CN103263877A - Preparation method of essential oil-contained silicon dioxide microcapsule - Google Patents
Preparation method of essential oil-contained silicon dioxide microcapsule Download PDFInfo
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Abstract
The invention discloses a preparation method of an essential oil-contained silicon dioxide microcapsule, which comprises the following steps: evenly mixing essential oil, a silicon dioxide precursor and co-emulsifier to obtain an oil phase mixed solution; adding acid into a silicon dioxide water dispersion solution until the pH value is regulated to 4.5-5.7, mixing with the oil phase mixed solution, and performing ultrasonic dispersion to obtain a fine emulsion; and performing closed reaction on the fine emulsion at 10-60 DEG C for 1-6 hours to obtain a colloid emulsion of the essential oil-contained silicon dioxide microcapsule. According to the invention, the liquid essential oil is contained in a hard shell of silicon dioxide; the preparation process is quick, convenient, clean and pollution-free; the essential oil-contained silicon dioxide microcapsule is small in particle size, high in structural strength and favorable in water-phase dispersibility; and the release performance adjustable range of the essential oil contained in the microcapsule is large. The preparation method disclosed by the invention is suitable for industrial large-scale production.
Description
Technical field
The present invention relates to the preparation field of microcapsules in the field of fine chemical, be specifically related to a kind of preparation method of microcapsules of silica parcel essential oil.
Background technology
Essential oil has skin to be nourished, pacifies agitation, improve effects such as sleeping, stimulate circulation, strengthen function immunity, when being used for the Aroma finishing of high-grade textiles such as silk when essential oil, can give fabrics such as underwear, pillow cover, nightwear, necktie with calm the nerves, health-care efficacies such as calm, hypnosis even physiotherapy.
But because most essential oils all are liquid oily matter at normal temperatures, and high volatility, easily oxidation in air.Thereby directly use natural essential oil to have many problems, be difficult to processing too by force as the essential oil flowability of liquid state and use; Liquid essential oil and water-compatible are poor, though under the emulsification of a large amount of emulsifying agents, stable dispersion in aqueous phase, but inconvenience further is attached to target matrix such as fabric, and the essential oil drop specific area after the emulsification enlarges markedly more volatile and oxidation deterioration.
By materials such as organic polymer, inorganic particle parcel essential oil drop, make essential oil microcapsules, then can improve the problems referred to above.Numerous advantages such as wherein have capsule size with the inorganic silicon dioxide for the microcapsules of wall material preparation and wall equipment structure controllability is strong, essential oil rate of release adjustable range is big, good biocompatibility, pollution are little.For example publication number is the preparation method that the Chinese invention patent application of CN101259399A discloses a kind of method for preparing inorganic nano microcapsule by one-step, comprise: emulsifying agent, pH conditioning agent are dissolved in the water, obtain the pH value and be 3～13 emulsifying agent and the mixed solution of pH conditioning agent; Monomer, small molecule hydrocarbon template compound and co-stabilizer are mixed, join in the mixed solution, disperse with ultrasonic wave, obtain stable miniemulsion; With miniemulsion adjustment to 30 ℃～80 ℃, react after 3 hours～5 days, obtain inorganic compound and be shell, small molecule hydrocarbon and be the inorganic nano microcapsule of nuclear.Above-mentioned product is core with the small molecule hydrocarbon, and the nanometer silicon dioxide particle that generates with silica presoma TEOS one one-step hydrolysis condensation is single shell material, and the sandwich construction of shell can guarantee the controlled exchange in microcapsules inner material and the external world.But all SiO in the inorganic microcapsules product that makes by above-mentioned one-step method
2Shell is produced by the TEOS hydrolytic condensation fully.Therefore, there is preparation time length, severe reaction conditions, structural strength shortcoming such as good inadequately in this method.
