CN114470288B - Fragrance with relieving effect and preparation method thereof - Google Patents

Fragrance with relieving effect and preparation method thereof Download PDF

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CN114470288B
CN114470288B CN202210245746.3A CN202210245746A CN114470288B CN 114470288 B CN114470288 B CN 114470288B CN 202210245746 A CN202210245746 A CN 202210245746A CN 114470288 B CN114470288 B CN 114470288B
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essential oil
montmorillonite
fragrance
soothing
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CN114470288A (en
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石锋
张照荣
李远兵
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Zhejiang Songchaozhenxuan Technology Co ltd
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00—Disinfection, sterilisation or deodorisation of air
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00—Disinfection, sterilisation or deodorisation of air
    • A61L9/01—Deodorant compositions
    • A61L9/013—Deodorant compositions containing animal or plant extracts, or vegetable material
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2209/00—Aspects relating to disinfection, sterilisation or deodorisation of air
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    • A61L2209/21—Use of chemical compounds for treating air or the like
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2209/00—Aspects relating to disinfection, sterilisation or deodorisation of air
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    • A61L2209/22—Treatment by sorption, e.g. absorption, adsorption, chemisorption, scrubbing, wet cleaning
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention discloses a fragrance with a relieving effect and a preparation method thereof. According to the invention, natural plant essential oil is diffused under vacuum to form saturated steam, and then modified montmorillonite is utilized to adsorb, so that adverse effects of solvents on specific sensitive people are eliminated, and the application range of the fragrance with a relieving effect is widened.

