CN103506021A - Small-particle-size water-in-oil nano emulsion and preparation method thereof - Google Patents
Small-particle-size water-in-oil nano emulsion and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a small-particle-size water-in-oil nano emulsion and a preparation method thereof. The small-particle-size water-in-oil nano emulsion is characterized by comprising the following components in percentage by weight: 30-55% of alkane as an oil phase, 30-45% of emulsifier and the balance of water, wherein the emulsifier is a nonionic surfactant-cosurfactant mixture. The preparation method comprises the following steps: uniformly mixing the alkane and emulsifier at 5-40 DEG C with a magnetic stirrer at the stirring speed of 100-500 rpm, and dropwisely adding the water into the system while keeping stirring at the speed of 100-500 rpm for 5-60 minutes, thereby obtaining the transparent-appearance water-in-oil nano emulsion of which the liquid drop average diameter is less than 20nm. The method is simple to operate; and the prepared nano emulsion has the characteristics of small particle size, narrow distribution and the like.
Description
Technical field
The present invention relates to a kind of small particle diameter Water-In-Oil nanoemulsions and preparation method thereof.
Background technology
Nanoemulsions may be defined as a kind of emulsion type, wherein disperse the average droplet size of discontinuous phase be less than 1000nm, continuous phase and disperse the component of discontinuous phase must be enough not miscible, make to form phase separately, these emulsions comprise nonpolar phase (being commonly referred to oil phase), polarity phase (conventionally moisture and be referred to as water-based phase or water), surfactant and cosurfactant, according to preparation method, may there is narrow droplets size distribution.
Conventionally exist two kinds of methods of preparing nanoemulsions.The modal method of the first is under high pressure to use high pressure homogenisers to be prepared, the preparation of thick emulsion before this, conventionally according to processing compound, oil, water, surfactant and other stabilizer elements are mixed, utilize agitator to obtain the conventional emulsions that certain particle size distributes, then the homogeneous processing that utilizes Ultra high-pressure microfluidization machine or ultrasonic wave and high pressure homogenizer coupling to carry out under specified conditions thick emulsion obtains nanoemulsions, this method is only suitable for small lot preparation, and apparatus expensive; Second method is phase transition method, under the condition of constant composition, regulates temperature to target emulsification system, then cooling fast, can make nanoemulsions, and the deficiency of this method maximum is exactly that heating and cooling in preparation process make the energy consumption of the method higher.
Nanoemulsions and ordinary emulsion have similarity, but also there is basic difference: the formation of (1) ordinary emulsion generally needs the external world that energy is provided, as needing the processing such as stirring, supersonic oscillations to form, nanoemulsions forms automatically, without the external world, provides energy; (2) ordinary emulsion is thermodynamic unstable system, deposit in process and can occur coalescent and be finally separated into oil, water, and nanoemulsions is thermodynamic stable system, can not occur coalescent, even if there is temporary transient layering under ultracentrifugation effect, once cancellation centrifugal force field, lamination disappears immediately, automatically restores to again original stabilising system.
Nanoemulsions compare with ordinary emulsion size droplet diameter little, be uniformly dispersed, have certain dynamic stability, its pooled applications is at some value segments, as fields such as medicine, food, cosmetics.Along with the further of research gos deep into, nanoemulsions, in oil exploitation, particularly, for the exploitation aspect of the tiny low-permeability oil deposit in duct, stratum, has represented huge application potential in recent years.At present, the poly-silicon powder of solid nano is having successful application aspect the step-down water filling of oil field, but the tiny feature in low permeability reservoirs duct requires nano polysilicon diameter of particle used little and even, because the particle of large particle diameter easily stops up low permeability reservoirs duct, cause difficult water injection.At present also there is no nanoemulsions for the report of oil-field flooding aspect, but little, the finely dispersed characteristic of the particle diameter that nanoemulsions has makes it aspect water filling, have unique advantage, particle diameter little and that be evenly distributed can avoid the phenomenon of stopping up low permeability reservoirs duct to occur on the one hand, the nano-meter characteristic of nanoemulsions can also reduce system flow resistance in duct, stratum on the other hand, prevent the hydration swelling of clay, be conducive to normally carrying out of oil-field flooding.