In the physics composite algorithm preparation of microcapsules, mainly use physisorption content fast, controllably is wrapped in the wall materials/substances.Wherein, pik woods emulsification effect (Pickering emulsification effect) is a kind of typical effect mechanism of using always.Thereby this effect refer to granule have all the time be adsorbed onto automatically large particle surface effectively reduce whole system total surface can trend.Though preparing microcapsules, application Pickering emulsification effect has advantages such as speed is fast, system is stable, but it is still a kind of physics compound action with dynamic adsorption equilibrium feature in essence, granule and be adsorbed the mutual cementation that shortage is enough between the large scale material, therefore, pik woods emulsification effect is subject to the change of external environment and lost efficacy.
Summary of the invention
The invention provides a kind of preparation method of microcapsules of silica parcel essential oil, liquid essential oil is wrapped in the hard shell of silica, preparation process is quick and convenient, the microcapsule granule size of silica parcel essential oil is little, structural strength is high, at the aqueous phase good dispersion, the release performance adjustable extent of essential oil that microcapsules wrap up is big.
A kind of preparation method of microcapsules of silica parcel essential oil may further comprise the steps:
(1) essential oil, silica presoma and assistant for emulsifying agent are mixed, obtain the oil phase mixed liquor;
(2) add acid for adjusting pH to 4.5～5.7 in the aqueous dispersions of silica, the oil phase mixed liquor with step (1) mixes again, obtains thin emulsion through ultrasonic dispersion;
(3) with the thin emulsion in the step (2) at 10 ℃～60 ℃ capping 1h～6h, obtain the colloid emulsion of the microcapsules of silica parcel essential oil.
The colloid emulsion of the microcapsules of silica parcel essential oil can obtain the microcapsules of silica parcel essential oil after breakdown of emulsion, suction filtration, drying.
The present invention makes up the inorganic hard shell fast in conjunction with Pickering physical absorption and original position interface generation technique, thereby realizes the small size microencapsulation parcel of liquid towards essential oil.The microcapsules of the silica parcel essential oil that obtains are the inorganic hard shell with the inorganic silicon dioxide, are core with the essential oil.Be the core template with essential oil sub-micro drop specifically, elder generation is the skeleton particle of inorganic shell with the silica granule that the Pickering effect is adsorbed in essential oil drop surface, again the SiO that is produced with oil-water interfaces place silica presoma hydrolysis-condensation reaction
2Material is the binding agent between above-mentioned skeleton particle.The SiO that silica dioxide granule and silica presoma hydrolysis-condensation reaction produce in the aqueous dispersions of final silica
2Formation has the inorganic shell of continuous hard of better compactness extent and structural strength, thus final effective parcel of realizing the essential oil drop.
In the step (1), described essential oil can be selected existing essential oil on the market as required for use, is preferably santal essential oil, olive essential oil, Rosemary Oil, Rosa Damascana or cinnamon essential oil.Above-mentioned essential oil odor type is stable, effect is obvious, lipophile is strong and be widely used, and is modal commercialization plants essential oil.
These essential oils can with the silica presoma with arbitrarily than miscible, thereby easily form the homogeneous mixture of essential oil and silica presoma, under the homeo-osmosis effect of assistant for emulsifying agent, after ultrasonic dispersion, be dispersed in uniformly and stably in the aqueous phase system that contains silica dioxide granule with sub-micro drop form, thereby form thin emulsion.
The silica presoma is used for the SiO in the generation of oil-water interfaces place hydrolysis-condensation reaction
2As the intergranular binding agent of framework silica, thereby form compactness extent and the good solid-state hard shell of silica of structural strength, as preferably, described silica presoma is ethyl orthosilicate (hereinafter to be referred as TEOS), and ethyl orthosilicate can produce SiO at oil-water interfaces place hydrolysis-condensation reaction
2, be conducive to obtain the better silica hard of compactness extent and structural strength shell.
Described assistant for emulsifying agent plays the effect of homeo-osmosis, and as preferably, described assistant for emulsifying agent is hexadecane, and is further preferred, and described assistant for emulsifying agent is isohexadecane (being called for short HD).
As preferably, the mass ratio of described silica presoma and essential oil is 3～60:100, an amount of silica presoma can be at oil-water interfaces generation hydrolysis, these newly-generated silica species can be tied a large amount of silica dioxide granules of Pickering physical absorption in the oil-water interfaces place, and this is conducive to form fast the silica hard shell of high compactness extent and high structural strength.
