CN104874326A - Preparation method of intelligent wormlike micelle - Google Patents
Preparation method of intelligent wormlike micelle Download PDFInfo
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- CN104874326A CN104874326A CN201510171008.9A CN201510171008A CN104874326A CN 104874326 A CN104874326 A CN 104874326A CN 201510171008 A CN201510171008 A CN 201510171008A CN 104874326 A CN104874326 A CN 104874326A
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- enuatrol
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- vermiculate glues
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Abstract
The invention relates to a preparation method of an intelligent wormlike micelle, and belongs to the technical field of application of surfactants. The intelligent wormlike micelle is prepared by inducing sodium oleate (NaOA) by using organic cation salt at temperature of 15-40 DEG C and adjusting the pH to be 8-10. The character of the wormlike micelle can change along with the change of pH value, so that the wormlike micelle has pH responsiveness.
Description
Technical field
This technology relates to a kind of preparation method of intelligent vermiculate glues, belongs to the applied technical field of surfactant.
Background technology
Surfactant comprises Small molecular and high molecular surfactant, both forms the multiple orderly body such as micella and vesica by molecular self-assembling.Vermiculate glues, refer to there is ad hoc structure surfactant under certain condition, increase the flexibility that formed bar-shaped or cylindrical micellar by spherical micelle along non axial one dimension through self assembly in the solution.Vermiculate glues is wound around mutually, forms instantaneous three-dimensional net structure, macroscopically shows the viscoelasticity being similar to polymer solution.
When intelligent vermiculate glues refers to that minor variations occurs external environmental condition (temperature, pH, electrolyte concentration, optical, electrical field etc.), its physicochemical properties (surface tension, aggregated forms etc.) can produce the surfactant obviously changed.Its in oil field, the numerous areas such as medicine controlled releasing, bioengineering, microfluid, cosmetics has important using value.
Enuatrol (NaOA), be a kind of flaxen grease-like solid, have good solubility in the hot water, aqueous solution facile hydrolysis alkalize, alcohol liquid is not hydrolyzed.Have it to be a kind of carboxylate anion's surfactant, containing 18 carbon atoms in molecule, containing a unsaturated bond in hydrophobic chain, very well water-soluble, its raw materials for production can regenerate, cheap, aboundresources.The emulsifying ability that enuatrol is excellent, penetration and detergency, in a lot of field as cleaning agent, anticorrisive agent, fabric waterproofing agent are widely used.In recent years about the research of vermiculate glues has many bibliographical informations, dominant cation surfactant is main.Also someone studies anionic vermiculate glues, as the people such as prune assistant have studied the vermiculate glues containing Na ionic electrolytes induction NaOA formation such as NaCO3, NaPO3.The people such as Kalur have studied the vermiculate glues that KCl induces enuatrol to be formed.
Summary of the invention
The invention provides a kind of intelligent vermiculate glues, to pH value sensitive, there is certain PH response.
A preparation method for intelligent vermiculate glues, comprises the following steps:
(1) preparation of mother liquor
Preparation enuatrol mother liquor, organic cation salt mother liquor, hydrochloric acid solution and sodium hydroxide solution;
(2) preparation of enuatrol/organic cation salt system
Pipette enuatrol mother liquor respectively, organic cation salt mother liquor mixes and is diluted with water, through stir/shaking and carrying out ultrasonic water bath after mixing, leave standstill;
(3) preparation of intelligent vermiculate glues
The enuatrol that step (2) obtains/organic cation salt system, control temperature is at 15 ~ 40 DEG C, after the hydrochloric acid solution adding step (1) gained and sodium hydroxide solution adjust ph value 8 ~ 10, after the system that is mixed to is homogeneous, namely obtain the intelligent vermiculate glues to pH value response.
Further, described organic cation salt is one of following: benzyltrimethylammonium bromide (Benzyltrimethyl ammonium bromide, BTAB), triethylamine hydrochloride (Ethanamine, N, N-diethyl-, hydrochloride, Et3NHCl) or triethanolamine hydrochloride (Triethanolamine hydrochloride, TEA).
Further, in described step (1), the molar concentration of enuatrol mother liquor is 0.2 ~ 0.3 mol/L, and the concentration of organic cation salt mother liquor is molar concentration 0.8 ~ 1.0 mol/L, and the mass concentration of hydrochloric acid solution is 30 ~ 37%, and sodium hydroxide solution is its saturated solution.
Further, described step (2) ultrasonic water bath supersonic frequency 30 ~ 35kHz ultrasonic time 8 ~ 12 min, time of repose 12 ~ 14h.
