CN108159906A - A kind of W/O/W multiple emulsion and preparation method thereof - Google Patents
A kind of W/O/W multiple emulsion and preparation method thereof Download PDFInfo
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- CN108159906A CN108159906A CN201711470185.2A CN201711470185A CN108159906A CN 108159906 A CN108159906 A CN 108159906A CN 201711470185 A CN201711470185 A CN 201711470185A CN 108159906 A CN108159906 A CN 108159906A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
- B01F23/4105—Methods of emulsifying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
- B01F23/414—Emulsifying characterised by the internal structure of the emulsion
- B01F23/4141—High internal phase ratio [HIPR] emulsions, e.g. having high percentage of internal phase, e.g. higher than 60-90 % of water in oil [W/O]
Abstract
The present invention relates to a kind of W/O/W multiple emulsions and preparation method thereof, and the preparation method includes the following steps：Oil phase is prepared, deionized water is added dropwise, adds emulsifier conditioning agent, cooling stirring addition pH five steps of buffer solution.W/O/W multiple emulsion preparation method provided by the invention is simple, simplifies emulsification number, it is only necessary to primary emulsification.
Description
Technical field
The present invention relates to lotion preparing technical field more particularly to a kind of W/O/W multiple emulsion and its preparation sides
Method.
Background technology
Emulsion, mutual exclusive two-phase liquid mixing, wherein a phase liquid is scattered in drop state in another phase liquid
The heterogeneous liquid preparation of formation is emulsion.Emulsion can be divided into according to emulsifier, property, phase volume ratio：Oil-in-water
Three kinds of type (O/W) emulsion, water-in-oil type (W/O) emulsion and multiple emulsion (W/O/W or Water-In-Oil packet oil).
Common multiple emulsion preparation method is two step emulsion processes in the prior art.Using W/O/W multiple emulsion as
Example：First step Jiang Shui, oil, emulsifier form the level-one lotion of Water-In-Oil；Second step using level-one lotion as dispersed phase,
It is scattered in water phase by emulsification, prepares water-in-oil-in water multiple emulsion.
The multiple emulsion preparation method prepared in the prior art is relatively cumbersome, and cannot be carried out under high temperature and low-temperature condition
Spontaneous adjustment.
Invention content
The technical problems to be solved by the invention are：First, multiple emulsion preparation method of the prior art is relatively cumbersome,
Second is that emulsion of the prior art cannot carry out spontaneous adjustment under high temperature and low-temperature condition.
In order to solve the above technical problems, the present invention provides a kind of preparation method of W/O/W multiple emulsion, take
Technical solution is as follows：
On the one hand, the present invention provides a kind of preparation method of W/O/W multiple emulsion, the preparation method include with
Lower step:
A, low cloud point emulsifier, high cloud point emulsifier and assistant for emulsifying agent are added in into silicone oil, and heating and melting obtains oil
Phase；
B, deionized water is added dropwise into oil phase, obtains the first mixture, deionized water is added dropwise state and continues 1-2.5 h,
Under dropwise addition state, the temperature of first mixture is kept to be in the first temperature, and be stirred to first mixture；
C, emulsifier conditioning agent is added into the first mixture, the first mixture temperature is kept to be in the in adding procedure
One temperature, and operation is stirred to the first mixture, until emulsifier conditioning agent is completely dissolved, obtain the second mixture；
D, the temperature for reducing the second mixture is stirred to second temperature, and to second mixture；
E, the temperature of the second mixture is reduced to room temperature, pH buffer solutions is then added into the second mixture, and stir straight
It is completely dissolved to the pH buffer solutions, obtains W/O/W multiple emulsion.
Further, the second temperature is less than first temperature, and first temperature range is 80-92 DEG C, described
Second temperature is 40-70 DEG C.
Further, in stepb, the mixing speed ranging from 500-800r/min, in step C, the stirring
Including quickly stirring and mixing slowly, the quick mixing time is 10-40min, rotating speed 500-800r/min, it is described at a slow speed
Mixing time is 1-3.5h, mixing speed 200-250r/min, in step D, mixing speed ranging from 150-250r/min,
Mixing time ranging from 1-2h.