The use amount of described assistant for emulsifying agent can be selected a small amount of that those skilled in the art know for use, and as preferably, the mass ratio of described assistant for emulsifying agent and essential oil is 2.5～10:100, is conducive to form thin emulsion.
In the step (2), need to drip pH to 4.5～5.7 that the aqueous dispersions (being aqueous phase system) of silica is regulated in acid, this is for the static behaviour of regulating silica particles and intergranular active force.Because the equipotential point of nanometer silicon dioxide particle is about pH=2.5, system pH=4.5～5.7 o'clock silica particles will have an amount of negative electrical charge (this moment the particle surface Zeta potential be about-42～-27mv).The fainter electrostatic repulsion that is provided by these an amount of negative electrical charges can guarantee that silica dioxide granule has dispersion stabilization preferably at aqueous phase, simultaneously is unlikely to have a strong impact on after the thin emulsification treatment drop dense packing of silica sol granule at the interface again.Be lower than this scope as aqueous pH values, be in stronger sour environment, then not only silica particles Ztea current potential is low, a little less than the electrostatic repulsion, large-scale aggregating easily taking place between particle, and understand Essential Oil Chemistry composition in the destruction system before microcapsules are finished, influences the odor type of microcapsules.Be higher than this scope as aqueous pH values, system is in neutrality, and then silica particles is electrically strong, and repulsion force is big each other.Namely enable to be adsorbed in sub-micro essential oil drop surface, also can produce a large amount of spaces between silica dioxide granule, effective parcel that this both had been unfavorable for improving to essential oil also is unfavorable for improving the structural strength of microcapsules.Described acid can be adopted pure acid or aqueous acid, for the convenient pH that regulates, as preferably, selects aqueous acetic acid for use.This weak acid is few to ambient influnence, and removes by mode of heating easily.Under ultrasonic dispersion (being hyperacoustic powerful dispersion) effect; produce a large amount of submicron order essential oil drops and a large amount of oil-water interfaces; utilize the Pickering emulsification effect between bulky grain and granule simultaneously; to hang down electronegative silica dioxide granule and be adsorbed onto the big drop of oil phase surface efficiently and stably (for reducing the interface energy of whole system; silica dioxide granule can be adsorbed onto between oil-water interfaces automatically equably), form stable Pickering emulsion.
With the aqueous dispersions of acid for adjusting pH to 4.5～5.7 silica as water, itself just contains a certain amount of water in the aqueous dispersions of silica, the aqueous dispersions of silica is with after the oil phase mixed liquor of step (1) mixes, and can replenish as required to add a certain amount of water.The constant that the use total amount of water can adopt those skilled in the art to know, using total amount as water content in the aqueous dispersions of silica and replenishing of water adds water the content sum, as preferably, in the step (2), the total amount of water and the mass ratio of essential oil are 300～1800:100.
As preferably, the particle diameter of silica dioxide granule is 5～30nm in the aqueous dispersions of described silica, because the power of silica dioxide granule absorption is the Pickering emulsification effect between big drop and the granule, therefore the silica dioxide granule particle diameter that uses must satisfy certain size, just can efficiently be adsorbed onto the oil phase drop surface that ultrasonic homogeneous changes into fast, reach the effect of stable emulsion, realize the preliminary adjusting to shell thickness simultaneously.Excessive silica sol granule (〉 30nm) and the adsorption between drop a little less than, easily cause silica sol granule free at continuous aqueous phase; And too small silica dioxide granule (＜5nm), then can't guarantee capsule shell structural strength and compactness preferably.Further preferred, the particle diameter of silica dioxide granule is 5～15nm in the aqueous dispersions of described silica, the silica dioxide granule of above-mentioned size can efficiently be adsorbed onto the oil phase drop surface that ultrasonic homogeneous changes into fast, reach the effect of stable emulsion, and behind capping, form the silica hard shell that structural strength is good and compactness is good.
