CN104531117B - A kind of non-molten oil systems of temperature sensitive type lysotropic liquid crystal and its preparation method and application - Google Patents
A kind of non-molten oil systems of temperature sensitive type lysotropic liquid crystal and its preparation method and application Download PDFInfo
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- CN104531117B CN104531117B CN201510018779.4A CN201510018779A CN104531117B CN 104531117 B CN104531117 B CN 104531117B CN 201510018779 A CN201510018779 A CN 201510018779A CN 104531117 B CN104531117 B CN 104531117B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/26—Oil-in-water emulsions
- C09K8/28—Oil-in-water emulsions containing organic additives
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Abstract
The application provides a kind of non-molten oil systems of temperature sensitive type lysotropic liquid crystal, and the system is made of the component including following parts by weight:20 55 85 parts of 50wt% inorganic salt solutions;5 10 parts of nonionic surface active agent;5 10 parts of ionic surfactant;And the system is free of cosurfactant.The non-molten oil systems of temperature sensitive type lysotropic liquid crystal of the application meet every industrial requirements of environmental protection, are easy to transport, and are made by conventional surfactants, and preparation method is simple, and production cost is low and easy to implement.
Description
Technical field
This application involves but be not limited to a kind of molten oil systems of solute liquid crystal, and in particular, to a kind of non-molten cause liquid of temperature sensitive type
Brilliant molten oil systems and its preparation method and application.
Background technology
Lysotropic liquid crystal is the liquid crystal that a kind of two or more compounds comprising including solvated compounds are formed, and is in solution
There is liquid crystalline phase when being in a certain range in middle solute molecule concentration.Structure type includes hexagonal phase, Emission in Cubic or lamellar phase, layer
Shape phase and hexagonal phase have typical birefringent phenomenon under polarizer, and Emission in Cubic does not have.The special rheology of lysotropic liquid crystal
It is important that behavior makes it play the role of in many fields, and lyotropic lamellar phase has the lamellar structure of similar graphite, piece interlayer energy phase
To sliding, as described in 6,130,190 grades of U.S. Patent application US;It can also effectively improve the dispersion stabilization of solid matter,
As described in the grades of United States Patent (USP) US 7,931,824.What is more important, lysotropic liquid crystal have very strong solubilising power, being capable of solubilising
The oil phase of some polar/non-polars, forms emulsion oil-in-water, such as in " Functional Liquid-Crystalline
Assemblies:There is detailed report in Self-Organized Soft Materials ".Wherein, cleaning process can simplify
Be oil phase in aqueous surfactant solution is scattered, and oil droplet in water dispersed will significantly improve cleaning efficiency.
The special construction of lysotropic liquid crystal is applied for it important influence, such as such as United States Patent (USP) US7, and 791,694
Middle reported, the change of temperature, salinity and pressure can all change the structure of former lysotropic liquid crystal, and then influence lysotropic liquid crystal
Application effect.From the point of view of the document delivered at present, there have been in-depth study in foreign countries for the field, achieve certain
Progress, the report that the country is made a search for the field is less, the useful lyotropic liquid crystal flooding only in patent CN101475796
Application report.However, lysotropic liquid crystal prepared in above-mentioned document has used a large amount of auxiliary agents, dosage of surfactant is big, resists
Salt ability is poor and temperature sensitive.Therefore, before a kind of salt tolerant, the lysotropic liquid crystal of temperature-insensitive have particularly important application
Scape.
The content of the invention
On the one hand, the purpose of the application is to provide a kind of non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
Specifically, the application provides a kind of non-molten oil systems of temperature sensitive type lysotropic liquid crystal, and the system is by including following weight
The component of part is made:55-85 parts of 20-50wt% inorganic salt solutions;5-10 parts of nonionic surface active agent;Ionic surface
5-10 parts of activating agent;And the system is free of cosurfactant.
More than or in other embodiment, the nonionic surface active agent can be 5-8 parts, the ionic table
Face activating agent can be 5-8 parts.
More than or in other embodiment, the nonionic surface active agent can be selected from sorbitan oleate class
Nonionic surfactant (such as Span20, Span40, Span60 or Span65), sorbitan monooleate polyoxyethylene ether
Class nonionic surfactant (such as Tween20, Tween40, Tween60 or Tween80), polyoxyethylene non-ionic surface are lived
Property agent (such as 4 ether C of dodecyl polyoxyethylene12EO4, 9 ether C of dodecyl polyoxyethylene12EO9, 23 ether of dodecyl polyoxyethylene
C12EO23) or its combination;The ionic surfactant can be selected from Sulfonates, Sulfates, metal carboxylate (such as 12
Sodium alkyl sulfate SDS, Cocoamidopropyl betaine CAB, dodecyl sodium sulfate AS, sodium sulfate of polyethenoxy ether of fatty alcohol
AES), dodecanamide propyl decil lactone ionic surfactant or its combination.
