CN111631214A - Essential oil microcapsule, preparation method and application of essential oil microcapsule in humidifier - Google Patents
Essential oil microcapsule, preparation method and application of essential oil microcapsule in humidifier Download PDFInfo
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- CN111631214A CN111631214A CN202010638091.7A CN202010638091A CN111631214A CN 111631214 A CN111631214 A CN 111631214A CN 202010638091 A CN202010638091 A CN 202010638091A CN 111631214 A CN111631214 A CN 111631214A
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- essential oil
- limonene
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/18—Vapour or smoke emitting compositions with delayed or sustained release
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N27/00—Biocides, pest repellants or attractants, or plant growth regulators containing hydrocarbons
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/22—Lamiaceae or Labiatae [Mint family], e.g. thyme, rosemary, skullcap, selfheal, lavender, perilla, pennyroyal, peppermint or spearmint
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24F—AIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
- F24F3/00—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems
- F24F3/12—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling
- F24F3/14—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling by humidification; by dehumidification
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24F—AIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
- F24F3/00—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems
- F24F3/12—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling
- F24F3/16—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling by purification, e.g. by filtering; by sterilisation; by ozonisation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
Abstract
The invention provides an essential oil microcapsule, a preparation method and application thereof in a humidifier. The capsule wall isolates the contact between the capsule core and the outside, thereby effectively reducing the volatilization speed of the essential oil, further prolonging the effective time of the essential oil and reducing the replacement frequency of the essential oil microcapsules; meanwhile, the two essential oils are matched with each other, so that the bacteriostatic ability of the essential oil microcapsule is improved, and the effective bacteriostatic time of the essential oil microcapsule is prolonged to a certain extent.
Description
Technical Field
The invention relates to the technical field of microcapsules, in particular to an essential oil microcapsule, a preparation method and application thereof in a humidifier.
Background
Humidifiers are becoming more and more popular as small household appliances that increase the humidity of indoor air in a daily life. The humidifier enables the indoor relative humidity to be kept between 40% and 60% of the most comfortable degree by releasing a certain amount of water mist into the air, and the comfort degree and the health of the living and working environment of people are greatly improved. However, the water tank and other parts in the humidifier are in a wet state for a long time, and if the parts are not cleaned regularly, various bacteria are bred, so that the health of a human body is adversely affected.
At present, water body disinfection is mainly carried out by adding a bactericide into a water tank of a humidifier, however, the commonly used bactericide is an artificially synthesized chemical substance and has certain toxicity, the bactericide easily causes symptoms such as pneumonia, pulmonary fibrosis and the like of a human body after entering the human body along with atomized water vapor, and certain stimulation and harm can be caused to the human body while disinfecting, sterilizing and refreshing air.
Researches show that most of aromatic plant essential oil has good sterilization and disinfection characteristics, can refresh air, makes people happy and relieve pressure, and does not cause harm to human bodies. However, most of the natural plant essential oil has volatility and short effective time, and is required to be replaced frequently when being applied to a humidifier as a bactericide, so that the natural plant essential oil is inconvenient to use and increases the use cost.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the existing plant essential oil is short in effective time and needs to be replaced frequently, so that the essential oil microcapsule, the preparation method and the application of the essential oil microcapsule in a humidifier are provided.
To this end, the invention provides an essential oil microcapsule, which comprises a capsule wall and a capsule core filled in the capsule wall, wherein the capsule core comprises oregano essential oil and limonene.
Further, the mass of the oregano essential oil is 1-5 times of that of the limonene.
Further, the mass of the oregano essential oil is 1-1.5 times of that of the limonene.
Furthermore, the capsule core also comprises sodium alginate or chitosan, porous starch and an emulsifier.
Further, the ratio of the total mass of the sodium alginate or the chitosan and the porous starch to the total mass of the oregano essential oil and the limonene is 1: (1-2).
Further, the mass of the emulsifier is 0.5-1.5% of the total mass of the oregano essential oil and the limonene.
Further, the emulsifier is tween-80 or span-60.
Further, the mass ratio of the sodium alginate or the chitosan, the porous starch and the capsule wall is (1-2): (1-2): (1-2).
Further, the capsule wall is gelatin or chitosan.
Further, the capsule wall is made of gelatin, and the capsule core comprises sodium alginate, porous starch, an emulsifier, oregano essential oil and limonene.