Further, described step (2) enuatrol molar concentration is all 0.1 ~ 0.15 mol/L, for enuatrol/benzyltrimethylammonium bromide system, benzyltrimethylammonium bromide molar concentration is 0.1 ~ 0.5 mol/L, for enuatrol/triethylamine hydrochloride system, triethylamine hydrochloride molar concentration is 0.1 ~ 0.5 mol/L, and for enuatrol/triethanolamine hydrochloride system, triethanolamine hydrochloride molar concentration is 0.2 ~ 0.4 mol/L.
Further, in described step (3), enuatrol/benzyltrimethylammonium bromide system adjust ph is 8 ~ 9, and enuatrol/triethylamine hydrochloride system adjust ph is 8.0 ~ 9.5, and enuatrol/triethanolamine hydrochloride system adjust ph is 9 ~ 10.
Further, the mode of mixing adopts stirrings/concussion also ultrasonic water bath or mix rear standing 10 ~ 60 min in described step (3).
Further, in described step (3), the supersonic frequency of ultrasonic water bath chooses 30 ~ 35kHz.
Beneficial effect of the present invention:
The preparation method of the intelligent worm dress micella that the present invention proposes, raw material composition is simple, cheap, the vermiculate glues viscosity formed is large, and the sensitive to pH, there is certain responsive intelligent, in the field such as controlled release of medicine, there is very large application potential.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is under different pH, the relation between the shear viscosity of NaOA/BTAB system and shear rate;
Fig. 2 is under different pH, the relation between the shear viscosity of NaOA/Et3NHCl system and shear rate;
Fig. 3 is under different pH, the relation between the shear viscosity of NaOA/TEAHCl system and shear rate;
Fig. 4 is when pH=8.45, the relation of NaOA/BTAB system shear viscosity and complex viscosity and shear rate and angle of throw frequency
Fig. 5 is under different pH, the Cole-Cole figure of NaOA/ Et3NHCl system;
Fig. 6 is under different pH, the Cole-Cole figure of NaOA/ TEAHCl system.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for intelligent vermiculate glues, comprises the following steps:
(1) preparation of mother liquor
Prepare enuatrol mother liquor, benzyltrimethylammonium bromide mother liquor, hydrochloric acid solution and sodium hydroxide solution respectively; Wherein the molar concentration of enuatrol mother liquor is 0.2 mol/L, and the molar concentration of benzyltrimethylammonium bromide mother liquor is 0.8 mol/L, and the mass concentration of hydrochloric acid solution is 30%, and sodium hydroxide solution is its saturated solution;
(2) preparation of enuatrol/organic cation salt system
Pipette enuatrol mother liquor respectively, benzyltrimethylammonium bromide mother liquor mixes and to be diluted with water to enuatrol molar concentration be 0.1 mol/L, BTAB molar concentration is 0.1mol/L, through stir/shaking and choosing 30 ~ 35kHz ultrasonic water bath 8 ~ 12 min after mixing, rear standing 12 ~ 14 h, obtain enuatrol/benzyltrimethylammonium bromide (NaOA/BTAB) system;
(3) preparation of pH response type intelligent vermiculate glues
The NaOA/BTAB system that step (2) obtains, the hydrochloric acid solution and the sodium hydroxide solution adjust ph that add step (1) gained are 8, stir/shake and choose 30 ~ 35kHz ultrasonic water bath homogeneous to system after namely obtain to pH value response intelligent vermiculate glues.
Embodiment 2
A preparation method for intelligent vermiculate glues, its operation is identical with embodiment 1, and distinguishing characteristics is: in described step (2), BTAB being diluted to molar concentration is 0.3 mol/L; PH value is regulated to be 8.5 in described step (3).
Embodiment 3
A preparation method for intelligent vermiculate glues, its operation is identical with embodiment 1, and distinguishing characteristics is: in described step (2), BTAB being diluted to molar concentration is 0.5 mol/L; PH value is regulated to be 9 in described step (3).
Embodiment 4
A preparation method for intelligent vermiculate glues, comprises the following steps:
(1) preparation of mother liquor
Prepare enuatrol mother liquor, triethylamine hydrochloride mother liquor, hydrochloric acid solution and sodium hydroxide solution respectively; Wherein the molar concentration of enuatrol mother liquor is 0.24 mol/L, and the molar concentration of triethylamine hydrochloride mother liquor is 1 mol/L, and the mass concentration of hydrochloric acid solution is 35%, and sodium hydroxide solution is its saturated solution;
(2) preparation of enuatrol/organic cation salt system
Pipette enuatrol mother liquor respectively, triethylamine hydrochloride mother liquor mixes and be diluted with water to that concentrations of sodium oleate is 0.12 mol/L, triethylamine hydrochloride concentration is 0.1 mol/L, through stir/shaking and choosing 30 ~ 35kHz ultrasonic water bath 8 ~ 12 min after mixing, rear standing 12 ~ 14 h, obtain enuatrol/triethylamine hydrochloride (NaOA/Et3NHCl) system;
(3) preparation of pH response type intelligent vermiculate glues
The NaOA/Et3NHCl system that step (2) obtains, the hydrochloric acid solution and the sodium hydroxide solution adjust ph that add step (1) gained are 8.0, mix rear leave standstill 10 ~ 60 min homogeneous to system after namely obtain to pH value response intelligent vermiculate glues.