Summary of the invention
The invention provides a kind of small particle diameter Water-In-Oil nanoemulsions and preparation method thereof.
The technical solution used in the present invention is: a kind of small particle diameter Water-In-Oil nanoemulsions is provided, this nanoemulsions comprises following several component, weight fraction is that the alkane of 30%-55% is as oil phase, weight fraction is the emulsifying agent of 30%-45%, emulsifying agent is the mixture of non-ionic surface active agent and cosurfactant, and remainder is water.
Described preparation method is: at 5-40 ℃, first oil phase and emulsifying agent are passed through to magnetic stirring apparatus, mixing speed with 100-500rpm stirs, in system, drip water again, keep the mixing speed of 100-500rpm to stir 5-60min simultaneously, can obtain appearance transparent, drop diameter is less than the Water-In-Oil nanoemulsions of 20nm.
Described alkane is mixture or the linear paraffin of n-alkane and isoparaffin; described emulsifying agent is to mix by the non-ionic surfactant polyoxyethylene ether fatty alcohol as first type surface activating agent with as the low-carbon alcohols of cosurfactant, and wherein the weight ratio of APEO fatty alcohol and low-carbon alcohols is 12:1 to 1:1;
Described linear paraffin is hexane, heptane, octane, decane, n-dodecane, n-tetradecane hexadecane, and described n-alkane and isoparaffin mixture are atoleine or white oil.
The structure of the described non-ionic surfactant polyoxyethylene ether fatty alcohol as first type surface activating agent is R-(O-C-C)
x-OH, wherein R is that carbon number is the straight chained alkyl of 12-15, x is 2-11; The described low-carbon alcohols as cosurfactant is ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, 1-amylalcohol, 2-amylalcohol, 3-amylalcohol, 2-methyl-1-butene alcohol, 2-methyl-2-butanols, 3-methyl-2-butanols, 3-methyl-1-butanol, 2,2-dimethyl-1-propyl alcohol, 1-hexanol, 2-hexanol, 3-hexanol, 4-methyl-2-amylalcohol, n-heptanol, n-octyl alcohol and composition thereof.
Water-In-Oil nanoemulsions prepared by the present invention, its preparation method is simple, and made nanoemulsions has the features such as particle diameter is little, narrow diameter distribution.
The specific embodiment
Embodiment 1
Take 4.00g APEO fatty alcohol MOA-3 and 3.00g n-butanol in beaker, add again 10.00g white oil, hierarchy of control temperature remains on 25 ℃, on magnetic stirring apparatus, with 200rpm, stir 15 min and obtain settled solution, now drip 2.0g water, keep magnetic stirrer speed 200rpm, after water droplet adds completely, mixing speed at 200rpm continues to stir 40min, can obtain the nanoemulsions of outward appearance clear.The size droplet diameter that adopts the ZetaPlus mensuration nanoemulsions of U.S. Brooker Hai Wen instrument company, prepared nanoemulsions average grain diameter and particle diameter distribute as shown in table 1.
Table 1 APEO fatty alcohol/n-butanol/white oil/water nanoemulsions system particle diameter distributes
Embodiment 2
Take 11.0g APEO fatty alcohol MOA-3 and 1.0g n-butanol in beaker, add again 11.0g n-hexane, hierarchy of control temperature remains on 10 ℃, on magnetic stirring apparatus, with 200rpm, stir 15 min and obtain settled solution, now drip 7.0g water, keep magnetic stirrer speed 450rpm, after water droplet adds completely, mixing speed at 450rpm continues to stir 60min, can obtain the nanoemulsions of outward appearance clear.The size droplet diameter that adopts the ZetaPlus mensuration nanoemulsions of U.S. Brooker Hai Wen instrument company, prepared nanoemulsions average grain diameter and particle diameter distribute as shown in table 2.