More than or in other embodiment, the inorganic salts can be one kind in sodium salt, calcium salt or aluminium salt or
It is a variety of.Such as water-soluble NaCl, CaCl2.Also, the application is primarily directed to high calcium salt system.
More than or in other embodiment, the inorganic salt solution is the calcium chloride of mass percent 20%-40%
Aqueous solution.
On the other hand, the purpose of the application is in providing above-mentioned system in the oil phase for dissolving polarity alkanes
Purposes.
More than or in other embodiment, the oil phase can be white oil or atoleine.
In other respects, the application provides the purposes that system as described above is used for completion cleaning solution.
In a further aspect, the application provides one kind and is used to prepare the above-described non-molten oil systems of temperature sensitive type lysotropic liquid crystal
Method, including:Take each component of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer,
If it is observed that oil stripping shape decorative pattern, and using the rheological equationm of state of rheometer measurement system, if the rheological equationm of state for elastic modulus G '
It is parallel and be more than viscous modulus G ", that is, obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
More than or in other embodiment, wherein can by each group lease making water-bath of formula ratio, be stirred until homogeneous, band it is viscous
The system of property, is cooled to room temperature;The speed of wherein described stirring is 200-300 revs/min, and water solution temperature is 70-90 DEG C.
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal of the application are a kind of tables using non-temperature sensitive type lysotropic liquid crystal as cleaning agent
Face aqueous surfactant solutions system, there is good solubilising power under high temperature, high salt conditions, is the harsh bar such as high temperature, high salinity
Greasy dirt cleaning under part provides possibility, has broad application prospects." non-temperature sensitive " described herein is referred in 25-75
In the range of DEG C, structure, the rheological property of system do not change.
Also, the non-molten oil systems of temperature sensitive type lysotropic liquid crystal of the application are a kind of low cost, low surfactant, to temperature
The molten oil systems of the simple lysotropic liquid crystal of insensitive and preparation method.Also, the system of the application is free of surface-active auxiliary agent such as
There is the alcohols of certain injury with stronger volatility and to human body.
The appearance of the molten oil systems of lysotropic liquid crystal of the application is translucent bit bluish liquid, has necessarily steady in a long-term
Property (it is unchanged that half a year above appearance is placed at room temperature, i.e., without obvious layering and sedimentation phenomenon, samples and observed under polarizer,
It was observed that oil stripping shape decorative pattern, and the elastic modulus G of the system measured using rheometer ' parallel and it is more than viscous modulus G ", table
There is not significant change in the structure of phaneroplasm system);High-temperature stability is good, and (after when placement 15-18 is small at 120 DEG C, appearance is without bright
Aobvious change, i.e., without obvious layering and sedimentation phenomenon, sample and observed under polarizer, it was observed that oil stripping shape decorative pattern, and utilize rheology
The elastic modulus G for the system that instrument is measured ' parallel and it is more than viscous modulus G ", illustrates that the high-temperature stability of lysotropic liquid crystal is good);
Low-temperature stability is good, and (after being placed on when 5-8 is small at -10-0 DEG C, appearance is without significant change, i.e., without obvious layering and sedimentation phenomenon.
Sampling is observed under polarizer, it was observed that oil stripping shape decorative pattern, and the elastic modulus G of the system measured using rheometer ' parallel
And it is more than viscous modulus G ", illustrate that the low-temperature stability of lysotropic liquid crystal is good).
To sum up, the molten oil systems of the lysotropic liquid crystal of the application have following benefit:
(1) the non-molten oil systems of temperature sensitive type lysotropic liquid crystal of the application meet every industrial requirements of environmental protection, are easy to transport, and
It is made by conventional surfactants, preparation method is simple, and production cost is low and easy to implement;
(2) the non-molten oil systems of temperature sensitive type lysotropic liquid crystal of the application are to temperature-insensitive, and the change of temperature is to its rheological characteristic
Almost do not influence;
(3) the non-molten oil systems of temperature sensitive type lysotropic liquid crystal of the application can be used in the cleaning process in completion, so far
Have no report, which provides new method for oil exploitation.
Brief description of the drawings
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal texture picture under petrographic microscope in Fig. 1 embodiments herein 1
And the outside drawing after molten oil (LC is lysotropic liquid crystal, and 10%, 20% represents molten oil mass).