Embodiment 5
A preparation method for intelligent vermiculate glues, its operation is identical with embodiment 4, and distinguishing characteristics is: be 0.3 mol/L by triethylamine hydrochloride concentration in described step (2); PH value is regulated to be 9 in described step (3).
Embodiment 6
A preparation method for intelligent vermiculate glues, its operation is identical with embodiment 4, and distinguishing characteristics is: be 0.5 mol/L by triethylamine hydrochloride concentration in described step (2); ; PH value is regulated to be 9.5 in described step (3).
Embodiment 7
A preparation method for intelligent vermiculate glues, comprises the following steps:
(1) preparation of mother liquor
Prepare enuatrol mother liquor, triethanolamine hydrochloride mother liquor, hydrochloric acid solution and sodium hydroxide solution respectively; Wherein the molar concentration of enuatrol mother liquor is 0.3 mol/L, and the molar concentration of triethanolamine hydrochloride mother liquor is 1 mol/L, and the mass concentration of hydrochloric acid solution is 37%, and sodium hydroxide solution molar concentration is 4.0 mol/L;
(2) preparation of enuatrol/organic cation salt system
Pipette enuatrol mother liquor respectively, triethanolamine hydrochloride mother liquor mixes and is diluted with water to enuatrol molar concentration is 0.15 mol/L, triethanolamine hydrochloride concentration is 0.2mol/L; Through stir/shaking and choosing 30 ~ 35kHz ultrasonic water bath, 8 ~ 12min after mixing, rear standing 12 ~ 14 h, obtain enuatrol/triethanolamine hydrochloride (NaOA/TEAHCl) system;
(3) preparation of pH response type intelligent vermiculate glues
The NaOA/TEAHCl system that step (2) obtains, the hydrochloric acid solution and the sodium hydroxide solution adjust ph that add step (1) gained are 9; Stir/shake and choose 30 ~ 35kHz ultrasonic water bath homogeneous to system after namely obtain to pH value response intelligent vermiculate glues.
Embodiment 8
A preparation method for intelligent vermiculate glues, its operation is identical with embodiment 4, and distinguishing characteristics is: be 0.3 mol/L by triethanolamine hydrochloride concentration in described step (2); PH value is regulated to be 9.5 in described step (3).
Embodiment 9
A preparation method for intelligent vermiculate glues, its operation is identical with embodiment 4, and distinguishing characteristics is: be 0.4mol/L by triethanolamine hydrochloride concentration in described step (2); PH value is regulated to be 10 in described step (3).
The inspection that vermiculate glues is formed
The formation of vermiculate glues in the present invention's 3 kinds of systems is checked by rheol method, intelligent vermiculate glues respectively obtained by Example 1, embodiment 4 and embodiment 7, under pH environment, measure the relation of their relevant shear viscosity (ordinate) and shear rate (abscissa).FIG 1, FIG 2 and FIG 3.For NaOA/BTAB system, when pH lower than 8.90 time, all curves all present shear thinning phenomenon, illustrate in solution and have vermiculate glues to generate; For NaOA/Et3NHCl system, when pH value is less than 9.02, all curves all present shear thinning phenomenon, illustrate in solution and have vermiculate glues to generate; For NaOA/TEAHCl system, when pH value is less than 12.75, all curves all present shear thinning phenomenon, illustrate in solution and have vermiculate glues to generate.