Further, the total mass of the oregano essential oil and the limonene is 45-75% of the total mass of the essential oil microcapsule.
The invention also provides a preparation method of the essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution: dissolving sodium alginate or chitosan and porous starch in water to obtain the mixed solution;
(2) preparing a capsule core: adding oregano essential oil, limonene and an emulsifier into the mixed solution, sealing a reaction container, sequentially heating and homogenizing to form an oil-in-water emulsion, and curing the oil-in-water emulsion to obtain a capsule core;
(3) preparation of the capsule wall: and carrying out first washing on the capsule core, placing the capsule core in a solution containing a capsule wall material, and sequentially carrying out aging, cooling, suction filtration, second washing and drying to obtain the essential oil microcapsule.
Further, the step of curing the oil-in-water emulsion is:
adjusting the pH value of the oil-in-water emulsion to 2-5, and sequentially standing and filtering; or the like, or, alternatively,
adding the oil-in-water emulsion into 1-2 wt% calcium chloride aqueous solution, and sequentially standing and filtering.
The invention also provides application of the essential oil microcapsule in a humidifier.
Further, the essential oil microcapsules are attached to a filter screen of the humidifier.
Defining: the loading amount is the percentage of the total mass of the oregano essential oil and the limonene in the essential oil microcapsule.
The technical scheme of the invention has the following advantages:
1. the essential oil microcapsule provided by the invention comprises a capsule wall and a capsule core filled in the capsule wall, wherein the capsule core comprises oregano essential oil and limonene. The capsule wall isolates the contact between the capsule core and the outside, thereby effectively reducing the volatilization speed of the essential oil, further prolonging the effective time of the essential oil and reducing the replacement frequency of the essential oil microcapsules; meanwhile, the two essential oils are matched with each other, so that the bacteriostatic ability of the essential oil microcapsule is improved, and the effective bacteriostatic time of the essential oil microcapsule is prolonged to a certain extent.
2. The essential oil microcapsule provided by the invention has the advantages that the capsule wall is made of gelatin, and the capsule core comprises sodium alginate, porous starch, an emulsifier, oregano essential oil and limonene. The porous starch has rich micropores, so that the porous starch has good adsorption capacity and adsorption stability, is used for adsorbing oregano essential oil and limonene, and plays a role in storage and slow release; the sodium alginate or chitosan is used for forming a main body framework of the microcapsule, so that the microcapsule is prevented from swelling and soft collapse due to water absorption; the capsule wall is made of gelatin or chitosan and is coated outside the capsule core so as to protect the capsule core; the emulsifier reduces the interfacial tension of each component in the mixed system, prevents droplets from aggregating with each other and maintains the stability of the system.
3. According to the essential oil microcapsule provided by the invention, gelatin is used as a capsule wall, and due to the property that the gelatin is sticky and is soluble in hot water but not in cold water, when the essential oil microcapsule is used, the essential oil microcapsule is diluted by water and sprayed to the inner side of a filter screen of a humidifier, so that the essential oil microcapsule can be adhered to the filter screen; when the sterilizing capability of the filter screen is weak or disappears, the filter screen is washed by hot water, and after the filter screen is dried, the diluent is sprayed on the inner side of the filter screen of the humidifier again, so that the replacement of the essential oil microcapsules can be completed, the use and the replacement of the essential oil microcapsules are facilitated, and the reuse of the filter screen is guaranteed; meanwhile, the gelatin is not easy to lose in normal use, so that the use duration of the essential oil microcapsule is ensured, and the gelatin has good degradability and no pollution to the environment; in addition, the complex coacervate product is formed by the electrostatic interaction between the gelatin and the sodium alginate, and has better stability.
4. The preparation method of the essential oil microcapsule provided by the invention has the advantages that the capsule core is formed firstly, and then the capsule wall is formed on the outer side of the capsule core, so that the essential oil microcapsule with the microcapsule structure is obtained, and the preparation process is simple.
5. The essential oil microcapsule is attached to the filter screen of the humidifier, and the essential oil microcapsule is made of non-toxic materials such as oregano essential oil and limonene, so that the essential oil microcapsule can not affect human health while disinfecting a water body.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an electron microscope image of an essential oil microcapsule provided by an embodiment of the invention;
FIG. 2 is a sectional electron microscope image of the essential oil microcapsule provided by the embodiment of the invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
50g of sodium alginate and 50g of porous starch are dissolved in 500ml of water;
(2) preparing a capsule core:
(2a) adding 60g of oregano essential oil, 40g of limonene and 1.5g of tween-80 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 2% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 50g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) the solution was quenched and filtered in an ice-water bath, and after a second wash with deionized water, dried at 40 ℃ to obtain spherical essential oil microcapsules with a load of 49.8%.