Further, the cloud point temperature of the low cloud point emulsifier is 50-80 DEG C, the cloud point temperature of the high cloud point emulsifier
Degree is more than 85 DEG C.
Further, the low cloud point emulsifier includes fatty alcohol and ethylene oxide condensate class Emulsifier O -10, fat
Alcohol and ethylene oxide condensate class Emulsifier O -15, fatty alcohol and ethylene oxide condensate class emulsifier AEO-7, alkyl phenol and ring
Oxidative ethane condensation species emulsifier TX-9, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-10, alkyl phenol and ethylene oxide
It is condensed species emulsifier TX-12, alkyl phenol and ethylene oxide synthesis species polyoxyethylene nonylphenol ether -9, alkyl phenol and ethylene oxide synthesis
Class emulsifier op-10, alkyl phenol polyoxyethylene ether class emulsifier SOPE-10, castor oil and ethylene oxide condensate class emulsifier
It is one or more in EL-40, polyoxyethylene fatty acid lipid emulsifiers LAE-24.
Further, the high cloud point emulsifier includes fatty alcohol and ethylene oxide condensate class Emulsifier O -20, fat
Alcohol and ethylene oxide condensate class emulsifier AEO-23, fatty alcohol and ethylene oxide condensate class emulsifier AEO-20, alkyl phenol
With ethylene oxide condensate class emulsifier TX-13, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-15, alkyl phenol and ring
Oxidative ethane condensation species emulsifier TX-18, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-21, alkyl phenol and epoxy second
Alkane synthesis species polyoxyethylene nonylphenol ether -13, alkyl phenol polyoxyethylene ether class emulsifier SOPE-15, the emulsification of alkyl phenol polyoxyethylene ether class
Agent SOPE-20, castor oil and ethylene oxide condensate class Emulsifier EL-80, castor oil and ethylene oxide condensate class emulsifier
It is one or more in EL-60.
Further, the assistant for emulsifying agent include hexadecanol, octadecyl alcolol, polyethylene glycol-8 000, polyethylene glycol-400,
One or more in propylene glycol, n-butanol and glycerine, the silicone oil includes methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, methyl
It is one or more in containing hydrogen silicone oil, methyl phenyl silicone oil, methylchlorophenyl silicone oil and MethylethoxylsiliconFluid Fluid.
Further, the emulsifier conditioning agent includes aliphatic acid and ethylene oxide condensate class emulsifier, alkyl phenol
Polyethenoxy ether class emulsifier, alkyl phenol polyoxyethylene ether class emulsifier, condensation compound of alkyl phenol and epoxy ethane class emulsifier
One or more, the pH buffer solutions include phosphate standard buffer solution, potassium dihydrogen phosphate/sodium hydroxide and di(2-ethylhexyl)phosphate
It is one or more in hydrogen sodium/sodium hydroxide.
Further, the emulsifier conditioning agent includes aliphatic acid and ethylene oxide condensate class emulsifier SG-6, fat
Fat acid and ethylene oxide condensate class emulsifier SG-9, alkyl phenol polyoxyethylene ether class emulsifier SOPE-4, alkyl phenol polyoxy second
Alkene ethers emulsifier SOPE-7, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-5, condensation compound of alkyl phenol and epoxy ethane
Class emulsifier TX-7's and condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-9 is one or more.
In addition, the present invention also provides a kind of W/O/W multiple emulsion, main formula is as follows：
The pH buffer solutions of 0.1%-0.4% weight,
The emulsifier conditioning agent of 0.5%-3% weight,
The low cloud point emulsifier of 1.5%-5% weight,
The high cloud point emulsifier of 3.5%-8% weight,
The assistant for emulsifying agent of 0.3%-2% weight,
The silicone oil of 8%-15% weight,
Surplus is deionized water.
Due to the implementation of above technical scheme, the present invention has the following advantages that compared with prior art：
W/O/W multiple emulsion provided by the invention and preparation method thereof utilizes the distinctive cloud point of nonionic emulsifier
Characteristic realizes the preparation of W/O/W multiple emulsion using a step emulsion process.At high operating temperatures, low cloud point emulsifier and water
Between hydrogen bond fracture, lose emulsifying effectiveness, at this point, high cloud point emulsifier effect under, formed water-in-oil emulsion；And relatively low
During temperature, low cloud point emulsifier restores emulsifying effectiveness, under the collective effect of emulsifier conditioning agent, to the Water-In-Oil formed
The oil phase of lotion and the distribution of water phase carry out spontaneous adjustment, ultimately form the lotion of W/O/W.Preparation method is simple,
Step emulsification is only needed to can be completed, in addition W/O/W multiple emulsion provided by the invention has under high temperature and low-temperature condition
Spontaneous adjustment function, can play preferable emulsification under low temperature and the condition of high temperature.