The formation of vermiculate glues also can be proved in addition by Cox-Merz rule and Cole-Cole figure.For NaOA/BTAB system, when pH=8.58, the shear viscosity recorded by flow graph is mapped to shear rate, and " complex viscosity versus frequency through calculating is mapped, as shown in Figure 4 with being obtained the storage modulus G' of system by frequency scanning to loss modulus G.In Fig. 4, ordinate is only numerical value, and abscissa is shear rate and the hunting angle frequency of identical numerical value.As seen from Figure 4, this system is when pH=8.58, and its shear viscosity and complex viscosity at an order of magnitude, meet Cox-Merz rule substantially, illustrates that this system defines vermiculate glues.Fig. 5 is that NaOA/Et3NHCl system Cole-Cole schemes, and Fig. 6 is the Cole-Cole figure of NaOA/ TEAHCl system, and the two also defines vermiculate glues in provable above-mentioned system.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a preparation method for intelligent vermiculate glues, is characterized in that, comprises the following steps:
(1) preparation of mother liquor
Prepare enuatrol mother liquor, organic cation salt mother liquor, sodium hydroxide solution and hydrochloric acid solution respectively;
(2) preparation of enuatrol/organic cation salt system
Pipette enuatrol mother liquor respectively, organic cation salt mother liquor mixes and is diluted with water, through stir/shaking and carrying out ultrasonic water bath after mixing, leave standstill;
(3) preparation of pH response type intelligent vermiculate glues
After using pH value to 8 ~ 10 of the hydrochloric acid solution of step (1) gained and the enuatrol/organic cation salt system of sodium hydroxide solution regulating step (2) gained, control temperature, within the scope of 15 ~ 40 DEG C, namely obtains the intelligent vermiculate glues to pH response after the system that is mixed to is homogeneous.
2. the preparation method of a kind of intelligent vermiculate glues according to claim 1, is characterized in that, described organic cation salt is one of following: benzyltrimethylammonium bromide, triethylamine hydrochloride or triethanolamine hydrochloride.
3. the preparation method of a kind of intelligent worm dress micella according to claim 1, it is characterized in that: in described step (1), the molar concentration of enuatrol mother liquor is 0.2 ~ 0.3 mol/L, the molar concentration of organic cation salt mother liquor is 0.8 ~ 1.0mol/L, the mass concentration of hydrochloric acid solution is 30 ~ 37%, and sodium hydroxide solution is its saturated solution.
4. the preparation method of a kind of intelligent vermiculate glues according to claim 1, is characterized in that: described step (2) ultrasonic water bath supersonic frequency 30 ~ 35kHz, ultrasonic time 8 ~ 12 min, time of repose 12 ~ 14 h.
5. the preparation method of a kind of intelligent vermiculate glues according to claim 1, it is characterized in that: described step (2) concentrations of sodium oleate is all 0.1 ~ 0.15 mol/L, for enuatrol/benzyltrimethylammonium bromide system, benzyltrimethylammonium bromide concentration is 0.1 ~ 0.5 mol/L, for enuatrol/triethylamine hydrochloride system, triethylamine hydrochloride concentration is 0.1 ~ 0.5 mol/L, and for enuatrol/triethanolamine hydrochloride system, triethanolamine hydrochloride concentration is 0.2 ~ 0.4 mol/L.
6. the preparation method of a kind of intelligent vermiculate glues according to claim 1, it is characterized in that: in described step (3), enuatrol/benzyltrimethylammonium bromide system adjust ph is 8 ~ 9, enuatrol/triethylamine hydrochloride system adjust ph is 8.0 ~ 9.5, and enuatrol/triethanolamine hydrochloride system adjust ph is 9 ~ 10.
7. the preparation method of a kind of intelligent vermiculate glues according to claim 1, is characterized in that: the mode of mixing adopts stirrings/concussion also ultrasonic water bath or mix rear standing 10 ~ 60 min in described step (3).
8. the preparation method of a kind of intelligent vermiculate glues according to claim 7, is characterized in that: in described step (3), the supersonic frequency of ultrasonic water bath chooses 30 ~ 35kHz.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108837770A (en) * | 2018-06-25 | 2018-11-20 | 江南大学 | The four poly- surfactant worm-like micelle systems containing azobenzene group |
| CN108837771A (en) * | 2018-06-25 | 2018-11-20 | 江南大学 | A kind of dimeric surfactant vermiculate glues and preparation method thereof |
| CN108863817A (en) * | 2018-06-25 | 2018-11-23 | 江南大学 | The vermiculate glues that the four poly- surfactants based on electrostatic are constructed |
| CN108970535A (en) * | 2018-06-25 | 2018-12-11 | 江南大学 | A kind of dimeric surfactant vermiculate glues and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108837770A (en) * | 2018-06-25 | 2018-11-20 | 江南大学 | The four poly- surfactant worm-like micelle systems containing azobenzene group |
| CN108837771A (en) * | 2018-06-25 | 2018-11-20 | 江南大学 | A kind of dimeric surfactant vermiculate glues and preparation method thereof |
| CN108863817A (en) * | 2018-06-25 | 2018-11-23 | 江南大学 | The vermiculate glues that the four poly- surfactants based on electrostatic are constructed |
| CN108970535A (en) * | 2018-06-25 | 2018-12-11 | 江南大学 | A kind of dimeric surfactant vermiculate glues and preparation method thereof |
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