As preferably, the mass ratio of silica dioxide granule and essential oil is 10～100:100 in the aqueous dispersions of described silica, and the silica dioxide granule consumption directly influences the stability of Pickering emulsion., oil phase drop size very few as the silica dioxide granule amount is big and surface absorption is insufficient, then is difficult for forming stable Pickering emulsion system.And cross under the silica dioxide granule of volume, water free silicon dioxide particle increases, and the particle adsorption efficiency reduces.Simultaneously, the wall material thickens, and the silica binder that silica presoma hydrolytic condensation produces is insufficient to the bonding of silica dioxide granule, can cause the reduction of microcapsules cyst wall structural strength.
As preferably, the condition of described ultrasonic dispersion: ultrasonic power 40W～200W, ultrasonic 3s～7s, the a large amount of heats of the interval ultrasonic generation of 3s～7s(, and then can cause system temperature to raise fast, in the ultrasonic procedure, stopping ultrasonic at interval is to have more opportunity outwards to dispel the heat for ease of system, for example to the water-bath release heat), effectively ultrasonic time is 300s～700s.Namely at ultrasonic power 40W～200W ultrasonic 3s～7s earlier, 3s～7s at interval then, ultrasonic 3s～7s again, 3s～7s at interval replaces successively again, and batch (-type) is ultrasonic, and ultrasonic temporal summation is effective ultrasonic time, is 300s～700s.By the regulation system intensity that homogenizes, can effectively control the particle diameter of essential oil microcapsules.Generally, ultrasonic power is more high, ultrasonic time is more long, and the made product particle diameter of mini-emulsion polymerization is more little.Experiment is found under above-mentioned ultrasonic dispersion condition, the microcapsules average grain diameter of made silica parcel essential oil is generally at 180nm～410nm, particle diameter profile exponent Span value (Span=(D90-D10)/D50, wherein D90, D10 and D50 represent to be equivalent to by the mass accumulation that the little side of particle diameter begins 90%, 10% and 50% o'clock corresponding particle size of gross weight respectively)≤1.Particle diameter is distributed in this state following time, and the microcapsules size of silica parcel essential oil more homogeneous, system is more stable.Further preferred, the condition of described ultrasonic dispersion: ultrasonic power 40W～200W, ultrasonic 5s, interval 5s, effectively ultrasonic time is 500s.
Described ultrasonic dispersion is preferably carried out in ice-water bath, and a large amount of heats of ultrasonic generation are conducive to the water-bath release heat.
As preferably, in the thin emulsion after ultrasonic dispersion, add emulsifying agent, can improve the stability of thin emulsion.Further preferred, described emulsifying agent is softex kw (hereinafter to be referred as CTAB), softex kw (CTAB) is a kind of cationic surfactant, has certain emulsification, can improve the stability of emulsification system.The more important thing is this cationic surface active agent positively charged that is present in the oil-water interfaces place, with the silica dioxide granule of electronegative property in the system electrostatic adsorption is preferably arranged, thereby be conducive to the dense packing of oil-water interfaces silica dioxide granule, add emulsifying agent thin emulsion afterwards and carry out capping, also be conducive to the hydrolysis of silica presoma and generate silica dioxide granule in the enrichment of oil-water interfaces and to the bonding of silica dioxide granule, thereby be conducive to form the silica hard shell that structural strength is good and compactness is good.
The use amount of described emulsifying agent can be selected a small amount of that those skilled in the art know for use, and as preferably, the mass ratio of described emulsifying agent and essential oil is 0.75～3:100, and the emulsifying agent of above-mentioned use amount just can improve the stability of emulsification system well.
In the step (3), as preferably, thin emulsion is at 30 ℃～50 ℃ capping 2h～4h, and along with the rising of system temperature, silica presoma hydrolysis meeting is sharply accelerated.Thereby too high reaction temperature is unfavorable for that newly-generated silica is to the bonding of silica dioxide granule in the aqueous dispersions of silica.In addition, the essential oil volatilization strengthens under the higher temperature, and is also more perishable, the assurance of unfavorable aromatic micro-capsule quality.But reaction temperature is spent low, and hydrolysis reaction can be slower, unfavorable production.Take into account reaction efficiency and essential oil quality, the temperature of described capping is 30 ℃～50 ℃.Experiment finds that under the reaction condition of nitrogen protection deoxygenation, react after 2h～4h hour, silica presoma conversion ratio is substantially more than 90%.And reaction rate is moderate, and course of reaction is stable, and end product essential oil smell is pure.
