CN103721582B - A kind of original position forms the preparation method of the microemulsion of the nanoemulsions of high stability - Google Patents
A kind of original position forms the preparation method of the microemulsion of the nanoemulsions of high stability Download PDFInfo
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Abstract
The invention belongs to nanoemulsions preparing technical field.Relate to the preparation method that a kind of original position forms the microemulsion of the nanoemulsions of high stability, it is characterized in that: at least comprise: oil phase, nonionic surface active agent, inorganic salts, cationic surfactant, with 100 parts by weight, take following component respectively: oil phase 45-76 part, nonionic surface active agent 19-45 part, inorganic salts 0-2.5 part, cationic surfactant 0.1-2 part, surplus is water; Then the cationic surfactant taken is dissolved in water together with inorganic salts, obtains aqueous phase; Again the oil phase taken, non-ionic surface active agent are mixed with obtained aqueous phase, and add in beaker, obtain original position to form the microemulsion of the nanoemulsions of high stability.It provide that a kind of cost is low, place the preparation method that a kind of original position that the phenomenons such as layering not easily occur forms the microemulsion of the nanoemulsions of high stability in high and low temperature environment.
Description
Technical field
The invention belongs to nanoemulsions preparing technical field.Relate to the preparation method that a kind of original position forms the microemulsion of the nanoemulsions of high stability.
Background technology
Nanoemulsions is all widely used in fields such as oil exploitation, medicine, food, building energy conservation, concrete water-saving maintenance, agricultural, papermaking, wood-based plate, special cermacis, light industrys.
Inventor once applied for before this " a kind of multifunctional drilling fluid additive and preparation method thereof and application ", nanoemulsions in this patent has the effects such as good lubrication, but place a period of time in high and low temperature environment after, easily there is the phenomenons such as layering, lose original effect.
Summary of the invention
The invention provides that a kind of cost is low, place the preparation method that a kind of original position that the phenomenons such as layering not easily occur forms the microemulsion of the nanoemulsions of high stability in high and low temperature environment.
The object of the present invention is achieved like this, a kind of original position forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: at least comprise: oil phase, nonionic surface active agent, inorganic salts, cationic surfactant, with 100 parts by weight, take following component respectively: oil phase 45-76 part, nonionic surface active agent 19-45 part, inorganic salts 0-2.5 part, cationic surfactant 0.1-2 part, surplus is water; Then the cationic surfactant taken is dissolved in water together with inorganic salts, obtains aqueous phase; Again the oil phase taken, non-ionic surface active agent are mixed with obtained aqueous phase, and add in beaker, stir after 10-40 minute with the rotating speed of 150-500 rev/min at normal temperatures and leave standstill, obtain original position to form the microemulsion of the nanoemulsions of high stability.
Under 70 ° of C, utilize and above-mentioned microemulsion is diluted to water content for 70wt%, original position forms the nanoemulsions that aqueous phase content is 70 parts, and translucent blueing light, narrow diameter distribution, the polydispersion factor is less than 0.2, and domain size distribution is between 50nm-200nm.
Described speed of agitator is 200-300 rev/min.
Described oil phase is alkane, that is: the mixture of linear paraffin or n-alkane and isoparaffin; Described linear paraffin is decane, n-dodecane, n-tetradecane or hexadecane; Described n-alkane and the mixture of isoparaffin are atoleine or white oil.
Described non-ionic surface active agent is polyethenoxy ether class non-ionic surface active agent and the polyol ester class non-ionic surface active agent mixture by weight 44:56; Described polyethenoxy ether class non-ionic surface active agent is Span20, Span40, Span60 or Span65; Described polyol ester class non-ionic surface active agent Tween20, Tween40, Tween60, Tween65 or Tween80.
Described inorganic salts are the mixture of sodium salt, sylvite, magnesium salts, calcium salt, aluminium salt or these five kinds of any part by weight of inorganic salts.
Described cationic surfactant is alkyl trimethyl ammonium bromide or alkyl trimethyl ammonium chloride is one of DTAB, TTAB, CTAB, DTAC, TTAC; Described pair of alkyl chain cationic surfactant is one of DDAB, DODAC, DODAB.
