Summary of the invention
The object of the invention is to overcome weak point that prior art exists and provide a kind of lysotropic liquid crystal, present invention also offers the preparation method of this lysotropic liquid crystal, invention further provides the purposes of this lysotropic liquid crystal, be applied in cream acids cosmetics, cosmetics can be made to have liquid crystal structure, and stability, moisture retention are good.At present, there is not been reported in the research of this respect.
For achieving the above object, the technical scheme taked: a kind of lysotropic liquid crystal, described lysotropic liquid crystal is composed of the following components: fatty alcohol-polyoxyethylene ether, hexadecanyl phosphate potassium salt, water.
Preferably, described water accounts for 10.0 ~ 59.8% of described lysotropic liquid crystal gross mass, and described fatty alcohol-polyoxyethylene ether accounts for 10.0 ~ 61.9% of described lysotropic liquid crystal gross mass, and described hexadecanyl phosphate potassium salt accounts for 0 ~ 80.0% of described lysotropic liquid crystal gross mass.Present inventor find at described water and described fatty alcohol-polyoxyethylene ether AEO9 the content in described lysotropic liquid crystal respectively lower than 10% time, though can form lysotropic liquid crystal, effect is not fine, is not suitable for being applied in cosmetics.
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 carried out preheating respectively;
(2a) water, fatty alcohol-polyoxyethylene ether, hexadecanyl phosphate potassium salt in step (1a) are mixed and heated and stirred mixing, carry out constant temperature after sealing immediately and leave standstill, after leaving standstill, obtain described lysotropic liquid crystal.
Preferably, in described step (1a), preheat temperature is 70 DEG C, and preheating time is 20 ~ 30min; In described step (2a), 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, and time of repose is 2d ~ 3d.
Invention further provides lysotropic liquid crystal described above and prepare the purposes had in the cosmetics of lysotropic liquid crystal phase.
Invention further provides a kind of preparation method with the cosmetics of lysotropic liquid crystal phase, said method comprising the steps of:
(1b) by aqueous phase and water soluble emulsifier mixing, be placed in constant temperature and heat, be stirred to simultaneously and dissolve completely;
(2b) by oil phase and oil soluble emulsifying agent mixing, be placed in constant temperature and heat, be stirred to simultaneously and melt completely;
(3b) under heated at constant temperature, stirring condition, mixture prepared by step (1b) is joined in mixture prepared by step (2b), continue to stir to obtain emulsion;
(4b) under heated at constant temperature condition, by emulsator, emulsifying is carried out to the emulsion in step (3b) and obtain mastic;
(5b) when the mastic in step (4b) leaves standstill to room temperature, lysotropic liquid crystal as claimed in claim 1 or 2 is joined in described mastic, there are described in continuation emulsifying obtains the cosmetics of lysotropic liquid crystal phase.
Preferably, lysotropic liquid crystal addition described in described step (5b) account for described in there is 10% ~ 15% of the cosmetics gross mass of lysotropic liquid crystal phase.
Preferably, described aqueous phase is the mixture of G & W, has 65.72% of the cosmetics gross mass of lysotropic liquid crystal phase described in accounting for; Described oil phase is the mixture of stearic acid, isopropyl palmitate, white oil and monoglyceride, has 16.2% of the cosmetics gross mass of lysotropic liquid crystal phase described in accounting for; Described oil soluble emulsifying agent is Span-80, has 0.69% of the cosmetics gross mass of lysotropic liquid crystal phase described in accounting for; Described water soluble emulsifier is Tween-80, has 2.39% of the cosmetics gross mass of lysotropic liquid crystal phase described in accounting for.
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, and emulsification times is 3 ~ 7min; In described step (5b), emulsification times is 2 ~ 3min.
Beneficial effect of the present invention is: the present invention, by controlling ratio and preparation temperature, time of repose and the stirring condition of fatty alcohol-polyoxyethylene ether AEO9, hexadecanyl phosphate potassium salt and water, prepares three components lysotropic liquid crystal.And this lysotropic liquid crystal is applied in cream acids cosmetics, prepares the cosmetics with lysotropic liquid crystal phase.Preparation method of the present invention is simple to operate, mild condition, less energy consumption, and the prepared cosmetics with lysotropic liquid crystal phase have excellent stability, moisture retention and coating performance, have good application prospect.