In the step (3), as preferably, described capping is 200～300rmin in stir speed (S.S.)
-1Under carry out because the hydrolysis of silica presoma is slower, and reacting environment is at oil-water interfaces.Therefore, extraneous disturbance is moderate, and excessive disturbance meeting makes the oil-water interfaces instability influences the absorption of nano silicon, causes Pickering emulsion instability.In addition, excessive disturbance also can influence the morphosis of microcapsules, makes the sphericity of microcapsules and the perfect degree variation of parcel essential oil, and disturbs silica SiO that presoma generates
2Cementation to silica dioxide granule.If but the disturbance undermixing, the water insufficient flow on oil phase drop surface causes microcapsules suspension deficiency in the system easily, and then influences the stability of reaction system.
From characterization data, the effect of embodiment 5 and embodiment 10 is best, essential oil coating efficiency height, release performance is good, therefore, and can be further preferred, first optimized technical scheme, in the step (1), the mass ratio of described silica presoma and essential oil is 25:100, and the mass ratio of described assistant for emulsifying agent and essential oil is 5:100.In the step (2), the mass ratio of silica dioxide granule and essential oil is 50:100 in the aqueous dispersions of described silica, and the mass ratio of described emulsifying agent and essential oil is 1.5:100.Wherein, the mass ratio of silica dioxide granule and essential oil is the significant effects factor in the mass ratio of silica presoma and essential oil and the aqueous dispersions of silica, the microcapsules of made silica parcel essential oil, essential oil coating efficiency height, particle size is little, structure is strong, good dispersion, and the sustained release performance of the microcapsules of silica parcel essential oil is good.
Among the present invention, described stirring, ultrasonic dispersion etc. are the typical unit operation in the chemical process, purpose be make mixing of materials evenly, be uniformly dispersed, and make sample segment produce the oiliness droplet with specific modality structure, can adopt the existing conventional device to realize.
Compared with prior art, the present invention has following beneficial effect:
One, the preparation method of the microcapsules of silica parcel essential oil of the present invention, in conjunction with Pickering physical absorption and two kinds of microcapsule preparation methods of original position interfacial polymerization, wherein Pickering physical absorption silica constitutes the skeleton of shell, and the silica that the original position interfacial polymerization generates is as the binding agent between above-mentioned skeleton particle.Can rapidly high volatility, perishable liquid essential oil be coated in the silica wall material of porous hard thereby, and then " curing of small size powdery " of realization liquid towards essential oil.Quick and convenient, the cleanliness without any pollution of above-mentioned preparation process, the particle size of the microcapsules of made silica parcel essential oil is little, structure strong, good dispersion, and the release performance adjustable extent of the microcapsules of silica parcel essential oil is big.
Two, the present invention is by content, particle diameter and the silica presoma consumption of control silica dioxide granule, comes the wall material thickness size on the wall material and wall material crosslinking compactness extent are controlled and strengthened.This not only can effectively improve the external stressed opposing of microcapsules, prevents caving in and molten problem of essential oil microcapsules, guarantees that microcapsules have nucleocapsid structure preferably.And what is more important, the adjustability of wall material thickness, compactness extent is big, can give the wider volatilization of microcapsules and discharge adjustability.
Three, the made product of preparation method of the present invention is the polymolecularity latex that blue light is arranged, essential oil microcapsules structural strength height wherein, in water and polar organic matter dispersiveness all better, can tolerate a large amount of abominable chemical environments such as strong acid and strong base.Can make uniform and stable white powder through simple breakdown of emulsion, suction filtration, drying under the normal temperature, can be applied to fields such as weaving, building, furniture as additive and filler easily.