Example 2
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of sodium alginate and 100g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 90g of oregano essential oil, 60g of limonene and 2.25g of span-60 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 2% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 50g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) the solution was quenched and filtered in an ice-water bath, and after a second wash with deionized water, dried at 40 ℃ to obtain spherical essential oil microcapsules with a loading of 63.5%.
Example 3
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 100g of sodium alginate and 50g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 90g of oregano essential oil, 60g of limonene and 2.25g of tween-80 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 2% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 50g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) and (3) placing the solution in an ice water bath for quenching and suction filtration, and drying at 40 ℃ after secondary washing by deionized water, thereby obtaining the spherical essential oil microcapsule with the loading capacity of 55.3%.
Example 4
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of sodium alginate and 100g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 250g of oregano essential oil, 50g of limonene and 4.5g of tween-80 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 2% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 50g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) and (3) placing the solution in an ice-water bath for quenching and suction filtration, and drying at 40 ℃ after secondary washing by deionized water, thereby obtaining the spherical essential oil microcapsule with the loading capacity of 70.4%.
Example 5
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of sodium alginate and 100g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 75g of oregano essential oil, 75g of limonene and 1.5g of span-60 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 1% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 50g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) and (3) placing the solution in an ice-water bath for quenching and suction filtration, and drying at 40 ℃ after secondary washing by deionized water, thereby obtaining the spherical essential oil microcapsule with the loading capacity of 66.8%.
Example 6
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of sodium alginate and 100g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 75g of oregano essential oil, 75g of limonene and 1.5g of tween-80 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 2% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 100g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) the solution was quenched and filtered in an ice-water bath, and after a second wash with deionized water, dried at 40 ℃ to obtain spherical essential oil microcapsules with a loading of 63.1%.
Example 7
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of chitosan and 50g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 60g of oregano essential oil, 40g of limonene and 1.5g of span-60 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; adjusting the pH value of the oil-in-water emulsion to 2, standing and crosslinking for 30min, and performing suction filtration to obtain capsule cores;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 50g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) the solution was quenched and filtered in an ice-water bath, and after a second wash with deionized water, dried at 40 ℃ to obtain spherical essential oil microcapsules with a load of 39.6%.
Example 8
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of chitosan and 100g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 90g of oregano essential oil, 60g of limonene and 0.75g of tween-80 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; adjusting the pH value of the oil-in-water emulsion to 5, standing and crosslinking for 30min, and performing suction filtration to obtain capsule cores;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core into a gelatin aqueous solution, wherein the gelatin aqueous solution comprises 50g of gelatin and 500ml of water, and mechanically stirring the capsule core at the speed of 150 r/min at the temperature of 60 ℃ for 60 min;
(3b) and (3) placing the solution in an ice-water bath for quenching and suction filtration, and drying at 40 ℃ after secondary washing by deionized water, thereby obtaining the spherical essential oil microcapsule with the loading capacity of 48.9%.
Example 9
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of sodium alginate and 100g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 75g of oregano essential oil, 75g of limonene and 1.5g of tween-80 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 2% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core in a chitosan solution, wherein the chitosan solution comprises 50g of chitosan, 1g of sodium hydroxide and 30ml of isopropanol solution, and mechanically stirring the solution at the temperature of 60 ℃ for 60min at the speed of 150 r/min;
(3b) the solution was quenched and filtered in an ice-water bath, and after a second wash with deionized water, dried at 40 ℃ to obtain spherical essential oil microcapsules with a loading of 63.8%.