Described oil phase is white oil 45 parts or atoleine 45 parts preferably, and preferred non-ionic surface active agent is the mixture of 26.4 parts of Span80 and 33.6 part Tween80, and cationic surfactant is CTAB2 part.
Described inorganic salts are NaCl, NaBr, KCl, KBr, Na
2s0
4, K
2s0
4, MgCl
2, MgBr
2, CaCl
2, MgS0
4, AlCl
3.
The microemulsion outward appearance that original position prepared by the present invention forms high-stability nano emulsion is transparent or semitransparent liquid, narrow diameter distribution, there is good long-time stability, high-temperature stability, low-temperature stability, can control strip electricity easily, meet environmental protection and every industrial requirements, be easy to transport, utilize this microemulsion original position can form good stability, the nanoemulsions that can place for a long time.
Accompanying drawing explanation
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Accompanying drawing 1 is the microemulsion of the CTAB adding variable concentrations in the present invention, the grain size distribution of the nanoemulsions obtained after original position dilution.
Accompanying drawing 2 adds different microemulsions prepared by different cationic surfactant in the present invention, the grain size distribution of the nanoemulsions obtained after original position dilution.
Detailed description of the invention
Embodiment 1
With 100 parts by weight, get 76 parts of white oils, 8.36 parts of Span80,10.64 parts of Tween80,0.1 part of CTAB, 5 parts of water, wherein Span80 and Tween80 totally 19 parts, both weight ratios are 11:14.Then put together and mix in the reactor, stir with the rotating speed of 500 revs/min under normal temperature and namely can be made into microemulsion in 10 minutes.
In example, nonionic surface active agent used is all purchased from Chemical Reagent Co., Ltd., Sinopharm Group (No. 52, Ningbo road, Shanghai City postcode 200002), and cationic surfactant all likes Sha (Tianjin) Chemical Co., Ltd. (No. 16, East, Yongan, Chaoyang District, Beijing City CBD International Building 1509 postcode 100022) purchased from Alpha.
The domain size distribution of the nanoemulsions that original position is formed after investigating the microemulsion high-temperature stability of the fabricated in situ nanoemulsions of preparation, long-time stability, low-temperature stability and dilution respectively by the following method:
1. stability measurement:
Long-time stability: the long-time static placement of product, observe outward appearance, note whether occurring layering clearly, if product places half a year, above outward appearance is unchanged, namely without obvious layering and sedimentation phenomenon.
Whether high-temperature stability: sample to be placed in 70 ° of C insulating boxs 5 hours, observes outward appearance, layering or sedimentation, if at product is placed on 70 DEG C after 4-5 hour, outward appearance is unchanged, namely without obvious layering and sedimentation phenomenon, illustrates that emulsion high-temperature stability is good.
Low-temperature stability: sample is placed on refrigerator freezing layer (about-17 ° of C), observes outward appearance, whether layering or sedimentation, if product is freezing 1-2 hour at being placed on-15 to-20 DEG C, outward appearance is unchanged, namely without obvious layering and sedimentation phenomenon, illustrates that emulsion low-temperature stability is good.
2. grain diameter measurement:
After microemulsion is diluted to aqueous phase content in the process constantly stirred is 70wt% water, during dilution, temperature maintains 70 ° of C.
Get proper amount of nano emulsion in measuring element, dilute general 500 times, be then placed in BI-200SM dynamic light scattering, measure the domain size distribution of emulsion, the domain size distribution of emulsion is narrower, and average grain diameter is less, then emulsion intercalation method is better.
Result is as shown in the table:
Embodiment 2
With 100 parts by weight, get atoleine 45 parts, 19.8 parts of Span80,25.2 parts of Tween80,2 parts of CTAB and 8 part water, wherein Span80 and Tween80 totally 45 parts, both weight ratios are 11:14(0.7857).2 parts of CTAB are dissolved in 8 parts of water, obtain aqueous phase; Again 45 parts of atoleines, 19.8 parts of Span80 and 25.2 part Tween80 are mixed in the reactor with obtained aqueous phase, under normal temperature, within 15 minutes, namely can be made into microemulsion with 300 revs/min of stirrings.