Specific embodiment
In order to which those skilled in the art is made to more fully understand the present invention program, below in conjunction with the embodiment of the present invention to this
The technical solution of invention is clearly and completely described, it is clear that described embodiment is only the implementation of a present invention part
Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness
All other embodiments obtained under the premise of labour should all belong to the scope of protection of the invention.
It should be noted that the term " first " of description and claims of this specification, " second " etc. are for area
Not similar object describes specific sequence or precedence without being used for.It should be appreciated that the data used in this way are appropriate
In the case of can be interchanged, so as to the embodiment of the present invention described herein can in addition to illustrate or describe herein those with
Outer sequence is implemented.In addition, term " comprising " and " having " and their any deformation, it is intended that cover non-exclusive packet
Contain, for example, containing the process of series of steps or unit, method, apparatus, product or equipment is not necessarily limited to what is clearly listed
Those steps or unit, but may include not listing clearly or intrinsic for these processes, method, product or equipment
Other steps or unit.
The present invention provides a kind of preparation method of W/O/W multiple emulsion, includes the following steps：
A, low cloud point emulsifier, high cloud point emulsifier and assistant for emulsifying agent are added in into silicone oil, and heating and melting obtains oil
Phase；
It is not limited in the step for holding the container of oil phase, can be flask or flask, mode of heating is not also done
It limits, can be heating water bath, it can also direct electro heating；
B, deionized water is added dropwise into oil phase, obtains the first mixture, deionized water is added dropwise state and continues 1-2.5 h,
Under dropwise addition state, the temperature of first mixture is kept to be in the first temperature, and be stirred to first mixture；
In the steps, mode or method that deionized water is added dropwise are not limited, can be added dropwise using constant speed pump,
It can be carried out using buret；Under dropwise addition state, the heat preserving mode of the first mixture is not limited, specifically refers to step
The mode of heating of A.The mixing plant of mixture is not limited, magnetic agitation well-known to those skilled in the art, machinery stir
It mixes；
C, emulsifier conditioning agent is added into the first mixture, the first mixture temperature is kept to be in the in adding procedure
One temperature, and operation is stirred to the first mixture, until emulsifier conditioning agent is completely dissolved, obtain the second mixture；
In the step, the addition manner for emulsifying conditioning agent is not limited, can be added dropwise, can also disposably add in；It stirs
Mixing equipment is not specifically limited with step C；It is completely dissolved, is that emulsification conditioning agent uniformly disperses in the first mixture, formation
Second mixture is uniform, will not generate layering or other apparent non-uniform phenomenons.
D, the temperature for reducing the second mixture is stirred to second temperature, and to second mixture；
Mixing plant in the step is not specifically limited with step C.
E, the temperature of the second mixture is reduced to room temperature, pH buffer solutions is then added into the second mixture, and stir straight
It is completely dissolved to the pH buffer solutions, obtains W/O/W multiple emulsion.
It in the step, is completely dissolved, with the definition in step C, i.e. pH buffer solutions are uniformly dispersed in the second mixture, no
Apparent layering or other apparent non-uniform phenomenons can be generated.
In the present embodiment, the cloud point temperature of the low cloud point emulsifier is 50-80 DEG C, the cloud point of the high cloud point emulsifier
Temperature >=85 DEG C.
Substance mentioned in the present invention is the prior art, can be bought in the market before the applying date, therefore no longer right
Its specific ingredient or preparation method are described in detail.