Example 10
The embodiment provides a preparation method of an essential oil microcapsule, which comprises the following steps:
(1) preparing a mixed solution:
dissolving 50g of sodium alginate and 100g of porous starch in 500ml of water;
(2) preparing a capsule core:
(2a) adding 75g of oregano essential oil, 75g of limonene and 2.25g of span-60 into the mixed solution;
(2b) sealing the reaction container with sealing film or preservative film to prevent the essential oil from volatilizing, heating at 40 deg.C for 10min, and homogenizing at 10000 r/min for 5min to form oil-in-water emulsion; dropwise and slowly adding the oil-in-water emulsion into a calcium chloride aqueous solution with the mass concentration of 2% by using an injector, standing and crosslinking for 30min, and then carrying out suction filtration to obtain a capsule core;
(3) preparation of the capsule wall:
(3a) carrying out first washing on the capsule core by using deionized water, placing the capsule core in a chitosan solution, wherein the chitosan solution comprises 100g of chitosan, 2g of sodium hydroxide and 60ml of isopropanol solution, and mechanically stirring the capsule core at the temperature of 60 ℃ for 60min at the speed of 150 r/min;
(3b) the solution was quenched and filtered in an ice-water bath, and after a second wash with deionized water, dried at 40 ℃ to obtain 61.3% loading of spherical essential oil microcapsules.
Comparative example 1
This embodiment provides a bacteriostatic agent, which contains nipagin ester as a main ingredient.
Comparative example 2
This example provides an essential oil microcapsule which differs from the essential oil microcapsule provided in example 1 only in that: limonene in the essential oil microcapsules provided in example 1 was replaced with an equal mass of oregano essential oil.
Comparative example 3
This example provides an essential oil microcapsule, which is different from the essential oil microcapsule provided in example 1 in that: the oregano essential oil in the essential oil microcapsules provided in example 1 was replaced with equal mass of limonene.
Test example 1
The essential oil microcapsules prepared in examples 1 to 10 and comparative examples 1 to 3 were subjected to a zone of inhibition experiment to test the bacteriostatic ability and the effective time of the essential oil microcapsules, and the strains were staphylococcus aureus, bacillus subtilis and escherichia coli, respectively. The experimental method comprises the following steps: placing the essential oil microcapsules in a bacterial liquid, and measuring the sizes of the inhibition zones after 12h and 84 h. Wherein, when the diameter of the inhibition zone is more than 20mm, the bactericide has extremely high inhibition capacity; when the diameter range of the bacteriostatic circle is 15-20mm, the bactericide has higher bacteriostatic ability; when the diameter range of the bacteriostatic circle is 10-15mm, the bactericide has medium bacteriostatic ability; when the diameter range of the bacteriostatic circle is 7-9mm, the bactericide has lower bacteriostatic ability; when the diameter of the inhibition zone is less than 7mm, the bactericide is not sensitive to the strains. The test results are shown in table 1:
TABLE 1
As can be seen from table 1, compared with the conventional bacteriostatic agent, the bacteriostatic ability of the essential oil microcapsules prepared in examples 1 to 10 is greater than that of paraben against staphylococcus aureus, bacillus subtilis and escherichia coli; meanwhile, compared with the essential oil microcapsules provided by comparative examples 2-3, the essential oil microcapsules prepared in examples 1-10 have longer effective time and stronger bacteriostatic ability, which shows that the oregano essential oil and limonene have a synergistic effect; in addition, when the mass of the oregano essential oil is 1.5 times of that of the limonene, the bacteriostatic ability is stronger.
Test example 2
The essential oil microcapsules prepared in examples 1 to 10 and comparative examples 2 to 3 were placed in an environment with a humidity of 50 ± 5% and a temperature of 26 ℃ for 240 hours, and retention rate and release efficiency of the essential oil in the essential oil microcapsules were obtained, wherein the retention rate is the mass ratio of the essential oil after the test to the essential oil before the test to reflect the storage sustained-release effect of the product, and the release efficiency is (100% -retention rate) load/test duration to reflect the release efficiency of the product. The test results are shown in table 2:
TABLE 2
As can be seen from table 2, by comparing example 1 with example 2, the addition amount of the porous starch affects the loading amount of the essential oil microcapsules, and the porous starch has abundant micropores for adsorbing oregano essential oil and limonene, so the addition amount affects the loading amount of the essential oil microcapsules;
the comparison between the example 1 and the example 3 shows that the addition amount of the sodium alginate has an influence on the retention rate and the release efficiency of the essential oil microcapsule, the sodium alginate has certain compactness, so that the release efficiency and the retention rate of the essential oil microcapsule are influenced, and the release efficiency is reduced and the retention rate is increased along with the increase of the addition amount of the sodium alginate;
as is clear from comparison between example 5 and example 6, the addition amount of gelatin affects the retention rate and release efficiency of the essential oil microcapsules, and as the addition amount of sodium alginate increases, the release efficiency decreases and the retention rate increases.
