CN114632478B - Preparation method of Pickering emulsion gel based on modified attapulgite clay - Google Patents
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- CN114632478B CN114632478B CN202210062085.0A CN202210062085A CN114632478B CN 114632478 B CN114632478 B CN 114632478B CN 202210062085 A CN202210062085 A CN 202210062085A CN 114632478 B CN114632478 B CN 114632478B
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Abstract
The invention relates to a preparation method of Pickering emulsion gel based on modified attapulgite clay, which comprises the steps of firstly modifying the attapulgite clay to obtain modified attapulgite clay, wherein the modified attapulgite clay has certain hydrophobicity, and in the process of preparing Pickering emulsion gel, the modified attapulgite clay is dispersed in an aqueous phase, and after homogenization, the modified attapulgite clay is crosslinked into a net-shaped or cage-shaped structure in the aqueous phase, and oil drops are wrapped in the modified attapulgite clay to form stable oil-in-water Pickering emulsion gel. The formed emulsion gel has good stability even under the condition of less oil, stable gel structure and long-term stability, good temperature resistance and salt resistance effect, is easy to degrade, and can stabilize various oil phases (C9-C16 liquid straight-chain alkane, aromatic hydrocarbon, diesel oil, crude oil or edible oil); has wide application prospect in the fields of functional grease construction, daily necessities grease construction and the like.
Description
Technical Field
The invention relates to a preparation method of Pickering emulsion gel based on modified attapulgite clay, belonging to the field of new materials.
Background
Pickering emulsion is a novel emulsion which is stabilized by micro-nano scale solid particles instead of traditional organic surfactants. In order to enable the solid particles to effectively emulsify and disperse the oil phase, the solid particles are required to be wetted by oil and water respectively, and micro-nano solid particles with proper wettability are required to be adsorbed on an oil/water interface and form a stable interfacial film, so that the emulsification and dispersion effects are achieved. The Pickering emulsion gel is characterized in that on the basis of Pickering emulsion, solid particles are self-assembled or bridged into a three-dimensional network structure in a continuous phase under certain conditions, so that the whole emulsion system can achieve solid-like gel, has strong mechanical strength, becomes stable and is not easy to break, and a gel medium generally contains dispersed water drops or dispersed oil drops; because of the special structure and property of the emulsion gel, the emulsion gel has wide application in the fields of biological medicine, food processing, new material manufacturing, oily wastewater treatment and the like.
The existing emulsion gel is mainly a hydrogel system containing dispersed oil drops, starch, cellulose, protein substances and polymer colloid materials are used as solid particles for preparing Pickering emulsion, the materials generally need certain hydrophobic modification to achieve a good emulsifying effect, the currently reported modification method is complex, the preparation process is complex, and the volume fraction of oil is generally controlled to be high in all the preparation of the Pickering emulsion gel, so that a certain application range is limited.
The attapulgite clay is a natural clay substance, has abundant reserves in the nature, and has biocompatibility and environmental friendliness. The Pickering emulsion gel prepared from the attapulgite clay has great application prospect and can be used in various fields such as cosmetics, medicines, papermaking, functional materials, foods and the like. Has a plurality of unique advantages: 1) The attapulgite clay has wide sources, rich resources, low cost and easy obtainment; 2) The attapulgite clay is natural clay, is taken from the nature, is a layered chain-like rod-shaped structure which has no pollution to the environment and no side effect on human bodies or other organisms, has higher specific surface area, has better emulsification effect and has stronger adsorption capacity. Therefore, the attapulgite clay particles have wide prospect for preparing Pickering emulsion gel, but the dosage of the attapulgite clay is very high, and the stable state cannot be achieved, and along with the increase of the content of the attapulgite, a large amount of particle agglomeration can occur, the total mass of the solid particles is increased, a large amount of attapulgite can fall off from an oil-water interface, the effect of stabilizing the emulsion cannot be achieved, and meanwhile, the material waste can be caused.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of Pickering emulsion gel based on modified attapulgite clay.