In the present embodiment, the low cloud point emulsifier includes fatty alcohol and ethylene oxide condensate class Emulsifier O -10, fat
Fat alcohol and ethylene oxide condensate class Emulsifier O -15, fatty alcohol and ethylene oxide condensate class emulsifier AEO-7, alkyl phenol with
Ethylene oxide condensate class emulsifier TX-9, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-10, alkyl phenol and epoxy second
Alkane condensation species emulsifier TX-12, alkyl phenol and ethylene oxide synthesis species polyoxyethylene nonylphenol ether -9, alkyl phenol and ethylene oxide integrate
Species emulsifier op-10, alkyl phenol polyoxyethylene ether class emulsifier SOPE-10, castor oil and ethylene oxide condensate class emulsify
It is one or more in agent EL-40, polyoxyethylene fatty acid lipid emulsifiers LAE-24.It is described a kind of or more in the embodiment
Kind, refer to can be provided substance classes one or two or three kinds and more than substance combine.
Embodiment 1
Electronic scale weighs 15g fatty alcohols and ethylene oxide condensate class emulsifier AEO-7,30g fatty alcohol and epoxy second
Alkane condensation species Emulsifier O -20,6g hexadecanols, 72g methyl-silicone oils are placed in 1000ml three-necked flasks, by three-necked flask water-bath
60 DEG C are heated to, silicone oil and emulsifier is made to melt and be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 85 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 500r/min
Under the conditions of, deionized water 471g, time for adding 2h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2h under 500r/min speed conditions at 85 DEG C；
Then to 6g condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-7 are added in oil phase, in turning for 500r/min
Then the lower stirring 25min of speed turns down rotating speed to 200r/min, continues to stir 1h.
Then oil phase temperature is reduced to 45 DEG C, is turned magnetic stirring apparatus rotating speed down to 200r/min, is persistently stirred 2h；
Continue to reduce oil phase temperature to room temperature, 1.5g phosphate standard buffer solutions are added in into oil phase, stop stirring, i.e.,
Obtain W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 2
Electronic scale weighs 18g castor oil and ethylene oxide condensate class Emulsifier EL-40,36g castor oil and epoxy second
Alkane condensation species Emulsifier EL-60,4.8g PEG 8000s, 60g phenyl silicone oils are placed in 1000ml three-necked flasks, by three
Mouth flask water-bath is heated to 60 DEG C, silicone oil and emulsifier is made to melt and be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 87 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 500r/min
Under the conditions of, deionized water 472.2g, time for adding 2.5h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 1h under 500r/min speed conditions at 85 DEG C；
Then to addition 9g alkyl phenol polyoxyethylene ether class emulsifier SOPE-4 in oil phase, under the rotating speed of 500r/min
30min is stirred, rotating speed is then turned down to 225r/min, continues to stir 2h.
Then oil phase temperature is reduced to 60 DEG C, is turned magnetic stirring apparatus rotating speed down to 200r/min, is persistently stirred 1.5h；
Continue to reduce oil phase temperature to room temperature, it is molten that 1.8g sodium dihydrogen phosphates/sodium hydroxide standard buffers are added in into oil phase
Liquid stops stirring to get to W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 3
Electronic scale weighs 7.5g alkyl phenols and ethylene oxide synthesis species emulsifier op-10,6g alkyl phenols and epoxy second
Alkane is condensed species emulsifier TX-12,30g fatty alcohol and ethylene oxide condensate class emulsifier AEO-20,4.5g n-butanol, 60g
Methyl phenyl silicone oil is placed in 1000ml three-necked flasks, by three-necked flask heating water bath to 60 DEG C, melts silicone oil and emulsifier
And be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 87 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 600r/min
Under the conditions of, deionized water 468g, time for adding 2h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2.5h under 500r/min speed conditions at 87 DEG C；
Then to addition 9g alkyl phenol polyoxyethylene ether class emulsifier SOPE-4 in oil phase, under the rotating speed of 500r/min
20min is stirred, rotating speed is then turned down to 250r/min, continues to stir 3.5h.