Detect by method described in embodiment 1, result is as follows:
Embodiment 3
With 100 parts by weight, get 76 parts of white oils, 8.36 parts of Span80,10.64 parts of Tween80,1 part of DODMAC, 4 parts of water, wherein Span80 and Tween80 totally 19 parts, both weight ratios are 11:14.Then put together and mix in the reactor, stir with the rotating speed of 150 revs/min under normal temperature and namely can be made into microemulsion in 40 minutes.
Detect by method described in embodiment 1, result is as follows:
Embodiment 4
With 100 parts by weight, get atoleine 45 parts, 19.8 parts of Span80,25.2 parts of Tween80,2.5 parts of NaCl, 2 parts of CTAB and 5.5 part water, wherein Span80 and Tween80 totally 45 parts, both weight ratios are 11:14(0.7857).2.5 parts of NaCl and 2 part CTAB are dissolved in 5.5 parts of water, obtain aqueous phase; Again 45 parts of atoleines, 19.8 parts of Span80 and 25.2 part Tween80 are mixed in the reactor with obtained aqueous phase, under normal temperature, within 20 minutes, namely can be made into microemulsion with 250 revs/min of stirrings.
Detect by method described in embodiment 1, result is as follows:
Embodiment 5
With 100 parts by weight, get atoleine 76 parts, 8.36 parts of Span80,10.64 parts of Tween80,1.5 parts of CaCl
2, 1 part of NaCl, 1 part of CTAB and 5.5 part water, wherein Span80 and Tween80 totally 45 parts, both weight ratios are 11:14(0.7857).By 1.5 parts of CaCl
2with 1 part of NaCl
2, 1 part of CTAB is dissolved in 5.5 parts of water, obtains aqueous phase; Again 45 parts of atoleines, 8.36 parts of Span80 and 10.64 part Tween80 are mixed in the reactor with obtained aqueous phase, under normal temperature, within 15 minutes, namely can be made into microemulsion with 300 revs/min of stirrings.
Detect by method described in embodiment 1, result is as follows:
Embodiment 6
With 100 parts by weight, get atoleine 60 parts, 13.2 parts of Span80,16.8 parts of Tween80,1 part of DTAB and 9 part water, wherein Span80 and Tween80 totally 30 parts, both weight ratios are 11:14(0.7857).1 part of CTAB is dissolved in 9 parts of water, obtains aqueous phase; Again 60 parts of atoleines, 13.2 parts of Span80 and 16.8 part Tween80 are mixed in the reactor with obtained aqueous phase, under normal temperature, within 25 minutes, namely can be made into microemulsion with 350 revs/min of stirrings.
Detect by method described in embodiment 1, result is as follows:
Inorganic salts of the present invention are the mixture of sodium salt, sylvite, magnesium salts, calcium salt, aluminium salt or these five kinds of any part by weight of inorganic salts.Described inorganic salts preferred NaCl, NaBr, KCl, KBr, Na
2s0
4, K
2s0
4, MgCl
2, MgBr
2, CaCl
2, MgS0
4, AlCl
3.Described cationic surfactant is DTAB, TTAB, CTAB, DTAC, TTAC, DDAB, DODAC, DODAB mono-.
The part that the present embodiment does not describe in detail and english abbreviation belong to the common practise of the industry, can search on the net, do not describe one by one here.
Claims (7)
1. an original position forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: at least comprise: oil phase, nonionic surface active agent, inorganic salts, cationic surfactant, with 100 parts by weight, take following component respectively: oil phase 45-76 part, nonionic surface active agent 19-45 part, inorganic salts 0-2.5 part, cationic surfactant 0.1-2 part, surplus is water; Then the cationic surfactant taken is dissolved in water together with inorganic salts, obtains aqueous phase; Again the oil phase taken, non-ionic surface active agent are mixed with obtained aqueous phase, and add in beaker, stir after 10-40 minute with the rotating speed of 150-500 rev/min at normal temperatures and leave standstill, obtain original position to form the microemulsion of the nanoemulsions of high stability;
Described cationic surfactant is alkyl trimethyl ammonium chloride is one of DTAC, TTAC;
Under 70 ° of C, utilize and above-mentioned microemulsion is diluted to water content for 70wt%, original position forms the nanoemulsions that aqueous phase content is 70 parts, and translucent blueing light, narrow diameter distribution, the polydispersion factor is less than 0.2, and domain size distribution is between 50nm-200nm.