Detailed description of the invention
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with specific embodiment, the invention will be further described.In embodiment, fatty alcohol-polyoxyethylene ether AEO-9 A represents below, and hexadecanyl phosphate potassium salt B represents, 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) beaker that fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water are housed is placed in respectively the water bath with thermostatic control preheating 20min of 70 DEG C.
(2) in mass ratio for A:B=5:5 takes the raw material that gross mass is 3g, 2.7g, 2.4g, 2.1g, 1.8g, 1.5g, 1.2g, 0.9g, 0.6g, 0.3g preheating, join in 10 clean beakers, then to add deionized water to gross mass be respectively 3g.
(3) water-bath beaker that mixed material is housed in step (2) being placed in 70 DEG C is heated, and slowly stirs 15s with glass rod simultaneously, is placed in the water bath with thermostatic control of 25 DEG C leaves standstill 2d with diaphragm seal.
(4) by the A in step (1), the mass ratio of B changes 0:10,1:9,2:8,3:7,4:6,6:4,7:3,8:2,9:1,10:0 into respectively, and the method for employing step (2), (3) prepares mixed material respectively.
(5) dip a small amount of mixed material on microscope slide with glass rod, covered also, gently after compacting, is placed in polarized light microscopy Microscopic observation, draws the ternary phase diagrams of mixed material according to Formation of liquid crystals situation.Result as shown in Figure 1a.
Embodiment 2
Experimental technique is with embodiment 1, and difference is: change A, B in step (2), (4) into A, C, and change the C finally added into B.Its ternary phase diagrams as shown in Figure 1 b.
Embodiment 3
Experimental technique is with embodiment 1, and difference is: change A, B in step (2), (4) into B, C, and change the C finally added into A.Its ternary phase diagrams as illustrated in figure 1 c.
Fig. 1 a, 1b, 1c gather formation Fig. 1 d.Can find out, fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt, water three components can form liquid crystal within the scope of wider proportioning raw materials, this relative broad range is: described fatty alcohol-polyoxyethylene ether AEO9 accounts for 5% ~ 61.9% of described mixed material gross mass, described hexadecanyl phosphate potassium salt accounts for 0 ~ 90% of described mixed material gross mass, and described water accounts for the 2%-59.8% of described mixed material gross mass; Liquid crystal region area reaches 45%.
Embodiment 4
The impact that time of repose is formed lysotropic liquid crystal
After the water-bath constant temperature beaker that fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and water are housed respectively being placed in 70 DEG C is about 25min, take 1.59g fatty alcohol-polyoxyethylene ether AEO-9 respectively, 0.36g hexadecanyl phosphate potassium salt, 1.05g water (A:B:C=0.53:0.12:0.35) joins in the beaker of another cleaning.The water-bath that the beaker that mixed material is housed is placed in 75 DEG C is heated, after slowly stirring 10s with glass rod simultaneously, is placed on diaphragm seal in the water bath with thermostatic control of 25 DEG C and leaves standstill.And the 1d after leaving standstill, 2d, 3d, with the formational situation of polarized light microscope observing lysotropic liquid crystal, the polarisation texture maps under different time of repose is as shown in Fig. 2 a, 2b, 2c.Can find out, when mixed material leaves standstill 1d, its polarisation texture is also unintelligible, shows that aligning of molecule not yet completes; Leave standstill after 2d, the polarisation clean mark of formation, regular, show that aligning of mixed material system Middle molecule completes, define the liquid crystal of certain ad hoc structure; After leaving standstill 3d, the polarisation texture of formation is still clear, regular, shows that in mixed material system, liquid crystal still exists.
Embodiment 5
The impact that dwell temperature is formed lysotropic liquid crystal
Experimental technique is with embodiment 4, difference is, standing temperature is changed into 5 DEG C (refrigerators), the polarisation texture maps of prepared mixed material is as shown in Fig. 3 a, 3b, 3c, its result is similar with embodiment 4, when mixed material leaves standstill 1d, its polarisation texture is also unintelligible, shows that aligning of molecule not yet completes; Leave standstill after 2d, the polarisation clean mark of formation, regular, show that aligning of mixed material system Middle molecule completes, define the liquid crystal of certain ad hoc structure; After leaving standstill 3d, the polarisation texture of formation is still clear, regular, shows that in mixed material system, liquid crystal still exists.
Embodiment 6
The XRD of lysotropic liquid crystal of the present invention characterizes
Form by the raw material of A:B:C=0.33:0.30:0.37, the method for embodiment 4, preparation 3g lysotropic liquid crystal (time of repose is 2d).