Then oil phase temperature is reduced to 55 DEG C, is turned magnetic stirring apparatus rotating speed down to 150r/min, is persistently stirred 1.5h；
Continue to reduce oil phase temperature to room temperature, 1.8g phosphate standard buffer solutions are added in into oil phase, stop stirring, i.e.,
Obtain W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 4
Electronic scale weighs 21g alkyl phenol polyoxyethylene ether class emulsifier SOPE-10,39g alkyl phenols and ethylene oxide contracts
Conjunction species emulsifier TX-13,12g n-butanol, 60g Methyl Hydrogen Polysiloxane Fluids are placed in 1000ml three-necked flasks, by three-necked flask water
Bath is heated to 70 DEG C, silicone oil and emulsifier is made to melt and be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 80 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 600r/min
Under the conditions of, deionized water 468g, time for adding 3h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2.5h under 600r/min speed conditions at 87 DEG C；
Then to 18g condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-5 are added in oil phase, in turning for 600r/min
Then the lower stirring 30min of speed turns down rotating speed to 200r/min, continues to stir 1h.
Then oil phase temperature is reduced to 50 DEG C, is turned magnetic stirring apparatus rotating speed down to 150r/min, is persistently stirred 2h；
Continue to reduce oil phase temperature to room temperature, 1.8g phosphate standard buffer solutions are added in into oil phase, stop stirring, i.e.,
Obtain W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 5
Electronic scale weighs 6g alkyl phenols and ethylene oxide synthesis species emulsifier op-10,6g alkyl phenols and ethylene oxide
It is condensed species emulsifier TX-12,12.5g fatty alcohol and ethylene oxide condensate class Emulsifier O -20,23.5g fatty alcohols and ring
Oxidative ethane condensation species emulsifier AEO-20,6g propylene glycol, 90g ethyl silicon oils are placed in 1000ml three-necked flasks, by three mouthfuls of burnings
Bottle heating water bath makes silicone oil and emulsifier melt and be uniformly mixed, as oil phase to 65 DEG C；
By uniformly mixed oil phase heating water bath to 87 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 600r/min
Under the conditions of, deionized water 443.4g, time for adding 1.5h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2.5h under 600r/min speed conditions at 87 DEG C；
Then to 12g aliphatic acid and ethylene oxide condensate class emulsifier SG-6 is added in oil phase, in turning for 600r/min
Then the lower stirring 40min of speed turns down rotating speed to 200r/min, continues to stir 1h.
Then oil phase temperature is reduced to 70 DEG C, is turned magnetic stirring apparatus rotating speed down to 200r/min, is persistently stirred 1h；
Continue to reduce oil phase temperature to room temperature, 0.6g sodium dihydrogen phosphates/sodium hydroxide buffer solution is added in into oil phase, is stopped
It only stirs to get to W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 6
Electronic scale weighs 9g fatty alcohols and ethylene oxide condensate class Emulsifier O -10,21g alkyl phenol polyoxyethylene ether
Class emulsifier SOPE-15,6g hexadecanol, 24g methyl-silicone oils, 24g full refinings silicone oil 54 are placed in 1000ml three-necked flasks, will
Three-necked flask heating water bath makes silicone oil and emulsifier melt and be uniformly mixed, as oil phase to 60 DEG C；
By uniformly mixed oil phase heating water bath to 80 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 800r/min
Under the conditions of, deionized water 511.2g, time for adding 1h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2.5h under 800r/min speed conditions at 80 DEG C；
Then to 3g aliphatic acid and ethylene oxide condensate class emulsifier SG-9 is added in oil phase, in turning for 800r/min
Then the lower stirring 30min of speed turns down rotating speed to 250r/min, continues to stir 1h.
Then oil phase temperature is reduced to 45 DEG C, is turned magnetic stirring apparatus rotating speed down to 150r/min, is persistently stirred 1h；
Continue to reduce oil phase temperature to room temperature, 1.8g phosphate standard buffer solutions are added in into oil phase, stop stirring, i.e.,
Obtain W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 7
Electronic scale weighs 12g fatty alcohols and ethylene oxide condensate class emulsifier AEO-7,30g castor oil and epoxy second
Alkane condensation species Emulsifier EL-80,12g propylene glycol, 60g MethylethoxylsiliconFluid Fluids are placed in 1000ml three-necked flasks, Jiang Sankou
Flask water-bath is heated to 50 DEG C, silicone oil and emulsifier is made to melt and be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 88 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 500r/min
Under the conditions of, deionized water 474.5g, time for adding 2h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2h under 500r/min speed conditions at 88 DEG C；
Then to 12g aliphatic acid and ethylene oxide condensate class emulsifier SG-9 is added in oil phase, in turning for 500r/min
Then the lower stirring 30min of speed turns down rotating speed to 200r/min, continues to stir 3h.