According to the preparation method, the attapulgite clay is modified to obtain modified attapulgite clay, the modified attapulgite clay has certain hydrophobicity, in the process of preparing Pickering emulsion gel, the modified attapulgite clay is dispersed in an aqueous phase, and after homogenization, the modified attapulgite clay is crosslinked into a net-shaped or cage-shaped structure in the aqueous phase, and oil drops are wrapped in the modified attapulgite clay to form stable oil-in-water Pickering emulsion gel. The formed emulsion gel has good stability even under the condition of less oil, stable gel structure and long-term stability, good temperature resistance and salt resistance effect, is easy to degrade, and can stabilize various oil phases (C9-C16 liquid straight-chain alkane, aromatic hydrocarbon, diesel oil, crude oil or edible oil); has wide application prospect in the fields of functional grease construction, daily necessities grease construction and the like.
In order to solve the problems, the invention is realized by the following technical scheme:
a preparation method of Pickering emulsion gel based on modified attapulgite clay comprises the following steps:
(1) Preparation of modified attapulgite clay
Mixing anhydride and attapulgite clay particles, dispersing in water, stirring to fully mix, freeze-drying the mixture, transferring the mixture into an oven for reaction, washing a sample obtained by the reaction with absolute ethyl alcohol, drying overnight, and grinding into powder to obtain modified attapulgite clay;
(2) Preparation of Pickering emulsion gel
Dispersing the modified attapulgite clay prepared in the step (1) in water to obtain a water phase, adding an oil phase into the water phase, and uniformly dispersing and emulsifying to obtain stable Pickering emulsion gel.
According to a preferred embodiment of the present invention, in step (1), the acid anhydride is octenyl succinic anhydride.
According to the preferred invention, in the step (1), the mass ratio of octenyl succinic anhydride to attapulgite clay particles is (1-2): (1-4).
Most preferably, in the step (1), the mass ratio of octenyl succinic anhydride to attapulgite clay particles is 2:1.
the weight ratio of octenyl succinic anhydride to attapulgite clay particles is too large, so that anhydride waste is caused, the ratio is too small, and the obtained modified attapulgite clay has poor or even no stabilizing effect on Pickering emulsion gel.
According to the present invention, preferably, in the step (1), the mass concentration of the attapulgite clay in water is 5 to 20wt%.
According to the present invention, in the step (1), the stirring is carried out by dispersing in a dispersing machine at a rotational speed of 8000 to 10000rpm for 1 to 5 minutes to thoroughly mix the materials.
According to a preferred embodiment of the present invention, in step (1), the freeze-drying temperature is from-55 to-65℃and the freeze-drying time is from 22 to 26 hours.
According to the invention, in step (1), the reaction temperature is 55-65℃and the reaction time is 2-6 hours.
According to a preferred embodiment of the invention, in step (1), the overnight drying temperature is 35-45 ℃.
According to the preferred embodiment of the present invention, in the step (1), the modified attapulgite clay obtained has a length of 1 to 3 μm and a diameter of 40 to 50nm.
According to the preferred embodiment of the present invention, in the step (2), the mass fraction of the modified attapulgite clay in the aqueous phase is 0.1 to 2%.
Most preferably, in the step (2), the mass fraction of the modified attapulgite clay in the aqueous phase is 1%.
According to a preferred embodiment of the invention, in step (2), the oil phase is selected from one of C9-C16 liquid linear alkanes, aromatic hydrocarbons, diesel, crude oil or edible oils.
Further preferably, the C9-C16 liquid linear alkane is n-tetradecane and the edible oil is soybean oil or palm oil.
According to a preferred embodiment of the invention, in step (2), the percentage of oil phase in the total volume is 15-75%.
According to the invention, in the step (2), the modified attapulgite clay accounts for 0.5-10.0% of the total mass of the oil phase and the water phase.
According to a preferred embodiment of the present invention, in step (2), the emulsification is carried out by placing the mixture in a disperser and homogenizing at 1000-10000 rpm for 1-2 minutes.
According to the invention, in the step (2), the stable Pickering emulsion gel has a suitable salinity of 0.1-3.0% and a pH of 5-9.
The invention is unexpectedly found in the experimental process, the mass fraction of the modified attapulgite clay in the water phase is controlled to be 0.1-2%, the sterilization effect of the disinfectant can be obviously improved, and the stability, the temperature resistance and the salt resistance of the emulsion gel are obviously improved.