The rheological curves of the non-molten oil systems of temperature sensitive type lysotropic liquid crystal in Fig. 2 embodiments herein 1.
The apparent viscosity of the non-molten oil systems of temperature sensitive type lysotropic liquid crystal at different temperatures in Fig. 3 embodiments herein 1
The texture picture of change and lysotropic liquid crystal under polarizer.
Embodiment
Presently filed embodiment is described below by embodiment, it will be appreciated by the person skilled in the art that these
Specific embodiment only indicates that to the implementation technical solution for achieving the purpose that the application and selecting, and is not to technical solution
Limitation.According to teachings of the present application, it is obvious with reference to improvement of the prior art to technical scheme, belongs to the application
The scope of protection.
In the following embodiments of the application, used chemicals is commercial products.
Embodiment 1
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal, the system are made of the component of following parts by weight:
The CaCl of 60 parts of 40wt%2Aqueous solution, 5 parts of C12EO9(it is purchased from:Japanese Nikkol companies), 5 parts of AES (are purchased from:Moral
BASF AG of state), 5 parts of CAB (are purchased from:Shandong Lv Sen Chemical Co., Ltd.s).
Its preparation method is as follows:
Take the above components of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer,
If it is observed that oil stripping shape decorative pattern, and using rheometer measurement system elastic modulus G ' parallel and be more than viscous modulus G ", i.e.,
Obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
Investigate the high-temperature stability, steady in a long-term of the non-molten oil systems of temperature sensitive type lysotropic liquid crystal of preparation by the following method respectively
Property, low-temperature stability and add after oil phase the appearance and particle diameter of lotion formed, refer to wherein adding oil phase at 70 DEG C upwards
The molten oil systems of non-temperature sensitive type lysotropic liquid crystal are stated to add 25 parts of white oils and be cooled to room within 5 minutes with 300 revs/min of rotating speed stirring
Temperature, wherein 70 DEG C of temperature-rise periods mainly simulated during field application in embodiments herein.
The stability measurement of the non-molten oil systems of temperature sensitive type lysotropic liquid crystal:
Long-time stability:By product static placement for a long time at 25 DEG C, appearance is observed, is noticed that whether occur clearly dividing
Layer, samples and is observed under polarizer, if it was observed that oil stripping shape decorative pattern, while the elastic modulus G of utilization rheometer measurement system '
With the relation of viscous modulus G ".
High-temperature stability:When sample is placed on constant temperature 15-18 is small in 120 DEG C of high temperature furnaces, observe appearance, if layering or
Sedimentation, samples and is observed under polarizer, if it was observed that oil stripping shape decorative pattern, while utilize the elasticity modulus of rheometer measurement system
The relation of G ' and viscous modulus G ".
Low-temperature stability:Sample is placed in refrigerator (about -10 DEG C), observes appearance, if layering or sedimentation, sample
Observed under polarizer, if it was observed that oil stripping shape decorative pattern, while the elastic modulus G ' using rheometer measurement system and sticky mould
Measure the relation of G ".
Emulsion appearance and grain diameter measurement:
At room temperature, the lotion being formed as described above is stood and observes appearance after stablizing;Surveyed according to dynamic light scattering (DLS)
Determine the method measure emulsion particle diameter of emulsion particle diameter, measuring method such as document " Highly Stable Concentrated
Nanoemulsions by the Phase Inversion Composition Method at Elevated
Temperature " is described.Wherein, after adding oil phase, emulsion particle diameter is smaller, then the stability of system is higher.
The results are shown in Table 1:
Product appearance | It is transparent |
Long-time stability | Place six months and be not layered |
High-temperature stability | Stablize |
Low-temperature stability | Stablize |
The particle diameter (nm) of the lotion formed is added after oil phase | 25 |
Table 1
Wherein, Fig. 1 shows cosmetic variation of the lyotropic crystal system before and after oil phase is added in embodiment 1;Fig. 2 is molten cause
The rheological curves of liquid crystal system at normal temperatures, rheological curves illustrate that system carries special structure;Fig. 3 shows lysotropic liquid crystal
The apparent viscosity variation with temperature situation of system, as can be seen from Figure 3 apparent viscosity there is no variation with temperature and occur bright
Aobvious change, while there is no too big difference in appearance yet, so as to illustrate that the system is non-responsive to temperature type.
Embodiment 2
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal, the system are made of the component of following parts by weight:
The CaCl of 70 parts of 20wt%2Aqueous solution, 5 parts of C12EO9(it is purchased from:Japanese Nikkol companies), 5 parts of AES (are purchased from:Moral
BASF AG of state), 5 parts of CAB (are purchased from:Shandong Lv Sen Chemical Co., Ltd.s).