Then oil phase temperature is reduced to 40 DEG C, is turned magnetic stirring apparatus rotating speed down to 150r/min, is persistently stirred 2h；
Continue to reduce oil phase temperature to room temperature, 1.5g phosphate standard buffer solutions are added in into oil phase, stop stirring, i.e.,
Obtain W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 8
Electronic scale weighs 18g polyoxyethylene fatty acids lipid emulsifiers LAE-24,25g alkyl phenol and ethylene oxide condensation
Species emulsifier TX-18,5g polyethylene glycol 400,80g ethyl silicon oils are placed in 1000ml three-necked flasks, by three-necked flask water-bath
65 DEG C are heated to, silicone oil and emulsifier is made to melt and be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 90 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 500r/min
Under the conditions of, deionized water 456.2g, time for adding 2h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2h under 500r/min speed conditions at 90 DEG C；
Then to addition 5g alkyl phenol polyoxyethylene ether class emulsifier SOPE-7 in oil phase, under the rotating speed of 500r/min
30min is stirred, rotating speed is then turned down to 220r/min, continues to stir 2h.
Then oil phase temperature is reduced to 60 DEG C, is turned magnetic stirring apparatus rotating speed down to 150r/min, is persistently stirred 1h；
Continue to reduce oil phase temperature to room temperature, 1.8g phosphate standard buffer solutions are added in into oil phase, stop stirring, i.e.,
Obtain W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 9
Electronic scale weighs 20g fatty alcohols and ethylene oxide condensate class Emulsifier O -10,23g fatty alcohols and ethylene oxide
Condensation species Emulsifier O -10,5g polyethylene glycol 400s, 80g ethyl silicon oils are placed in 1000ml three-necked flasks, by three-necked flask
Heating water bath makes silicone oil and emulsifier melt and be uniformly mixed, as oil phase to 60 DEG C；
By uniformly mixed oil phase heating water bath to 80 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 500r/min
Under the conditions of, deionized water 456g, time for adding 2h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 1.5h under 500r/min speed conditions at 80 DEG C；
Then to addition 5g alkyl phenol polyoxyethylene ether class emulsifier SOPE-7 in oil phase, under the rotating speed of 500r/min
30min is stirred, rotating speed is then turned down to 225r/min, continues to stir 3h.
Then oil phase temperature is reduced to 60 DEG C, is turned magnetic stirring apparatus rotating speed down to 150r/min, is persistently stirred 1h；
Continue to reduce oil phase temperature to room temperature, 1.8g phosphate standard buffer solutions are added in into oil phase, stop stirring, i.e.,
Obtain W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 10
Electronic scale weighs 13g alkyl phenols and ethylene oxide synthesis species polyoxyethylene nonylphenol ether -9,30g alkyl phenol polyoxyethylene ether
Class emulsifier SOPE-20,5g PEG 8000,70g ethyl silicon oils are placed in 1000ml three-necked flasks, by three-necked flask water-bath
60 DEG C are heated to, silicone oil and emulsifier is made to melt and be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 85 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 600r/min
Under the conditions of, deionized water 461g, time for adding 2h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 1.5h under 500r/min speed conditions at 80 DEG C；
Then to 10g aliphatic acid and ethylene oxide condensate class emulsifier SG-6 is added in oil phase, in turning for 500r/min
Then the lower stirring 30min of speed turns down rotating speed to 200r/min, continues to stir 3.5h.
Then oil phase temperature is reduced to 50 DEG C, is turned magnetic stirring apparatus rotating speed down to 150r/min, is persistently stirred 1.5h；
Continue to reduce oil phase temperature to room temperature, 2g phosphate standard buffer solutions added in into oil phase, stop stirring to get
To W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 11
Electronic scale weighs 3g fatty alcohols and ethylene oxide condensate class emulsifier AEO-7,5g alkyl phenol and ethylene oxide
Comprehensive species emulsifier op-10,15g fatty alcohols and ethylene oxide condensate class emulsifier AEO-20,15g fatty alcohol and epoxy
Oxide condensate class emulsifier AEO-23,5g propylene glycol, 70g methyl-silicone oils are placed in 1000ml three-necked flasks, by three-necked flask
Heating water bath makes silicone oil and emulsifier melt and be uniformly mixed, as oil phase to 58 DEG C；
By uniformly mixed oil phase heating water bath to 85 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 600r/min
Under the conditions of, deionized water 470g, time for adding 1.5h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 1h under 600r/min speed conditions at 85 DEG C；
Then to addition 10g alkyl phenol polyoxyethylene ether class emulsifier SOPE-7 in oil phase, under the rotating speed of 500r/min
40min is stirred, rotating speed is then turned down to 200r/min, continues to stir 1h.