Table 2 APEO fatty alcohol/butanol/hexane/water nanoemulsions system particle diameter distributes
Embodiment 3
Take 8.5g APEO fatty alcohol MOA-3 and 2.0g 4-methyl-2-amylalcohol in beaker, add again 8.0g n-hexane, hierarchy of control temperature remains on 10 ℃, on magnetic stirring apparatus, with 200rpm, stir 15 min and obtain settled solution, now drip 4.5g water, keep magnetic stirrer speed 450rpm, after water droplet adds completely, mixing speed at 450rpm continues to stir 60min, can obtain the nanoemulsions of outward appearance clear.The size droplet diameter that adopts the ZetaPlus mensuration nanoemulsions of U.S. Brooker Hai Wen instrument company, prepared nanoemulsions average grain diameter and particle diameter distribute as shown in table 3.
Table 3 APEO fatty alcohol/4-methyl-2-amylalcohol/n-hexane/water nanoemulsions system
Particle diameter distributes
Embodiment 4
Take 9.5g APEO fatty alcohol MOA-3 and 1.0g 2,2-dimethyl-1-propyl alcohol is in beaker, add again 6.5g white oil, hierarchy of control temperature remains on 10 ℃, stirs 15 min obtain settled solution on magnetic stirring apparatus with 200rpm, now drips 2.0g water, keep magnetic stirrer speed 450rpm, after water droplet adds completely, in the mixing speed continuation of 450rpm, stir 60min, can obtain the nanoemulsions of outward appearance clear.The size droplet diameter that adopts the ZetaPlus mensuration nanoemulsions of U.S. Brooker Hai Wen instrument company, prepared nanoemulsions average grain diameter and particle diameter distribute as shown in table 4.
Table 4 APEO fatty alcohol/2,2-dimethyl-1-propyl alcohol/white oil/water nanoemulsions
System particle diameter distributes
According to the result of above-mentioned specific embodiment, the prepared nanoemulsions of the present invention has the advantages such as particle diameter is little, narrowly distributing.
Embodiment 5
According to " SY/T5971-94 water filling clay stabilizer method of evaluating performance ", the anti-swollen rate of several nanoemulsions of preparation is measured.
The anti-swollen rate of several nanoemulsions of table 5
| 1. | 2. Example 1 sample | 3. Example 2 samples | 4. Example 3 samples | 5. Example 4 samples |
| 6. Anti-swollen rate, % | 7. 95.61% | 8. 86.37% | 9. 83.49% | 10. 91.64% |
From the above results, can find out, the prepared nanoemulsions of the present invention has good anti-swollen performance.
Claims (6)
1. a small particle diameter Water-In-Oil nanoemulsions, is characterized in that: this nanoemulsions contains following component by weight percentage:
Alkane 30%-55%
Emulsifying agent 30%-45%
Water 10%-25%.
2. Water-In-Oil nanoemulsions as claimed in claim 1, is characterized in that: described alkane is mixture or the linear paraffin of n-alkane and isoparaffin.
3. Water-In-Oil nanoemulsions as claimed in claim 2, is characterized in that: described linear paraffin is hexane, heptane, octane, decane, n-dodecane, n-tetradecane or hexadecane, and described n-alkane and isoparaffin mixture are atoleine or white oil.
4. Water-In-Oil nanoemulsions as claimed in claim 1, it is characterized in that: described emulsifying agent is to mix by the non-ionic surfactant polyoxyethylene ether fatty alcohol as first type surface activating agent with as the low-carbon alcohols of cosurfactant, and wherein the weight ratio of APEO fatty alcohol and low-carbon alcohols is 12:1 to 1:1.