Its preparation method is as follows:
Take the above components of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer,
If it is observed that oil stripping shape decorative pattern, and using rheometer measurement system elastic modulus G ' parallel and be more than viscous modulus G ", i.e.,
Obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
High-temperature stability, the length of the prepared non-molten oil systems of temperature sensitive type lysotropic liquid crystal are investigated by the method in embodiment 1
Phase stability, low-temperature stability and the appearance and particle diameter that add after molten oil the lotion formed, refer at 70 DEG C wherein adding molten oil
It is lower to add 15 parts of white oils to the above-mentioned non-molten oil systems of temperature sensitive type lysotropic liquid crystal and cooling in 5 minutes is stirred with 300 revs/min of rotating speed
To room temperature.
The results are shown in Table 2:
Product appearance | It is translucent |
Long-time stability | Place six months and be not layered |
High-temperature stability | Stablize |
Low-temperature stability | Stablize |
The particle diameter (nm) of the lotion formed is added after oil phase | 28 |
Table 2
Embodiment 3
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal, the system are made of the component of following parts by weight:
The CaCl of 60 parts of 40wt%2Aqueous solution, 10 parts of C12EO9(it is purchased from:Japanese Nikkol companies), 5 parts of AES (are purchased from:Moral
BASF AG of state), 5 parts of CAB (are purchased from:Shandong Lv Sen Chemical Co., Ltd.s).
Its preparation method is as follows:
Take the above components of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer,
If it is observed that oil stripping shape decorative pattern, and using rheometer measurement system elastic modulus G ' parallel and be more than viscous modulus G ", i.e.,
Obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
High-temperature stability, the length of the prepared non-molten oil systems of temperature sensitive type lysotropic liquid crystal are investigated by the method in embodiment 1
Phase stability, low-temperature stability and the appearance and particle diameter that add after molten oil the lotion formed, refer at 70 DEG C wherein adding molten oil
It is lower to add 20 parts of white oils to the above-mentioned non-molten oil systems of temperature sensitive type lysotropic liquid crystal and cooling in 5 minutes is stirred with 300 revs/min of rotating speed
To room temperature.
The results are shown in Table 3:
Product appearance | It is muddy |
Long-time stability | Place six months and be not layered |
High-temperature stability | Stablize |
Low-temperature stability | Stablize |
The particle diameter (nm) of the lotion formed is added after oil phase | 78 |
Table 3
Embodiment 4
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal, the system are made of the component of following parts by weight:
The CaCl of 55 parts of 40wt%2Aqueous solution, 10 parts of C12EO9(it is purchased from:Japanese Nikkol companies), 5 parts of AES (are purchased from:Moral
BASF AG of state), 10 parts of CAB (are purchased from:Shandong Lv Sen Chemical Co., Ltd.s).
Its preparation method is as follows:
Take the above components of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer,
If it is observed that oil stripping shape decorative pattern, and using rheometer measurement system elastic modulus G ' parallel and be more than viscous modulus G ", i.e.,
Obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
High-temperature stability, the length of the prepared non-molten oil systems of temperature sensitive type lysotropic liquid crystal are investigated by the method in embodiment 1
Phase stability, low-temperature stability and the appearance and particle diameter that add after molten oil the lotion formed, refer at 70 DEG C wherein adding molten oil
It is lower to add 20 parts of white oils to the above-mentioned non-molten oil systems of temperature sensitive type lysotropic liquid crystal and cooling in 5 minutes is stirred with 300 revs/min of rotating speed
To room temperature.
The results are shown in Table 4:
Product appearance | Slightly, light blue translucent |
Long-time stability | Place six months and be not layered |
High-temperature stability | Stablize |
Low-temperature stability | Stablize |
The particle diameter (nm) of the lotion formed is added after oil phase | 90 |
Table 4
Embodiment 5
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal, the system are made of the component of following parts by weight:
The CaCl of 80 parts of 40wt%2Aqueous solution, 5 parts of C12EO9(it is purchased from:Japanese Nikkol companies), 5 parts of AES (are purchased from:Moral
BASF AG of state), 10 parts of CAB (are purchased from:Shandong Lv Sen Chemical Co., Ltd.s).