Then oil phase temperature is reduced to 45 DEG C, is turned magnetic stirring apparatus rotating speed down to 200r/min, is persistently stirred 1h；
Continue to reduce oil phase temperature to room temperature, 2g sodium dihydrogen phosphates/sodium hydroxide buffer solution is added in into oil phase, is stopped
Stirring is to get to W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
Embodiment 12
Electronic scale weighs 20g condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-9,30g alkyl phenols and ethylene oxide
Condensation species emulsifier TX-21,10g hexadecanol, 90g phenyl silicone oils are placed in 1000ml three-necked flasks, by three-necked flask water-bath
58 DEG C are heated to, silicone oil and emulsifier is made to melt and be uniformly mixed, as oil phase；
By uniformly mixed oil phase heating water bath to 92 DEG C, oil phase is then kept in the magnetic agitation that rotating speed is 800r/min
Under the conditions of, deionized water 430g, time for adding 2h are added dropwise into oil phase.
After being added dropwise, oil phase temperature is kept persistently to stir 2.5h under 800r/min speed conditions at 92 DEG C；
Then to 18g condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-9 are added in oil phase, in turning for 800r/min
Then the lower stirring 40min of speed turns down rotating speed to 250r/min, continues to stir 2h.
Then oil phase temperature is reduced to 45 DEG C, is turned magnetic stirring apparatus rotating speed down to 200r/min, is persistently stirred 2h；
Continue to reduce oil phase temperature to room temperature, 2g phosphate standard buffer solutions added in into oil phase, stop stirring to get
To W/O/W multiple emulsion.
The W/O/W multiple emulsion can be dissolved in the water in 2min.
The present invention is described in detail above, its object is to allow the personage for being familiar with this field technology that can understand this
The content of invention is simultaneously implemented, and it is not intended to limit the scope of the present invention, all Spirit Essence institutes according to the present invention
The equivalent change or modification of work should all cover within the scope of the present invention.
Claims (10)
1. a kind of preparation method of W/O/W multiple emulsion, which is characterized in that the preparation method includes the following steps:
A, low cloud point emulsifier, high cloud point emulsifier and assistant for emulsifying agent are added in into silicone oil, and heating and melting obtains oil phase；
B, deionized water is added dropwise into oil phase, obtains the first mixture, deionized water is added dropwise state and continues 1-2.5h, and shape is being added dropwise
Under state, the temperature of first mixture is kept to be in the first temperature, and be stirred to first mixture；
C, emulsifier conditioning agent is added into the first mixture, the first mixture temperature is kept to be in the first temperature in adding procedure
Degree, and operation is stirred to the first mixture, until emulsifier conditioning agent is completely dissolved, obtain the second mixture；
D, the temperature for reducing the second mixture is stirred to second temperature, and to second mixture；
E, the temperature of the second mixture is reduced to room temperature, pH buffer solutions is then added into the second mixture, and stir until institute
It states pH buffer solutions to be completely dissolved, obtains W/O/W multiple emulsion.
2. preparation method as described in claim 1, which is characterized in that the second temperature is less than first temperature, and described the
One temperature range is 80-92 DEG C, and the second temperature is 40-70 DEG C.
3. preparation method as described in claim 1, which is characterized in that in stepb, the mixing speed ranging from 500-
800r/min, in step C, the stirring includes quickly stirring and mixing slowly, and the quick mixing time is 10-40min,
Rotating speed is 500-800r/min, described to mix slowly the time as 1-3.5h, mixing speed 200-250r/min, in step D,
Mixing speed ranging from 150-250r/min, mixing time ranging from 1-2h.
