution is 7:3.The preparation of stratiform active particle aqueous dispersion is that the stratiform active particle of 1.5 parts is positioned in clear water, to stir under the speed of 5000 revolutions per seconds after 15 min, places and obtains for three days.Stratiform active particle is hectorite laminate granular.In the multiple-phase emulsion of W/O/W, the volume ratio of water-in-oil emulsion and stratiform active particle aqueous dispersion is 5:5.Prepared emulsion performance: apparently present even milky, have certain viscosity, mobility is better, and particle diameter is 25 microns, places and does not occur layering demulsifying phenomenon for three months, and the time that is converted into simple O/W emulsion is seven days.
Claims (5)
1. a stratiform active particle is prepared the method for multiple-phase emulsion, comprise preparation table surface-active agent oil solution, prepare water-in-oil emulsion, preparation stratiform active particle aqueous dispersion and then prepare the multiple-phase emulsion of W/O/W, it is characterized in that described surfactant oil solution is that 1.0-4.0 part surfactant is positioned in 100 parts of nonpolar paraffin oils, with the speed of 3000-5000 revolutions per second, stir 20-40s and obtain; Layered active particle aqueous dispersion is that the stratiform active particle of 0.5-1.5 part is positioned in clear water, to stir under the speed of 3000-5000 revolutions per second after 5-15 min, places and makes for three days; Layered active particle is magnalium positive colloid laminate granular or montmorillonite layered particle or hectorite laminate granular; The step of preparation process of its multiple-phase emulsion is as follows:
(A) the surfactant oil solution that preparation quality concentration is 1.0%～4.0%;
(B) clear water is progressively added in surfactant oil solution under the mixing speed of 800-1200 revolutions per second, obtain water-in-oil emulsion;
(C) the stratiform active particle aqueous dispersion that preparation quality concentration is 0.5%～1.5%;
(D) by water-in-oil emulsion progressively to add in stratiform active particle aqueous dispersion under 3000-5000 revolutions per second of high-speed stirred, obtain the multiple-phase emulsion of W/O/W.
2. stratiform active particle according to claim 1 is prepared the method for multiple-phase emulsion, it is characterized in that the surfactant in described surfactant oil solution is lipophile Span class surfactant.
3. stratiform active particle according to claim 2 is prepared the method for multiple-phase emulsion, it is characterized in that described lipophile Span class surfactant is Span20, Span40, Span60 or Span80.
4. stratiform active particle according to claim 1 is prepared the method for multiple-phase emulsion, it is characterized in that in described water-in-oil emulsion, the volume ratio of clear water and surfactant oil solution is 3-7:7-3.
5. active method of preparing multiple-phase emulsion of stratiform according to claim 1, is characterized in that in the multiple-phase emulsion of described W/O/W, the volume ratio of water-in-oil emulsion and stratiform active particle aqueous dispersion is 2-5:8-5.
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Citations (4)
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| EP0892035A1 (en) * | 1997-07-17 | 1999-01-20 | Intevep SA | Multiple emulsion and method for preparing same |
| CN1973976A (en) * | 2006-11-16 | 2007-06-06 | 山东大学 | Microemulsion with high heat stability |
| WO2007112967A1 (en) * | 2006-03-31 | 2007-10-11 | Eni S.P.A. | Process for the preparation of water-in-oil and oil-in-water nanoemulsions |
| CN101108324A (en) * | 2007-08-13 | 2008-01-23 | 江南大学 | Emulsion of hyperstable latex capable of varying phase of circulation |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0892035A1 (en) * | 1997-07-17 | 1999-01-20 | Intevep SA | Multiple emulsion and method for preparing same |
| WO2007112967A1 (en) * | 2006-03-31 | 2007-10-11 | Eni S.P.A. | Process for the preparation of water-in-oil and oil-in-water nanoemulsions |
| CN1973976A (en) * | 2006-11-16 | 2007-06-06 | 山东大学 | Microemulsion with high heat stability |
| CN101108324A (en) * | 2007-08-13 | 2008-01-23 | 江南大学 | Emulsion of hyperstable latex capable of varying phase of circulation |
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