A kind of lysotropic liquid crystal and its production and use
Technical field
The present invention relates to a kind of lysotropic liquid crystal, be specifically related to a kind of lysotropic liquid crystal and its production and use.
Background technology
Liquid crystal has anisotropy and the mobility of liquid, the seriality of crystal, between solid and liquid in
Jie's phase.In certain temperature range, the physical property such as the heat of the existing crystal of liquid crystal, optical, electrical, magnetic, have again liquid mobility,
The engineering properties such as viscosity, deformation.According to the condition formed and composition, liquid crystal can be divided into two big class, i.e. thermotropic liquid crystal and molten causes
Liquid crystal.Thermotropic liquid crystal is caused by temperature, can only exist, usually one-component in certain temperature range.Lysotropic liquid crystal
The system being made up of with solvent the compound meeting certain structural requirement, containing two or more component.
Thermotropic liquid crystal application in cosmetics, replaces the dyestuff in cosmetics to reduce dye mainly by thermotropic liquid crystal
The stimulation that skin is caused by material, gives the color that cosmetics are gorgeous simultaneously, and relevant report starts from the day at the end of the eighties in last century
This patent (JP K01/246209, JP K01/242690).Lysotropic liquid crystal applied research in cosmetics is more, but relevant
Report the most little.Lysotropic liquid crystal is added, owing to the rheological property of lysotropic liquid crystal is main in the preparation process of cosmetic emulsion
Showing as the behavior of non-Newtonian fluid, have yield stress and the highest viscoelasticity, the liquid crystal structure around oil droplet is in rheological characteristic
On serve the effect hindering cohesion, and the Van der Waals force between oil droplet becomes the least, therefore has increase emulsion stability
Effect;Further, since liquid crystalline phase can swelling substantial amounts of water and in multiple structure, be effectively prevented moisture evaporation, therefore have
Strengthen moisture retention and salubrious skinfeel.
At present, lysotropic liquid crystal application in daily chemical products is more, but really little for the production of cream acids cosmetics,
And it is expensive.Development effectiveness is excellent, low-cost lysotropic liquid crystal cosmetics, has wide market.
Summary of the invention
The weak point that it is an object of the invention to overcome prior art to exist and provide a kind of lysotropic liquid crystal, the present invention
Additionally provide the preparation method of this lysotropic liquid crystal, invention further provides the purposes of this lysotropic liquid crystal, be applied to cream acids
In cosmetics, cosmetics can be made to have liquid crystal structure, and stability, moisture retention are good.At present, the research of this respect not yet appears in the newspapers
Road.
For achieving the above object, the technical scheme taked: a kind of lysotropic liquid crystal, described lysotropic liquid crystal is by following components group
Become: fatty alcohol-polyoxyethylene ether, hexadecanyl phosphate potassium salt, water.
Preferably, described water accounts for the 10.0~59.8% of described lysotropic liquid crystal gross mass, described fatty alcohol-polyoxyethylene ether
Accounting for the 10.0~61.9% of described lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for described lysotropic liquid crystal gross mass
0~80.0%.Present inventor sends out water presently described and described fatty alcohol-polyoxyethylene ether AEO9 is at described lysotropic liquid crystal
In content when being respectively lower than 10%, though lysotropic liquid crystal can be formed, but effect is not fine, is unsuitable for cosmetics
In.
Present invention also offers the preparation method of lysotropic liquid crystal described above, said method comprising the steps of:
(1a) water, fatty alcohol-polyoxyethylene ether, hexadecanyl phosphate potassium salt are preheated respectively;
(2a) water, fatty alcohol-polyoxyethylene ether, hexadecanyl phosphate potassium salt in step (1a) are mixed and heated stirring
Mixing, carries out constant temperature standing immediately after sealing, obtain described lysotropic liquid crystal after standing.
Preferably, in described step (1a), preheating temperature is 70 DEG C, and preheating time is 20~30min;Described step (2a)
Middle heating-up temperature is 70 DEG C~75 DEG C, and mixing speed is 0.5~1 revolutions per second, and mixing time is 10~15s, and dwell temperature is 5 DEG C
~25 DEG C, time of repose is 2d~3d.
Invention further provides lysotropic liquid crystal described above in preparation has the cosmetics of lysotropic liquid crystal phase
Purposes.