4. preparation method as described in claim 1, which is characterized in that the cloud point temperature of the low cloud point emulsifier is 50-80
DEG C, the cloud point temperature of the high cloud point emulsifier is more than 85 DEG C.
5. preparation method as described in claim 1, which is characterized in that the low cloud point emulsifier includes fatty alcohol and epoxy second
Alkane condensation species Emulsifier O -10, fatty alcohol and ethylene oxide condensate class Emulsifier O -15, fatty alcohol and ethylene oxide condensation
Species emulsifier AEO-7, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-9, condensation compound of alkyl phenol and epoxy ethane class breast
Agent TX-10, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-12, alkyl phenol and ethylene oxide synthesis species emulsifier
OP-9, alkyl phenol and ethylene oxide synthesis species emulsifier op-10, alkyl phenol polyoxyethylene ether class emulsifier SOPE-10, castor-oil plant
Oil and ethylene oxide condensate class Emulsifier EL-40, it is one or more in polyoxyethylene fatty acid lipid emulsifiers LAE-24.
6. preparation method as described in claim 1, which is characterized in that the high cloud point emulsifier includes fatty alcohol and epoxy second
Alkane condensation species Emulsifier O -20, fatty alcohol and ethylene oxide condensate class emulsifier AEO-23, fatty alcohol and ethylene oxide contract
Close species emulsifier AEO-20, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-13, condensation compound of alkyl phenol and epoxy ethane
Class emulsifier TX-15, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-18, condensation compound of alkyl phenol and epoxy ethane class breast
Agent TX-21, alkyl phenol and ethylene oxide synthesis species polyoxyethylene nonylphenol ether -13, alkyl phenol polyoxyethylene ether class emulsifier SOPE-
15th, alkyl phenol polyoxyethylene ether class emulsifier SOPE-20, castor oil and ethylene oxide condensate class Emulsifier EL-80, castor oil
With it is one or more in ethylene oxide condensate class Emulsifier EL-60.
7. preparation method as described in claim 1, which is characterized in that the assistant for emulsifying agent includes hexadecanol, octadecyl alcolol, gathers
It is one or more in ethylene glycol -8000, polyethylene glycol-400, propylene glycol, n-butanol and glycerine；The silicone oil includes methyl silicon
Oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methylchlorophenyl silicone oil and MethylethoxylsiliconFluid Fluid
In it is one or more.
8. preparation method as described in claim 1, which is characterized in that the emulsifier conditioning agent includes aliphatic acid and epoxy
Oxide condensate class emulsifier, alkyl phenol polyoxyethylene ether class emulsifier, alkyl phenol polyoxyethylene ether class emulsifier, alkyl phenol with
Ethylene oxide condensate class emulsifier it is one or more, the pH buffer solutions include phosphate standard buffer solution, phosphorus
It is one or more in acid dihydride potassium/sodium hydroxide and sodium dihydrogen phosphate/sodium hydroxide.
9. preparation method as described in claim 1, which is characterized in that the emulsifier conditioning agent includes aliphatic acid and epoxy
Oxide condensate class emulsifier SG-6, aliphatic acid and ethylene oxide condensate class emulsifier SG-9, alkyl phenol polyoxyethylene ether class
Emulsifier SOPE-4, alkyl phenol polyoxyethylene ether class emulsifier SOPE-7, condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-
5th, the one of condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-7 and condensation compound of alkyl phenol and epoxy ethane class emulsifier TX-9
Kind is a variety of.
10. a kind of multiple emulsion prepared such as preparation method according to any one of claims 1-8, which is characterized in that described multiple
The ingredient for closing emulsion is as follows：
The pH buffer solutions of 0.1%-0.4% weight,
The emulsifier conditioning agent of 0.5%-3% weight,
The low cloud point emulsifier of 1.5%-5% weight,
The high cloud point emulsifier of 3.5%-8% weight,
The assistant for emulsifying agent of 0.3%-2% weight,
The silicone oil of 8%-15% weight,
Surplus is deionized water.
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| CN109517190A (en) * | 2018-11-23 | 2019-03-26 | 中国石油集团渤海钻探工程有限公司 | Compound emulsifying agent and preparation method thereof for low viscosity dimethyl silicone oil in emulsifying |
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