Four, preparation method of the present invention is raw materials used is easy to get, technology is simple, the controllability of microcapsules morphosis is good, do not relate to organic solvent, problems such as the solvent-free pollution of process can avoid existing silica presoma (TEOS) one-step method to generate problems such as shell rise time length, uneven thickness, release poor controllability in the shell method.Preparation method of the present invention is suitable for large-scale industrialization production.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) photo that the silica of embodiment 5 preparations wraps up the microcapsules of essential oil;
Fig. 2 is transmission electron microscope (TEM) photo that the silica of embodiment 1 preparation wraps up the microcapsules of essential oil;
Fig. 3 is that the colloid emulsion of microcapsules of silica parcel essential oil of embodiment 5 preparation is through ESEM (SEM) photo of breakdown of emulsion, suction filtration, dry gained white powder.
The specific embodiment
Embodiment 1～15
(1) (isohexadecane HD) mixes, and obtains the oil phase mixed liquor with essential oil, silica presoma TEOS and 0.5g assistant for emulsifying agent;
(2) in the aqueous dispersions of silica, add aqueous acetic acid adjusting pH to 4.5～5.7, embodiment 1 regulates pH to 4.5, embodiment 11 regulates pH to 5.7, other embodiment all regulate pH to 5, oil phase mixed liquor with step (1) mixes again, add an amount of water, make mixed total amount be adjusted to 100g, put into ice-water bath then, through ultrasonic dispersion (ultrasonic 5s, interval 5s, effectively ultrasonic time is 500s) obtain thin emulsion, in the thin emulsion after ultrasonic dispersion, add 0.15g emulsifying agent softex kw (CTAB);
(3) the thin emulsion that will add behind the emulsifying agent is 200～300rmin in stir speed (S.S.)
-1Down, at 10 ℃～60 ℃ capping 1h～6h, the silica that obtains polymolecularity wraps up the colloid emulsion of the microcapsules of essential oil.
The colloid emulsion of microcapsules that obtains the silica parcel essential oil of polymolecularity is the polymolecularity latex that blue light is arranged, and can make uniform and stable white powder through simple breakdown of emulsion, suction filtration, drying.
Other parameter conditions of embodiment 1～13 are as shown in table 1.
Table 1
The characterizing method explanation that relates among the embodiment 1～15:
Measure the granularity of microcapsule granule by the laser particle analyzer LB-550 of company (Japanese Holiba), obtain its average grain diameter value and particle diameter profile exponent Span value.
Observe the morphosis of microcapsule granule in the hanging drop sample by transmission electron microscope (the Japanese JEOL JSM-1200EX T20 of company).
Observe the morphosis of essential oil microcapsules powder by awkward silence at a meeting emission scan Electronic Speculum (FE-SEM) transmission electron microscope (the German Zeiss ULTRA55 of company).
Analyze in the microcapsules by the content of parcel essential oil by thermogravimetic analysis (TGA) (the Pyris1 type thermogravimetric analyzer of U.S. PE company).Concrete test process is: the colloid emulsion of microcapsules that silica is wrapped up essential oil through simple breakdown of emulsion, suction filtration, dry and can make white powder, be rapidly heated to 180 ℃, and under this constant temperature, measure its weight-loss curve.Etc. recording wherein weightless part---the proportion of essential oil in microscapsule powder after the constant weight, be designated as X%.
Be calculated as follows the parcel efficient of essential oil in the essential oil microcapsules:
Weightless percentage when the X:TGA curve reaches constant weight
M
Ludox: add the silica sol granule quality in the 100 gram systems
In last two formulas, M
TEOS: add the TEOS quality in the 100 gram systems
M
Essential oil: add the essential oil quality in the 100 gram systems
In addition, with half the required time of volatilizing of essential oil in the microcapsules be index, estimate the release performance of essential oil in the microcapsules.
Transmission electron microscope (TEM) photo of the colloid emulsion of the microcapsules of the silica parcel essential oil of embodiment 5 preparations, as shown in Figure 1, can obviously see the microcapsules that present hollow structure, the size of microcapsules between 270～410nm, the hard shell that the surface is made up of silica.
Transmission electron microscope (TEM) photo of the colloid emulsion of the microcapsules of the silica parcel essential oil of embodiment 1 preparation as shown in Figure 2, can be found the microcapsules of the solid or little liquid nuclear of a greater number, and this is because embodiment 1 essential oil content is low, and the oil phase ratio is low to be caused.