The XRD analysis of lysotropic liquid crystal of the present invention:
D/max-2004 type X-ray diffractometer characterizes prepared lysotropic liquid crystal.Condition determination: nickel filter disc, copper anode, K
αradiation, instrumentation tubes pressure 50kV, work pipe flow 150mA, scanning speed 0.01 °/s.Result as shown in Figure 4.
Utilize Bragg equation 2dsin θ=n λ (getting n=1) interlamellar spacing to liquid crystal to calculate, result is as shown in table 1.
As known from Table 1, the d of prepared lysotropic liquid crystal
1: d
2: d
3≈ 1:
be six side's phase liquid crystal.
The d value of the lysotropic liquid crystal that table 1 embodiment 6 is obtained
Embodiment 7
A kind of embodiment of the preparation method of lysotropic liquid crystal of the present invention, comprises the following steps:
(1) beaker that fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water are housed is placed in respectively the water bath with thermostatic control preheating 20min of 70 DEG C;
(2) 10.0 of described lysotropic liquid crystal gross mass is accounted for by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for 10.0 of described lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for 80.0% of described lysotropic liquid crystal gross mass, take the raw material that gross mass is 3g preheating, join in clean beaker;
(3) water-bath beaker that mixed material is housed in step (2) being placed in 70 DEG C is heated, slowly stir 15s with glass rod simultaneously, mixing speed is 0.5 revolutions per second, is placed in the water bath with thermostatic control of 25 DEG C and leaves standstill 2d, obtain described lysotropic liquid crystal with diaphragm seal.
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) beaker that fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water are housed is placed in respectively the water bath with thermostatic control preheating 30min of 70 DEG C;
(2) 59.8% of described lysotropic liquid crystal gross mass is accounted for by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for 40.2% of described lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for 0% of described lysotropic liquid crystal gross mass, take the raw material that gross mass is 3g preheating, join in clean beaker;
(3) water-bath beaker that mixed material is housed in step (2) being placed in 75 DEG C is heated, slowly stir 10s with glass rod simultaneously, mixing speed is 1 revolutions per second, is placed in the water bath with thermostatic control of 5 DEG C and leaves standstill 3d, obtain described lysotropic liquid crystal with diaphragm seal.
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) beaker that fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water are housed is placed in respectively the water bath with thermostatic control preheating 20min of 70 DEG C;
(2) 10% of described lysotropic liquid crystal gross mass is accounted for by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for 61.9% of described lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for 28.1% of described lysotropic liquid crystal gross mass, take the raw material that gross mass is 3g preheating, join in clean beaker;
(3) water-bath beaker that mixed material is housed in step (2) being placed in 73 DEG C is heated, slowly stir 12s with glass rod simultaneously, mixing speed is 0.3 revolutions per second, is placed in the water bath with thermostatic control of 15 DEG C and leaves standstill 2d, obtain described lysotropic liquid crystal with diaphragm seal.
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) beaker that fatty alcohol-polyoxyethylene ether AEO-9, hexadecanyl phosphate potassium salt and deionized water are housed is placed in respectively the water bath with thermostatic control preheating 20min of 70 DEG C;
(2) 36% of described lysotropic liquid crystal gross mass is accounted for by described water, described fatty alcohol-polyoxyethylene ether AEO-9 accounts for 53% of described lysotropic liquid crystal gross mass, described hexadecanyl phosphate potassium salt accounts for 11% of described lysotropic liquid crystal gross mass, take the raw material that gross mass is 3g preheating, join in clean beaker;
(3) water-bath beaker that mixed material is housed in step (2) being placed in 70 DEG C is heated, slowly stir 15s with glass rod simultaneously, mixing speed is 0.5 revolutions per second, is placed in the water bath with thermostatic control of 25 DEG C and leaves standstill 2d, obtain described lysotropic liquid crystal with diaphragm seal.
Prepared lysotropic liquid crystal is placed in polarized light microscopy Microscopic observation and has lysotropic liquid crystal phase.
Embodiment 11
Lysotropic liquid crystal of the present invention is preparing the application had in the cosmetics of lysotropic liquid crystal phase
Select the formula of table 2 to prepare cosmetics paste, preparation process is as follows:
(1) form by the raw material of A:B:C=0.53:0.11:0.36, the method for embodiment 4, preparation 3.75g lysotropic liquid crystal of the present invention (time of repose is 2d).