5. Water-In-Oil nanoemulsions as claimed in claim 1, is characterized in that: the structure of the described non-ionic surfactant polyoxyethylene ether fatty alcohol as first type surface activating agent is R-(O-C-C)
x-OH, wherein R is that carbon number is the straight chained alkyl of 12-15, x is 2-11; The described low-carbon alcohols as cosurfactant is ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, 1-amylalcohol, 2-amylalcohol, 3-amylalcohol, 2-methyl-1-butene alcohol, 2-methyl-2-butanols, 3-methyl-2-butanols, 3-methyl-1-butanol, 2,2-dimethyl-1-propyl alcohol, 1-hexanol, 2-hexanol, 3-hexanol, 4-methyl-2-amylalcohol, n-heptanol, n-octyl alcohol or its mixture.
6. the preparation method of a small particle diameter Water-In-Oil nanoemulsions, it is characterized in that at 5-40 ℃, pass through magnetic stirring apparatus, mixing speed at 100-500rpm mixes alkane and emulsifying agent, in system, drip water again, keep mixing speed is the 5-60min that stirs under the speed of 100-500rpm simultaneously, can obtain appearance transparent, and water droplet average diameter is less than the Water-In-Oil nanoemulsions of 20nm.
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Cited By (6)
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| CN104845605A (en) * | 2014-02-18 | 2015-08-19 | 中国石油化工股份有限公司 | Nanometer emulsion flooding increase agent for oilfield flooding, and preparation method thereof |
| CN105623767A (en) * | 2016-01-11 | 2016-06-01 | 天津大学 | Gas hydrate preparation method using phase-change heat transfer of oil wrapped water emulsion |
| CN106281274A (en) * | 2015-06-08 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of oil-field flooding Gemini surface active agent nanoemulsions injection agent and preparation method |
| CN106566506A (en) * | 2016-11-02 | 2017-04-19 | 成都劳恩普斯科技有限公司 | Nanopore throat cleaning agent, and preparation method and application thereof |
| CN109773207A (en) * | 2019-02-01 | 2019-05-21 | 山东青年政治学院 | Using the method for nano oil-in-water emulsion preparation branch-like gold nano grain |
| CN115991983A (en) * | 2021-10-20 | 2023-04-21 | 中国石油化工股份有限公司 | Nanoemulsion and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845605A (en) * | 2014-02-18 | 2015-08-19 | 中国石油化工股份有限公司 | Nanometer emulsion flooding increase agent for oilfield flooding, and preparation method thereof |
| CN106281274A (en) * | 2015-06-08 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of oil-field flooding Gemini surface active agent nanoemulsions injection agent and preparation method |
| CN106281274B (en) * | 2015-06-08 | 2019-03-29 | 中国石油化工股份有限公司 | A kind of oil-field flooding Gemini surface active agent nanoemulsions injection agent and preparation method |
| CN105623767A (en) * | 2016-01-11 | 2016-06-01 | 天津大学 | Gas hydrate preparation method using phase-change heat transfer of oil wrapped water emulsion |
| CN105623767B (en) * | 2016-01-11 | 2018-05-25 | 天津大学 | The gas hydrate preparation method of water-in-oil emulsion phase-change heat-exchange |
| CN106566506A (en) * | 2016-11-02 | 2017-04-19 | 成都劳恩普斯科技有限公司 | Nanopore throat cleaning agent, and preparation method and application thereof |
| CN109773207A (en) * | 2019-02-01 | 2019-05-21 | 山东青年政治学院 | Using the method for nano oil-in-water emulsion preparation branch-like gold nano grain |
| CN115991983A (en) * | 2021-10-20 | 2023-04-21 | 中国石油化工股份有限公司 | Nanoemulsion and preparation method and application thereof |
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Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: China Petroleum & Chemical Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: China Petroleum & Chemical Corp. Patentee before: Nanhua Group Research Institute |
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