2. a kind of original position according to claim 1 forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: described speed of agitator is 200-300 rev/min.
3. a kind of original position according to claim 1 forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: described oil phase is alkane, that is: the mixture of linear paraffin or n-alkane and isoparaffin; Described linear paraffin is decane, n-dodecane, n-tetradecane or hexadecane; Described n-alkane and the mixture of isoparaffin be atoleine or
White oil.
4. a kind of original position according to claim 1 forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: described non-ionic surface active agent is polyethenoxy ether class non-ionic surface active agent and the mixture of polyol ester class non-ionic surface active agent 44:56 by weight; Described polyethenoxy ether class non-ionic surface active agent is Span20, Span40, Span60 or Span65; Described polyol ester class non-ionic surface active agent Tween20, Tween40, Tween60, Tween65 or Tween80.
5. a kind of original position according to claim 1 forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: described inorganic salts are the mixture of sodium salt, sylvite, magnesium salts, calcium salt, aluminium salt or these five kinds of any part by weight of inorganic salts.
6. a kind of original position according to claim 1 forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: described oil phase is white oil 45 parts or atoleine 45 parts, non-ionic surface active agent is the mixture of 26.4 parts of Span80 and 33.6 part Tween80, and cationic surfactant is CTAB2 part.
7. a kind of original position according to claim 1 forms nanoemulsions and the microemulsion preparation method of high stability, it is characterized in that: described inorganic salts are NaCl, NaBr, KCl, KBr, Na
2s0
4, K
2s0
4, MgCl
2, MgBr
2, CaCl
2, MgS0
4, AlCl
3.
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| CN105038735A (en) * | 2015-06-03 | 2015-11-11 | 中国海洋石油总公司 | Environment-friendly microemulsion capable of being dispersed into nano liquid drops in situ and preparation method thereof |
| CN108114617B (en) * | 2017-12-13 | 2020-09-04 | 中国石油大学(北京) | Small-particle-size ultralow-concentration nano emulsion composition and preparation method thereof |
| CN109233788B (en) * | 2018-10-31 | 2021-09-10 | 重庆地质矿产研究院 | Nano-emulsion cleanup additive for unconventional gas reservoir fracturing and preparation method thereof |
| CN109467108B (en) * | 2019-01-06 | 2020-12-01 | 中盐金坛盐化有限责任公司 | Preparation method of nano-grade superfine sodium chloride |
| CN109773207B (en) * | 2019-02-01 | 2021-11-12 | 西南大学 | Method for preparing branched gold nanoparticles by adopting oil-in-water nano emulsion |
| CN111892117A (en) * | 2020-08-07 | 2020-11-06 | 吉林大学 | Microemulsion for solubilizing chlorinated hydrocarbon pollutants in underground environment and preparation method thereof |
| CN114832865B (en) * | 2022-06-15 | 2023-08-22 | 中国石油大学(华东) | Preparation method of molybdenum-based microemulsion catalyst applied to hydrocracking |
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| CN101721930A (en) * | 2009-12-15 | 2010-06-09 | 山东大学 | Low-energy preparation method of positive electricity nanometer emulsion |
| CN102698622A (en) * | 2012-06-20 | 2012-10-03 | 山东大学 | Micro-emulsion for forming nano-emulsion in situ and preparation method of micro-emulsion |
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|---|---|---|---|---|
| CN101721930A (en) * | 2009-12-15 | 2010-06-09 | 山东大学 | Low-energy preparation method of positive electricity nanometer emulsion |
| CN102698622A (en) * | 2012-06-20 | 2012-10-03 | 山东大学 | Micro-emulsion for forming nano-emulsion in situ and preparation method of micro-emulsion |
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