(2) take glycerol, Tween-80 add and fill in the beaker of deionized water, the water bath with thermostatic control being placed in 70 DEG C is heated, and is stirred to simultaneously and dissolves completely.
(3) take stearic acid, isopropyl palmitate, white oil, monoglyceride, Span-80 add in beaker, be placed in 85 DEG C of waters bath with thermostatic control and heat, be stirred to simultaneously and melt completely.
(4) under 85 DEG C of waters bath with thermostatic control, stirring condition, mixture prepared by step (2) is added in mixture prepared by step (3), continue to stir to obtain emulsion.
(5) under 85 DEG C of water bath with thermostatic control conditions, after emulsifying 3min being carried out to emulsion with 3000r/min rotating speed, the lysotropic liquid crystal prepared in step (1) is joined in emulsion system described in step (4), continue emulsifying 2min and obtain cosmetics paste.
(6) after leaving standstill 1d, observe the polarisation texture maps of cosmetics paste in step (5) with polarizing microscope, as shown in Figure 5 a, in step (5), the cosmetics paste of preparation has lysotropic liquid crystal phase to result.
Table 2 mastic formula
Embodiment 12
Lysotropic liquid crystal of the present invention is preparing the application had in the cosmetics of lysotropic liquid crystal phase
Method with embodiment 11 prepares cosmetics, and difference is: emulsifying agent rotating speed changes 2000r/min into, and emulsifying, after 5 minutes, adds lysotropic liquid crystal of the present invention and continues emulsifying 2min.As shown in Figure 5 b, the cosmetics of preparation have lysotropic liquid crystal phase to its polarisation texture maps.
Embodiment 13
Lysotropic liquid crystal of the present invention is preparing the application had in the cosmetics of lysotropic liquid crystal phase
Method with embodiment 11 prepares cosmetics, and difference is: emulsifying agent rotating speed changes 1000r/min into, and emulsifying, after 7 minutes, adds lysotropic liquid crystal of the present invention and continues emulsifying 3min.As shown in Figure 5 c, the cosmetics of preparation have lysotropic liquid crystal phase to its polarisation texture maps.
Embodiment 14
Lysotropic liquid crystal of the present invention is preparing the application had in the cosmetics of lysotropic liquid crystal phase
Described method is with embodiment 11, and difference is: change the content of described lysotropic liquid crystal in described cosmetics into 10%, and in described aqueous phase, the content of water in described cosmetics changes 63.72% into.The cosmetics of preparation have lysotropic liquid crystal phase.
Embodiment 15
Lysotropic liquid crystal of the present invention is preparing the application had in the cosmetics of lysotropic liquid crystal phase
Described method is with embodiment 11, and difference is: change the content of described lysotropic liquid crystal in described cosmetics into 12%, and in described aqueous phase, the content of water in described cosmetics changes 61.72% into.The cosmetics of preparation have lysotropic liquid crystal phase.
Comparative example 1
Method with embodiment 11 prepares cosmetics, difference is: do not prepare lysotropic liquid crystal of the present invention in advance, but hexadecanyl phosphate potassium salt used for preparation lysotropic liquid crystal of the present invention and water are incorporated to aqueous phase, fatty alcohol-polyoxyethylene ether AEO-9 is incorporated to oil phase.Under polarizing microscope, display be 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, by s1, s2 numbering, and be placed in indoor environment, investigate its weight loss situation.Result, as bright, is placed after 5 days, and the weight-loss ratio of s1 is 7.8%, and the weight-loss ratio of s2 is 10.1%, shows that the cosmetics with lysotropic liquid crystal phase have stronger water holding capacity.
Embodiment 17
Prepare cosmetics paste by the method for embodiment 13, sealing is placed in 40 DEG C of baking ovens and leaves standstill 1d, is still uniform and smooth white mastic, without layering, thinning, metachromatism after returning to room temperature.
Embodiment 18
Prepare cosmetics paste by the method for embodiment 13, sealing is placed in-10 DEG C of refrigerators and leaves standstill 1d, is still uniform and smooth white mastic, without layering, coarse, metachromatism after returning to room temperature.
Embodiment 19
Prepare cosmetics paste by the method for embodiment 13, be placed in centrifuge with the centrifugal 30min of the rotating speed of 2000r/min, without oil-water separation phenomenon.
Finally to should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.