Invention further provides the preparation method of a kind of cosmetics with lysotropic liquid crystal phase, described method include with
Lower step:
(1b) aqueous phase and water soluble emulsifier are mixed, be placed in constant temperature heating, stir to being completely dissolved simultaneously;
(2b) oil phase and oil soluble emulsifying agent are mixed, be placed in constant temperature heating, stir to being completely melt simultaneously;
(3b) under heated at constant temperature, stirring condition, mixture prepared by step (1b) is joined prepared by step (2b)
In mixture, continue to stir to obtain emulsion;
(4b) under the conditions of heated at constant temperature, by emulsator, the emulsion in step (3b) is carried out emulsifying and obtain mastic;
(5b), when the mastic in step (4b) stands to room temperature, lysotropic liquid crystal as claimed in claim 1 or 2 is added
In described mastic, continue emulsifying obtain described in there are the cosmetics of lysotropic liquid crystal phase.
Preferably, lysotropic liquid crystal addition described in described step (5b) account for described in have the cosmetics of lysotropic liquid crystal phase total
The 10%~15% of quality.
Preferably, described aqueous phase is the mixture of G & W, account for described in there is the cosmetics gross mass of lysotropic liquid crystal phase
65.72%;Described oil phase is the mixture of stearic acid, isopropyl palmitate, white oil and monoglyceride, account for described in there is molten cause liquid
The 16.2% of the cosmetics gross mass of crystalline phase;Described oil soluble emulsifying agent is Span-80, account for described in there is the change of lysotropic liquid crystal phase
The 0.69% of cosmetic gross mass;Described water soluble emulsifier is Tween-80, account for described in have the cosmetics of lysotropic liquid crystal phase total
The 2.39% of quality.
Preferably, in described step (1b), heating-up temperature is 70~85 DEG C;In described step (2b), heating-up temperature is 85 DEG C;
In described step (3b), heating-up temperature is 85 DEG C;In described step (4b), emulsifying rate is 1000~3000r/min, emulsification times
It is 3~7min;In described step (5b), emulsification times is 2~3min.
The beneficial effects of the present invention is: the present invention is by controlling fatty alcohol-polyoxyethylene ether AEO9, cetyl phosphoric acid
Ester potassium salt and the ratio of water and preparation temperature, time of repose and stirring condition, prepare three component lysotropic liquid crystals.And should
Lysotropic liquid crystal is applied in cream acids cosmetics, prepares the cosmetics with lysotropic liquid crystal phase.The preparation method behaviour of the present invention
Making simple, mild condition, less energy consumption, the prepared cosmetics with lysotropic liquid crystal phase have the stability of excellence, moisture retention
And coating performance, there is good application prospect.
Accompanying drawing explanation
Fig. 1 a, 1b, 1c, 1d are respectively what fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and water were formed
Ternary lysotropic liquid crystal phasor;
Fig. 2 a, 2b, 2c are respectively the inclined of the lysotropic liquid crystal prepared under different time of repose when dwell temperature is 25 DEG C
Light texture maps;
Fig. 3 a, 3b, 3c are respectively the polarisation texture of the lysotropic liquid crystal prepared under difference stands when dwell temperature is 5 DEG C
Figure;
Fig. 4 is the XRD spectra of the lysotropic liquid crystal that embodiment 6 prepares;
Fig. 5 a, 5b, 5c are respectively the polarisation texture maps of the cosmetics prepared under different emulsifying rates and emulsification times.
Detailed description of the invention
For better illustrating the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.In example below, fatty alcohol-polyoxyethylene ether AEO-9 A represents, hexadecanyl phosphate potassium salt B table
Showing, deionized water C represents.
Embodiment 1
The explorative experiment of the preparation method of lysotropic liquid crystal of the present invention, comprises the following steps:
(1) will be equipped with the beaker of fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water respectively
It is placed in the water bath with thermostatic control of 70 DEG C preheating 20min.
(2) in mass ratio for A:B=5:5 weigh gross mass be 3g, 2.7g, 2.4g, 2.1g, 1.8g, 1.5g, 1.2g,
The raw material that 0.9g, 0.6g, 0.3g are warmed-up, joins in 10 clean beakers, then is separately added into deionized water to gross mass
For 3g.
(3) by step (2) is placed in the water-bath of 70 DEG C heating equipped with the beaker mixing raw material, slowly stir with glass rod simultaneously
Mix 15s, be placed in the water bath with thermostatic control of 25 DEG C standing 2d with diaphragm seal.
(4) mass ratio of A, B in step (1) is changed into respectively 0:10,1:9,2:8,3:7,4:6,6:4,7:3,8:2,
9:1,10:0, use step (2), the method for (3) to prepare mixing raw material respectively.