Test example 3
The essential oil microcapsules prepared in examples 1 to 10 were diluted with water and sprayed on the inside of a filter screen of a humidifier so that the essential oil microcapsules inside the filter screen had a density of 80 to 120g/m2The method for measuring the wind resistance by using the filter screen resistance measuring device tests the wind resistance by measuring the pressure difference generated at two ends of the filter screen when the airflow is stable, and compares the shape, elasticity, viscosity and water absorbability of the essential oil microcapsule, and the result is shown in table 3:
TABLE 3
The comparison of examples 1-3 shows that the relative addition amount of the porous starch and the seaweed starch has an influence on the stress property of the essential oil microcapsules, and the stress property and elasticity of the essential oil microcapsules are increased along with the increase of the content of the porous starch;
it is clear from the comparison between example 5 and example 6 that the addition of gelatin can affect the viscosity of the essential oil microcapsules, thereby affecting the wind resistance of the essential oil microcapsules when used in a humidifier screen, with the greater the viscosity, the smaller the wind resistance.
Test example 4
The essential oil microcapsules prepared in example 1 were subjected to TEM testing. Fig. 1 is an electron microscope image of the essential oil microcapsules, and fig. 2 is a cross-sectional electron microscope image.
As can be seen from the figure, the essential oil microcapsule provided in example 1 includes a capsule wall using gelatin as a protective layer, the porous starch adsorbed with oregano essential oil and limonene is loaded in the main body framework composed of sodium alginate, and the porous starch and sodium alginate are located inside the capsule wall.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (14)
1. An essential oil microcapsule, which comprises a capsule wall and a capsule core filled inside the capsule wall, wherein the capsule core comprises oregano essential oil and limonene.
2. An essential oil microcapsule according to claim 1, characterized in that the mass of the oregano essential oil is 1-5 times the mass of the limonene.
3. An essential oil microcapsule according to claim 2, characterized in that the mass of oregano essential oil is 1-1.5 times the mass of the limonene.
4. An essential oil microcapsule according to any one of claims 1 to 3, wherein the core further comprises sodium alginate or chitosan and a porous starch and an emulsifier.
5. An essential oil microcapsule according to claim 4, wherein the ratio of the total mass of sodium alginate or chitosan and porous starch to the total mass of oregano essential oil and limonene is 1: (1-2).
6. An essential oil microcapsule according to claim 4 or 5, wherein the emulsifier is present in an amount of 0.5 to 1.5% by mass relative to the total mass of the oregano essential oil and limonene.
7. An essential oil microcapsule according to any one of claims 4 to 6, wherein the mass ratio of sodium alginate or chitosan, porous starch and capsule wall is (1-2): (1-2): (1-2).
8. An essential oil microcapsule according to any one of claims 1 to 7, wherein the wall is gelatin or chitosan.
9. An essential oil microcapsule according to claim 8, wherein the capsule wall is gelatin and the capsule core comprises sodium alginate, porous starch, an emulsifier, oregano essential oil and limonene.
10. Essential oil microcapsules according to any of claims 1-9, characterized in that the total mass of oregano essential oil and limonene is 45-75% of the total mass of the essential oil microcapsules.
11. The preparation method of the essential oil microcapsule is characterized by comprising the following steps:
(1) preparing a mixed solution: dissolving sodium alginate or chitosan and porous starch in water to obtain the mixed solution;
(2) preparing a capsule core: adding oregano essential oil, limonene and an emulsifier into the mixed solution, sealing a reaction container, sequentially heating and homogenizing to form an oil-in-water emulsion, and curing the oil-in-water emulsion to obtain a capsule core;
(3) preparation of the capsule wall: and carrying out first washing on the capsule core, placing the capsule core in a solution containing a capsule wall material, and sequentially carrying out aging, cooling, suction filtration, second washing and drying to obtain the essential oil microcapsule.
12. Process for the preparation of essential oil microcapsules according to claim 11, wherein the step of solidifying the oil-in-water emulsion is:
adjusting the pH value of the oil-in-water emulsion to 2-5, and sequentially standing and filtering; or the like, or, alternatively,
adding the oil-in-water emulsion into 1-2 wt% calcium chloride aqueous solution, and sequentially standing and filtering.
13. Use of essential oil microcapsules according to any one of claims 1 to 10 in a humidifier.
14. The use according to claim 13, wherein the essential oil microcapsules are attached to a screen of the humidifier.
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