The invention has the technical characteristics and advantages that:
1. according to the preparation method, the attapulgite clay is modified to obtain modified attapulgite clay, the modified attapulgite clay has certain hydrophobicity, in the process of preparing Pickering emulsion gel, the modified attapulgite clay is dispersed in an aqueous phase, and after homogenization, the modified attapulgite clay is crosslinked into a net-shaped or cage-shaped structure in the aqueous phase, and oil drops are wrapped in the modified attapulgite clay to form stable oil-in-water Pickering emulsion gel. The emulsion gel formed is stable even in the presence of a small amount of oil.
2. The Pickering emulsion gel provided by the invention has a stable gel structure and long-term stability, has good temperature resistance and salt resistance effects, is easy to degrade, and can stabilize various oil phases (C9-C16 liquid straight-chain alkane, aromatic hydrocarbon, diesel oil, crude oil or edible oil).
3. The Pickering emulsion gel disclosed by the invention is simple in preparation method, strong in feasibility, green and healthy in material use and has biocompatibility.
4. The Pickering emulsion gel prepared by the invention is a physical gel, does not change the chemical property of an oil phase, and has wide application prospects in the fields of construction of functional grease, daily necessities grease and the like.
5. The intermediate product modified attapulgite clay has strong emulsifying and dispersing properties, can emulsify oil into small oil drops, accelerates degradation and prevents formation of large-scale oil films, and has strong application value in the fields of treating oily wastewater and marine oil spills.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the modified attapulgite clay prepared in example 1;
FIG. 2 is a graph of contact angle of an oil-water-solid three-phase system of the modified attapulgite clay prepared in example 1;
FIG. 3 is an appearance and rheological analysis chart of Pickering emulsion gel prepared in example 1 after sealing and standing at room temperature for 24 hours; a is an appearance diagram after 24 hours, b is an inverted appearance diagram after 24 hours, c is a diagram of viscosity versus shear rate, and d is a graph of logarithm of viscous modulus and elastic modulus versus frequency;
FIG. 4 is an appearance and rheological analysis chart of Pickering emulsion gel prepared in example 2 after sealing and standing at room temperature for 24 hours; a is an appearance diagram after 24 hours, b is a diagram of viscosity change along with shear rate, and c is a logarithmic graph of viscosity modulus and elastic modulus versus frequency;
FIG. 5 is an appearance and rheological analysis chart of Pickering emulsion gel prepared in example 3 after sealing and standing at room temperature for 24 hours; a is an appearance diagram after 24 hours, b is a diagram of viscosity change along with shear rate, and c is a logarithmic graph of viscosity modulus and elastic modulus versus frequency;
FIG. 6 is an appearance and rheological analysis chart of Pickering emulsion gel prepared in example 4 after sealing and standing at room temperature for 24 hours; a is an appearance diagram after 24 hours, b is a diagram of viscosity change along with shear rate, and c is a logarithmic graph of viscosity modulus and elastic modulus versus frequency;
FIG. 7 is an appearance of Pickering emulsion gels prepared from OSA-PAL of different mass fractions after 24 hours of sealed placement at room temperature, a is an appearance after 24 hours, and b is an inverted appearance after 24 hours.
The specific embodiment is as follows:
for a better understanding of the present invention, reference will be made to the following description of specific embodiments and accompanying drawings.
Example 1
Preparation of modified attapulgite clay:
mixing octenyl succinic anhydride and attapulgite clay particles according to a mass ratio of 2:1, dispersing the obtained mixture in water, wherein the mass concentration of the attapulgite clay in the water is 10wt%, dispersing the mixture for 1 minute by using a dispersing machine at a rotating speed of 10000rpm to fully mix the octenyl succinic anhydride and the attapulgite clay, freeze-drying the uniformly mixed sample at-60 ℃ for 24 hours, transferring the sample into a 60 ℃ oven for reaction for 4 hours, finally washing the synthesized sample with absolute ethyl alcohol for 3 times, drying the sample at 40 ℃ overnight, and grinding the prepared sample into powder to obtain the modified attapulgite clay.