(5) dip mixing raw material on a small quantity with glass rod and, on microscope slide, after covered gently compacting, be placed in polarisation aobvious
Micro-Microscopic observation, draws the ternary phase diagrams of mixing raw material according to Formation of liquid crystals situation.Result is as shown in Figure 1a.
Embodiment 2
Experimental technique is with embodiment 1, and difference is: A, B in step (2), (4) change into A, C, and the C that will be eventually adding
Change B into.Its ternary phase diagrams is as shown in Figure 1 b.
Embodiment 3
Experimental technique is with embodiment 1, and difference is: A, B in step (2), (4) change into B, C, and the C that will be eventually adding
Change A into.Its ternary phase diagrams is as illustrated in figure 1 c.
Fig. 1 a, 1b, 1c collect formation Fig. 1 d.It can be seen that fatty alcohol-polyoxyethylene ether AEO-9, cetyl phosphoric acid
Ester potassium salt, water three component can form liquid crystal in the range of wider proportioning raw materials, and this relative broad range is: described fatty alcohol polyoxy
Vinyl Ether AEO9 accounts for the 5%~61.9% of described mixing raw material gross mass, and described hexadecanyl phosphate potassium salt accounts for described mixing
The 0~90% of raw material gross mass, described water accounts for the 2%-59.8% of described mixing raw material gross mass;Liquid crystal region area reaches
45%.
Embodiment 4
The impact that lysotropic liquid crystal is formed by time of repose
The beaker being respectively provided with fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and water is placed in 70 DEG C
Water-bath in after constant temperature about 25min, weigh 1.59g fatty alcohol-polyoxyethylene ether AEO-9,0.36g hexadecanyl phosphate respectively
Potassium salt, 1.05g water (A:B:C=0.53:0.12:0.35) joins in the beaker of another cleaning.Will be equipped with mixing the burning of raw material
Cup is placed in the water-bath of 75 DEG C heating, after being slowly stirred 10s with glass rod, is placed on the water bath with thermostatic control of 25 DEG C with diaphragm seal simultaneously
Middle standing.And 1d, 2d, the 3d after standing, with the formational situation of polarized light microscope observing lysotropic liquid crystal, under different time of repose
Polarisation texture maps as shown in Fig. 2 a, 2b, 2c.During it can be seen that mixing raw material stands 1d, its polarisation texture is the most unintelligible, table
Aligning of bright molecule not yet completes;Stand after 2d, the polarisation clean mark of formation, regular, show to mix in material system
Aligning of molecule completes, defines the liquid crystal of certain ad hoc structure;After standing 3d, the polarisation texture of formation is the most clear
Clear, regular, show to mix liquid crystal in material system and still exist.
Embodiment 5
The impact that lysotropic liquid crystal is formed by dwell temperature
Experimental technique is with embodiment 4, and difference is, the temperature of standing is changed into 5 DEG C (refrigerators), prepared mixing raw material
Polarisation texture maps is as shown in Fig. 3 a, 3b, 3c, and its result is similar to embodiment 4, and when mixing raw material stands 1d, its polarisation texture is also
Unintelligible, show that aligning of molecule not yet completes;Stand after 2d, the polarisation clean mark of formation, regular, show to mix former
Aligning of material system Middle molecule completes, defines the liquid crystal of certain ad hoc structure;After standing 3d, the polarisation texture of formation
The most clear, regular, show to mix liquid crystal in material system and still exist.
Embodiment 6
The XRD of lysotropic liquid crystal of the present invention characterizes
Forming by the raw material of A:B:C=0.33:0.30:0.37, the method for embodiment 4, preparation 3g lysotropic liquid crystal is (during standing
Between be 2d).
The XRD analysis of lysotropic liquid crystal of the present invention:
Prepared lysotropic liquid crystal is characterized by D/max 2004 type X-ray diffractometer.Condition determination: nickel is filtered
Sheet, copper anode, KαRadiation, instrumentation tubes pressure 50kV, work pipe flow 150mA, 0.01 °/s of scanning speed.Result is as shown in Figure 4.
Utilizing Bragg equation 2dsin θ=n λ (taking n=1) to calculate the interlamellar spacing of liquid crystal, result is as shown in table 1.
As known from Table 1, the d of prepared lysotropic liquid crystal1:d2:d3≈ 1:For hexagonal phase liquid crystal.