Its preparation method is as follows:
Take the above components of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer,
If it is observed that oil stripping shape decorative pattern, and using rheometer measurement system elastic modulus G ' parallel and be more than viscous modulus G ", i.e.,
Obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
High-temperature stability, the length of the prepared non-molten oil systems of temperature sensitive type lysotropic liquid crystal are investigated by the method in embodiment 1
Phase stability, low-temperature stability and the appearance and particle diameter that add after molten oil the lotion formed, refer at 70 DEG C wherein adding molten oil
It is lower to add 5 parts of white oils to the above-mentioned non-molten oil systems of temperature sensitive type lysotropic liquid crystal and cooling in 5 minutes is stirred with 300 revs/min of rotating speed
To room temperature.
The results are shown in Table 5:
Product appearance | It is transparent |
Long-time stability | Place six months and be not layered |
High-temperature stability | Stablize |
Low-temperature stability | Stablize |
The particle diameter (nm) of the lotion formed is added after oil phase | 73 |
Table 5
Embodiment 6
The non-molten oil systems of temperature sensitive type lysotropic liquid crystal, the system are made of the component of following parts by weight:
The CaCl of 55 parts of 40wt%2Aqueous solution, 5 parts of C12EO9(it is purchased from:Japanese Nikkol companies), 5 parts of AES (are purchased from:Moral
BASF AG of state), 5 parts of CAB (are purchased from:Shandong Lv Sen Chemical Co., Ltd.s).
Its preparation method is as follows:
Take the above components of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer,
If it is observed that oil stripping shape decorative pattern, and using rheometer measurement system elastic modulus G ' parallel and be more than viscous modulus G ", i.e.,
Obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
High-temperature stability, the length of the prepared non-molten oil systems of temperature sensitive type lysotropic liquid crystal are investigated by the method in embodiment 1
Phase stability, low-temperature stability and the appearance and particle diameter that add after molten oil the lotion formed, refer at 70 DEG C wherein adding molten oil
It is lower to add 30 parts of white oils to the above-mentioned non-molten oil systems of temperature sensitive type lysotropic liquid crystal and cooling in 5 minutes is stirred with 300 revs/min of rotating speed
To room temperature.
The results are shown in Table 6:
Product appearance | Milky, muddiness |
Long-time stability | Place three months and be not layered |
High-temperature stability | Stablize |
Low-temperature stability | Stablize |
The particle diameter (nm) of the lotion formed is added after oil phase | 65 |
Table 6
Upper described is only the preferred embodiment of the application, not the application is made in any form with substantial limit
System.Those skilled in the art, in the range of technical scheme is not departed from, in using disclosed above technology
The equivalent variations of a little change, modification and the differentiation holding and make are the equivalent embodiment of the application;It is meanwhile all according to this Shen
The changes of any equivalent variations that substantial technological please makees above example, modification are with developing etc. in the application by weighing
Profit is required in the range of defining.
Claims (7)
1. a kind of non-molten oil systems of temperature sensitive type lysotropic liquid crystal, the system are made of the component including following parts by weight:Quality hundred
Divide than 55-85 parts of the calcium chloride water for 20%-40%;5-10 parts of polyoxyethylene nonionic surface active agent;Ion
5-10 parts of type surfactant;
Wherein described system is free of cosurfactant, and wherein described ionic surfactant is cocamidopropyl propyl amide beet
The combination of alkali and sodium sulfate of polyethenoxy ether of fatty alcohol;The polyoxyethylene nonionic surface active agent is selected from dodecyl
4 ether C12EO4 of polyoxyethylene, 9 ether C12EO9 of dodecyl polyoxyethylene, 23 ether C12EO23 of dodecyl polyoxyethylene or its group
Close.
2. system according to claim 1, wherein, the polyoxyethylene nonionic surface active agent is 5-8 parts, institute
Ionic surfactant is stated as 5-8 parts.
3. purposes of the system in the oil phase for dissolving polarity alkanes as any one of claim 1-2.
4. purposes according to claim 3, wherein, the oil phase is white oil or atoleine.
5. the system as any one of claim 1-2 is used for the purposes of completion cleaning solution.
6. a kind of method for being used to prepare the non-molten oil systems of temperature sensitive type lysotropic liquid crystal as any one of claim 1-2,
Including:Take each component of formula ratio and be stirred until homogeneous, adhesive system, then sample and observed under polarizer, if seen
Observe oil stripping shape decorative pattern, and using the rheological equationm of state of rheometer measurement system, if the rheological equationm of state for elastic modulus G ' parallel and
More than viscous modulus G ", that is, obtain the non-molten oil systems of temperature sensitive type lysotropic liquid crystal.
7. method as claimed in claim 6, wherein by each group lease making water-bath of formula ratio, being stirred until homogeneous, adhesive body
System, is cooled to room temperature;The speed of wherein described stirring is 200-300 revs/min, and water solution temperature is 70-90 DEG C.
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