The SEM of the modified attapulgite clay prepared in example 1 is shown in fig. 1, and it can be seen from fig. 1 that the modified attapulgite clay has a length of 1-3 micrometers and a diameter of 40-50nm, and the modified attapulgite clay has good hydrophobicity, and the contact angle of an oil-water-solid three-phase system (water drops on the surface of the material in oil) of the prepared modified attapulgite clay is shown in fig. 2.
Example 2
The modified attapulgite clay according to example 1 was prepared as follows:
the mass concentration of the attapulgite clay in the water is 15wt%.
Example 3
Preparation of Pickering emulsion gel based on modified attapulgite clay:
dispersing the modified attapulgite clay particles prepared in example 1 in pure water as a water phase, wherein the mass fraction of the modified attapulgite clay particles in the water phase is 1.0wt%, adding an oil phase into the water phase, and controlling the volume fractions of the oil phase to be 15%, 25%, 40%, 50%, 60% and 75%, respectively; homogenizing the oil phase with tetradecane, pH of 7.0 and salinity of 0 with a homogenizer at 10000rpm for 2min, and standing for 24 hr to obtain Pickering emulsion gel with different oil volume fractions.
The appearance diagram and the rheological characteristic analysis diagram of Pickering emulsion gel prepared under different oil volume fractions after being placed for 24 hours at room temperature are shown in FIG. 3, and as can be seen from FIG. 3a and FIG. 3b, the emulsion gel provided by the invention has a stable gel structure and long-term stability, and is good in stability even under the condition of less oil. As can be seen from fig. 3c, 3d, the emulsion gel of the present invention is shear resistant.
Example 4
Preparation of Pickering emulsion gel based on modified attapulgite clay:
dispersing the modified attapulgite clay particles prepared in example 1 in pure water as a water phase, wherein the mass fraction of the modified attapulgite clay particles in the water phase is 1.0wt%, adding an oil phase into the water phase, and controlling the volume fractions of the oil phase to be 50% respectively; the oil phase is n-tetradecane, the pH is 5, 6, 7, 8 and 9, the salinity is 0, the oil-water mixture is homogenized for 2min by using a homogenizer at 10000rpm, and the mixture is stood for 24 hours, so that Pickering emulsion gel prepared at different pH values is obtained.
The appearance and rheological analysis of Pickering emulsion gels prepared at different pH values after being sealed and placed at room temperature for 24 hours are shown in FIG. 4, and it can be seen from FIG. 4a that the emulsion gel of the present invention has a stable gel structure and long-term stability at different pH values.
Example 5
Preparation of Pickering emulsion gel based on modified attapulgite clay:
dispersing the modified attapulgite clay particles prepared in example 1 in pure water as a water phase, wherein the mass fraction of the modified attapulgite clay particles in the water phase is 1.0wt%, adding an oil phase into the water phase, and controlling the volume fractions of the oil phase to be 50% respectively; the oil phase is n-tetradecane, the pH is 7, the salinity is 0, 0.5%, 1%, 2% and 3%, the oil-water mixture is homogenized for 2min by using a homogenizer at 10000rpm, and standing is carried out for 24 hours, so as to obtain Pickering emulsion gel prepared under different salinity.
The appearance diagram and the rheological characteristic analysis diagram of Pickering emulsion gel prepared under different salinity after being sealed and placed for 24 hours at room temperature are shown in FIG. 5, and the emulsion gel has good salt tolerance as can be seen from FIG. 5.
Example 6
Preparation of Pickering emulsion gel based on modified attapulgite clay:
dispersing the modified attapulgite clay particles prepared in example 1 in pure water as a water phase, wherein the mass fraction of the modified attapulgite clay particles in the water phase is 1.0wt%, adding an oil phase into the water phase, and controlling the volume fractions of the oil phase to be 50% respectively; the oil phases are n-tetradecane, toluene, diesel oil, crude oil, soybean oil and palm oil respectively, the pH value is 7, the salinity is 0, the oil-water mixture is homogenized for 2min by using a homogenizer at 10000rpm, and the mixture is stood for 24 hours, so that Pickering emulsion gels of different oil phases are obtained.