The d value of the lysotropic liquid crystal that table 1 embodiment 6 prepares
Embodiment 7
A kind of embodiment of the preparation method of lysotropic liquid crystal of the present invention, comprises the following steps:
(1) will be equipped with the beaker of fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water respectively
It is placed in the water bath with thermostatic control of 70 DEG C preheating 20min;
(2) accounting for the 10.0 of described lysotropic liquid crystal gross mass by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for described
The 10.0 of lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for the 80.0% of described lysotropic liquid crystal gross mass, weighs
Gross mass is the raw material that 3g is warmed-up, joins in the beaker of cleaning;
(3) by step (2) is placed in the water-bath of 70 DEG C heating equipped with the beaker mixing raw material, slowly stir with glass rod simultaneously
Mixing 15s, mixing speed is 0.5 revolutions per second, is placed in the water bath with thermostatic control of 25 DEG C standing 2d with diaphragm seal, obtains described molten cause liquid
Brilliant.
Prepared lysotropic liquid crystal is placed in polarized light microscopy Microscopic observation and has lysotropic liquid crystal phase.
Embodiment 8
A kind of embodiment of the preparation method of lysotropic liquid crystal of the present invention, comprises the following steps:
(1) will be equipped with the beaker of fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water respectively
It is placed in the water bath with thermostatic control of 70 DEG C preheating 30min;
(2) accounting for the 59.8% of described lysotropic liquid crystal gross mass by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for institute
Stating the 40.2% of lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for the 0% of described lysotropic liquid crystal gross mass, weighs
Gross mass is the raw material that 3g is warmed-up, joins in the beaker of cleaning;
(3) by step (2) is placed in the water-bath of 75 DEG C heating equipped with the beaker mixing raw material, slowly stir with glass rod simultaneously
Mixing 10s, mixing speed is 1 revolutions per second, is placed in the water bath with thermostatic control of 5 DEG C standing 3d with diaphragm seal, obtains described lysotropic liquid crystal.
Prepared lysotropic liquid crystal is placed in polarized light microscopy Microscopic observation and has lysotropic liquid crystal phase.
Embodiment 9
A kind of embodiment of the preparation method of lysotropic liquid crystal of the present invention, comprises the following steps:
(1) will be equipped with the beaker of fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water respectively
It is placed in the water bath with thermostatic control of 70 DEG C preheating 20min;
(2) accounting for the 10% of described lysotropic liquid crystal gross mass by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for described
The 61.9% of lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for the 28.1% of described lysotropic liquid crystal gross mass, claims
Taking gross mass is raw material warmed-up for 3g, joins in the beaker of cleaning;
(3) by step (2) is placed in the water-bath of 73 DEG C heating equipped with the beaker mixing raw material, slowly stir with glass rod simultaneously
Mixing 12s, mixing speed is 0.3 revolutions per second, is placed in the water bath with thermostatic control of 15 DEG C standing 2d with diaphragm seal, obtains described molten cause liquid
Brilliant.
Prepared lysotropic liquid crystal is placed in polarized light microscopy Microscopic observation and has lysotropic liquid crystal phase.
Embodiment 10
A kind of embodiment of the preparation method of lysotropic liquid crystal of the present invention, comprises the following steps:
(1) will be equipped with the beaker of fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water respectively
It is placed in the water bath with thermostatic control of 70 DEG C preheating 20min;
(2) accounting for the 36% of described lysotropic liquid crystal gross mass by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for described
The 53% of lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for the 11% of described lysotropic liquid crystal gross mass, weighs total
Quality is the raw material that 3g is warmed-up, joins in the beaker of cleaning;
(3) by step (2) is placed in the water-bath of 70 DEG C heating equipped with the beaker mixing raw material, slowly stir with glass rod simultaneously
Mixing 15s, mixing speed is 0.5 revolutions per second, is placed in the water bath with thermostatic control of 25 DEG C standing 2d with diaphragm seal, obtains described molten cause liquid
Brilliant.
Prepared lysotropic liquid crystal is placed in polarized light microscopy Microscopic observation and has lysotropic liquid crystal phase.
Embodiment 11
The lysotropic liquid crystal of the present invention application in preparation has the cosmetics of lysotropic liquid crystal phase
The formula of selection table 2 prepares cosmetics paste, and preparation process is as follows:
(1) press the raw material composition of A:B:C=0.53:0.11:0.36, the method for embodiment 4, prepare 3.75g institute of the present invention
State lysotropic liquid crystal (time of repose is 2d).
(2) weigh in the beaker that glycerol, Tween-80 addition fill deionized water, be placed in the water bath with thermostatic control of 70 DEG C and add
Heat, stirs to being completely dissolved simultaneously.