The colloid emulsion of the microcapsules of the silica parcel essential oil of embodiment 5 preparations is through ESEM (SEM) photo of breakdown of emulsion, suction filtration, dry gained white powder, as shown in Figure 3, can see the hollow microcapsule that breaks in a large number clearly, illustrate that oil phase is coated on microcapsules inside preferably.Simultaneously, Fig. 3 microcapsules cyst wall that breaks has demonstrated the compactness of shell and the characteristics of " hard " well.
Embodiment 1～15 measured result is as shown in table 2.
Table 2
The measured result of table 2 and characterize as can be known in conjunction with collection of illustrative plates, the microcapsules of the silica parcel essential oil of embodiment 1～15 preparation, can well liquid essential oil be wrapped in the hard shell of silica, the microcapsule granule size of silica parcel essential oil is little, structural strength is high, at the aqueous phase good dispersion, the release performance adjustable extent of essential oil that microcapsules wrap up is big.Wherein, the microcapsules of the silica parcel essential oil of embodiment 5 and embodiment 10 preparations, characterize as can be known from the measured result of table 2 and in conjunction with collection of illustrative plates, its tactical rule, the microcapsules homogeneity is good, and is dispersed at aqueous phase, essential oil coating efficiency height, release performance is good, and embodiment 5 and embodiment 10 are optimum embodiment.
Claims (10)
1. the preparation method of the microcapsules of a silica parcel essential oil is characterized in that, may further comprise the steps:
(1) essential oil, silica presoma and assistant for emulsifying agent are mixed, obtain the oil phase mixed liquor;
(2) add acid for adjusting pH to 4.5～5.7 in the aqueous dispersions of silica, the oil phase mixed liquor with step (1) mixes again, obtains thin emulsion through ultrasonic dispersion;
(3) with the thin emulsion in the step (2) at 10 ℃～60 ℃ capping 1h～6h, obtain the colloid emulsion of the microcapsules of silica parcel essential oil.
2. the preparation method of the microcapsules of silica parcel essential oil according to claim 1 is characterized in that in the step (1), described essential oil is santal essential oil, olive essential oil, Rosemary Oil, Rosa Damascana or cinnamon essential oil;
Described silica presoma is ethyl orthosilicate;
Described assistant for emulsifying agent is hexadecane.
3. the preparation method of the microcapsules of silica parcel essential oil according to claim 1 is characterized in that in the step (2), the particle diameter of silica dioxide granule is 5～30nm in the aqueous dispersions of described silica.
4. the preparation method of the microcapsules of silica parcel essential oil according to claim 1 is characterized in that in the step (1), the mass ratio of described silica presoma and essential oil is 3～60:100;
In the step (2), the mass ratio of silica dioxide granule and essential oil is 10～100:100 in the aqueous dispersions of described silica.
5. the preparation method of the microcapsules of silica parcel essential oil according to claim 4 is characterized in that in the step (1), the mass ratio of described silica presoma and essential oil is 25:100;
In the step (2), the mass ratio of silica dioxide granule and essential oil is 50:100 in the aqueous dispersions of described silica.
6. the preparation method of the microcapsules of silica parcel essential oil according to claim 1 is characterized in that, in the step (2), the condition of described ultrasonic dispersion: ultrasonic power 40W～200W, ultrasonic 3s～7s, interval 3s～7s, effectively ultrasonic time is 300s～700s.
7. the preparation method of the microcapsules of silica parcel essential oil according to claim 1 is characterized in that, in the step (2), adds emulsifying agent in the thin emulsion after ultrasonic dispersion.
8. the preparation method of the microcapsules of silica parcel essential oil according to claim 7 is characterized in that described emulsifying agent is softex kw.
9. the preparation method of the microcapsules of silica parcel essential oil according to claim 1 is characterized in that, in the step (3), thin emulsion is at 30 ℃～50 ℃ capping 2h～4h.
10. the preparation method of the microcapsules of silica parcel essential oil according to claim 1 is characterized in that in the step (3), described capping is 200～300rmin in stir speed (S.S.)
-1Under carry out.
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