The appearance diagram and the rheological characteristic analysis diagram of Pickering emulsion gels of different oil phases after being placed for 24 hours at room temperature are shown in FIG. 6, and the fact that n-tetradecane, toluene, diesel oil, crude oil, soybean oil and palm oil are all oil phases has stable gel structures and long-term stability, and can stabilize various oil phases can be seen from FIG. 6.
Example 7
Preparation of Pickering emulsion gel based on modified attapulgite clay:
dispersing the modified attapulgite clay particles prepared in example 1 in pure water as a water phase, wherein the mass fractions of the modified attapulgite clay particles in the water phase are respectively 0.2wt%, 0.4wt%, 0.6wt%, 0.8wt% and 1wt%, adding an oil phase into the water phase, and controlling the volume fractions of the oil phase to be respectively 50%; homogenizing the oil phase with n-tetradecane, pH 7 and salinity 0 with a homogenizer at 10000rpm for 2min, and standing for 24 hr to obtain Pickering emulsion gel prepared from OSA-PAL with different mass fractions.
The appearance of Pickering emulsion gels prepared with OSA-PAL of different mass fractions after 24 hours of sealed standing at room temperature is shown in FIG. 7.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (9)
1. A preparation method of Pickering emulsion gel based on modified attapulgite clay comprises the following steps:
(1) Preparation of modified attapulgite clay
Mixing anhydride and attapulgite clay particles, dispersing in water, stirring to fully mix, freeze-drying the mixture, transferring the mixture into an oven for reaction, washing a sample obtained by the reaction with absolute ethyl alcohol, drying overnight, and grinding into powder to obtain modified attapulgite clay; the anhydride is octenyl succinic anhydride, and the mass ratio of octenyl succinic anhydride to attapulgite clay particles is (1-2): (1-4);
(2) Preparation of Pickering emulsion gel
Dispersing the modified attapulgite clay prepared in the step (1) in water to obtain a water phase, adding an oil phase into the water phase, and uniformly dispersing and emulsifying to obtain stable Pickering emulsion gel.
2. The preparation method according to claim 1, wherein in the step (1), the mass concentration of the attapulgite clay in water is 5-20wt%, and the stirring is carried out in a dispersing machine with a rotating speed of 8000-10000 rpm for 1-5min to fully mix the attapulgite clay.
3. The process according to claim 1, wherein in the step (1), the freeze-drying temperature is-55 to-65 ℃ and the freeze-drying time is 22 to 26 hours.
4. The process according to claim 1, wherein in step (1), the reaction temperature is 55 to 65 ℃, the reaction time is 2 to 6 hours, and the overnight baking temperature is 35 to 45 ℃.
5. The preparation method according to claim 1, wherein in the step (2), the mass fraction of the modified attapulgite clay in the aqueous phase is 0.1-2%.
6. The preparation method according to claim 1, wherein in the step (2), the mass fraction of the modified attapulgite clay in the aqueous phase is 1%.
7. The method according to claim 1, wherein in the step (2), the oil phase is one selected from the group consisting of C9-C16 liquid linear alkanes, aromatic hydrocarbons, diesel, crude oil and edible oil.
8. The preparation method of claim 1, wherein in the step (2), the oil phase accounts for 15-75% of the total volume, and the modified attapulgite clay accounts for 0.5% -10.0% of the total mass of the oil phase and the water phase.
9. The preparation method according to claim 1, wherein the emulsification is carried out by placing the mixture in a disperser and homogenizing at 1000-10000 rpm for 1-2 min; the applicable salinity of the stable Pickering emulsion gel is 0.1-3.0%, and the pH is 5-9.
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| CN115486494B (en) * | 2022-09-22 | 2023-09-19 | 中国科学院兰州化学物理研究所 | Method for constructing plant essential oil/dissociated attapulgite composite antibacterial product by taking emulsion as template |
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| CN108752603B (en) * | 2018-06-01 | 2020-06-19 | 华南理工大学 | Preparation method of starch-based Pickering emulsion gel |
| CN108641681A (en) * | 2018-06-19 | 2018-10-12 | 中国海洋大学 | A kind of preparation method of Attapulgite particle as oil-spill dispersant |
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