(3) weigh stearic acid, isopropyl palmitate, white oil, monoglyceride, Span-80 and add in beaker, being placed in 85 DEG C of perseverances
Tepidarium is heated, stirs to being completely melt simultaneously.
(4) under 85 DEG C of waters bath with thermostatic control, stirring conditions, prepared by mixture addition step (3) step (2) prepared mixed
In compound, continue to stir to obtain emulsion.
(5) under the conditions of 85 DEG C of waters bath with thermostatic control, after emulsion being carried out emulsifying 3min with 3000r/min rotating speed, by step
(1) lysotropic liquid crystal prepared in joins described in step (4) in emulsion system, continues emulsifying 2min and obtains cosmetics cream
Body.
(6) after standing 1d, with polarizing microscope, the polarisation texture maps of cosmetics paste in step (5) is observed, knot
As shown in Figure 5 a, in step (5), the cosmetics paste of preparation has lysotropic liquid crystal phase to fruit.
Table 2 mastic formula
Embodiment 12
The lysotropic liquid crystal of the present invention application in preparation has the cosmetics of lysotropic liquid crystal phase
Preparing cosmetics with the method for embodiment 11, difference is: emulsifying agent rotating speed changes 2000r/min, emulsifying 5 minutes into
After, add lysotropic liquid crystal of the present invention and continue emulsifying 2min.As shown in Figure 5 b, the cosmetics of preparation have its polarisation texture maps
There is lysotropic liquid crystal phase.
Embodiment 13
The lysotropic liquid crystal of the present invention application in preparation has the cosmetics of lysotropic liquid crystal phase
Preparing cosmetics with the method for embodiment 11, difference is: emulsifying agent rotating speed changes 1000r/min, emulsifying 7 minutes into
After, add lysotropic liquid crystal of the present invention and continue emulsifying 3min.As shown in Figure 5 c, the cosmetics of preparation have its polarisation texture maps
There is lysotropic liquid crystal phase.
Embodiment 14
The lysotropic liquid crystal of the present invention application in preparation has the cosmetics of lysotropic liquid crystal phase
Described method is with embodiment 11, and difference is: changed into by described lysotropic liquid crystal content in described cosmetics
10%, in described aqueous phase, water content in described cosmetics changes 63.72% into.The cosmetics of preparation have lysotropic liquid crystal phase.
Embodiment 15
The lysotropic liquid crystal of the present invention application in preparation has the cosmetics of lysotropic liquid crystal phase
Described method is with embodiment 11, and difference is: changed into by described lysotropic liquid crystal content in described cosmetics
12%, in described aqueous phase, water content in described cosmetics changes 61.72% into.The cosmetics of preparation have lysotropic liquid crystal phase.
Comparative example 1
Preparing cosmetics with the method for embodiment 11, difference is: prepare lysotropic liquid crystal of the present invention the most in advance, but
The hexadecanyl phosphate potassium salt used by lysotropic liquid crystal of the present invention will be prepared and water is incorporated to aqueous phase, fatty alcohol-polyoxyethylene ether
AEO-9 is incorporated to oil phase.Under polarizing microscope, being shown that details in a play not acted out on stage, but told through dialogues, the cosmetics prepared by explanation do not have lysotropic liquid crystal phase.
Embodiment 16
Prepare 2 cosmetics pastes by the method for embodiment 13 and comparative example 1, number by s1, s2, be placed in indoor environment
In, investigate its weight loss situation.Result is the brightest, and after placing 5 days, the weight-loss ratio of s1 is 7.8%, and the weight-loss ratio of s2 is
10.1%, show that the cosmetics with lysotropic liquid crystal phase have stronger water holding capacity.
Embodiment 17
Prepare cosmetics paste by the method for embodiment 13, seal and be placed in 40 DEG C of baking ovens standing 1d, recover to room temperature
After be still uniform and smooth white mastic, without layering, thinning, metachromatism.
Embodiment 18
Prepare cosmetics paste by the method for embodiment 13, seal and be placed in-10 DEG C of refrigerators standing 1d, recover to room temperature
After be still uniform and smooth white mastic, without layering, coarse, metachromatism.
Embodiment 19
Prepare cosmetics paste by the method for embodiment 13, be placed in a centrifuge and be centrifuged with the rotating speed of 2000r/min
30min, without oil-water separation phenomenon.
Last institute is it should be noted that, the present invention is only protected by above example in order to technical scheme to be described
Protecting the restriction of scope, although being explained in detail the present invention with reference to preferred embodiment, those of ordinary skill in the art should
Understand, technical scheme can be modified or equivalent, without deviating from the essence of technical solution of the present invention
And scope.