Description

Fragrance with relieving effect and preparation method thereof
Technical Field
The invention relates to the technical field of daily chemical industry, in particular to a fragrance with a relieving effect and a preparation method thereof.
Background
The natural plant essential oil has volatility, can be dispersed in the air through molecular diffusion, and creates a pleasant and comfortable atmosphere; however, the aromatic nature and instability of natural plant essential oils limit their use as fragrances. The preparation of liquid fragrance by mixing natural plant essential oils with organic solvents is a common technical solution; the traditional liquid fragrance has a smaller contact surface with air and a slower volatilization rate, and the fragrance formed by the technical improvement generally combines the liquid fragrance with a medium with a larger specific surface area, and the liquid fragrance enters the medium by capillary action and volatilizes out of the contact surface with air in the use process so as to achieve the purpose of enhancing the volatilization rate. Compared with natural plant essential oil, common solvents such as ethanol, isododecane, isohexadecane and the like do not have the effect of relaxing and soothing; in addition, the solvent volatilizes into the air, and adverse reactions can be generated by partial people or pets with more sensitive physique. In the process of fragrance emission, the diffusion rate of essential oil molecules is usually faster at the beginning, and gradually decreases along with the lapse of time, so that the phenomenon that fragrance smell is over-concentrated at the beginning and the smell is gradually diluted along with the lapse of time is generated, and the sensory experience of a user is affected.
Patent CN 111035787A discloses a fragrance and a preparation method and application thereof, the invention prepares a high-viscosity fragrance, the high-viscosity fragrance has higher viscosity and slower fluidity, can effectively avoid the leakage phenomenon of contents, can improve the production and use of products, is particularly suitable for being used as an air freshener in places such as indoor small spaces, automobiles and the like, and keeps good fragrance divergence. The patent CN 112274685A provides a space fragrance essential oil and a preparation method thereof, and the natural compound essential oil is used, so that the space fragrance essential oil has the advantages of natural environment protection, various and harmonious olfactory experiences and low sensitization rate. However, the above patents all use solvent to aid dissolution in the preparation process of the perfume, and may cause adverse effects on part of the population along with diffusion in practical use.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problems to be solved by the present invention are: (1) Providing a fragrance with a soothing effect, wherein the fragrance has good volatility and durability; (2) Solves the technical problem that the natural plant essential oil is effectively combined with the carrier montmorillonite without using an organic solvent in the preparation process of the perfume; (3) Solves the technical problem of low load of montmorillonite to natural plant essential oil.
Montmorillonite is an inorganic material with high cation exchange capacity, good expansion capacity and high specific surface area, and has potential use value as a natural plant essential oil carrier in fragrance. Adsorption of natural plant essential oils on inorganic materials often requires the use of organic solvents to aid in dissolution, but residues of organic solvents on the materials often have adverse effects. In order to eliminate the adverse effect of the solvent, prepare a fragrance with good volatility and durability and relieving effect, the inventor tries to mix natural plant essential oil and montmorillonite to load the essential oil on the montmorillonite; however, the combination of the essential oil and the montmorillonite in the loading mode is easy to form a slurry mixture, and the slurry mixture is accompanied by the agglomeration and aggregation of the montmorillonite, so that the aim is difficult to achieve. The inventor optimizes the loading process, diffuses natural plant essential oil under vacuum condition to form saturated steam, and further uses montmorillonite to adsorb gaseous essential oil, thereby preparing the fragrance with relieving effect.
A preparation method of a fragrance with relieving effect comprises the following steps: sodium-exchanged montmorillonite is treated by octyl trimethyl ammonium chloride to increase the interlayer spacing of the sodium-exchanged montmorillonite, so as to obtain modified montmorillonite; the preparation method comprises the steps of preparing compound type relieving essential oil by using lavender essential oil, rose essential oil, chamomile essential oil and lemon balm essential oil, wherein the compound type relieving essential oil is diffused under a vacuum condition to form saturated steam; the modified montmorillonite is used for absorbing saturated steam of the compound type soothing essential oil under the vacuum condition to prepare the fragrance.
Preferably, a method for preparing a fragrance with soothing effect comprises the following steps:
(1) Dispersing bentonite in water to form uniform bentonite mixed solution; centrifuging the bentonite mixed solution after acid treatment, oxidation treatment and particle exchange treatment, and taking out the lower-layer sediment, washing, drying and crushing to obtain sodium-exchanged montmorillonite;
(2) Dispersing the sodium-exchanged montmorillonite in water to form uniform montmorillonite mixed solution; adding octyl trimethyl ammonium chloride into the montmorillonite mixed solution and reacting; centrifuging after the reaction is finished, taking the lower layer precipitate, washing with water, drying and crushing to obtain modified montmorillonite;
(3) Mixing lavender essential oil, rose essential oil, chamomile essential oil and lemon balm essential oil to form composite type relieving essential oil; placing the compound soothing essential oil in a vacuum environment, and forming saturated steam through diffusion; and then the modified montmorillonite is used for adsorbing saturated steam to obtain the fragrance with the relieving effect.
In order to increase the adsorption capacity of montmorillonite to essential oil and increase the volatilization rate of the essential oil, the inventor firstly carries out sodium exchange treatment on the montmorillonite, and the obtained sodium exchange montmorillonite has strong electrostatic interaction on the surface, thereby being beneficial to adsorption of montmorillonite and essential oil molecules; in addition, hydroxyl groups exist on the surface of the sodium-exchanged montmorillonite, so that hydrogen bonds can be formed between the sodium-exchanged montmorillonite and essential oil, and adsorbed essential oil is reserved in the montmorillonite.
The adsorption of sodium-exchanged montmorillonite and gaseous essential oil is affected by the surface area. The sodium-exchanged montmorillonite has a multi-layer crystal structure, and in order to increase the adsorption area of the sodium-exchanged montmorillonite, the inventor uses octyl trimethyl ammonium chloride to treat the sodium-exchanged montmorillonite so as to increase the crystal layer spacing; under the strong electrostatic interaction of the sodium exchange montmorillonite surface, octyl trimethyl ammonium chloride enters between crystal layers, and the space between the crystal layers is increased through the steric hindrance formed by long carbon chains, so that favorable conditions are created for the montmorillonite to adsorb essential oil molecules.
Further preferred is a process for the preparation of a fragrance having a soothing effect comprising the steps of, in parts by weight:
(1) Dispersing 5-9 parts of bentonite in 30-54 parts of water, mixing the bentonite and the water sequentially through mechanical stirring and ultrasonic treatment, and dispersing to form uniform bentonite mixed solution; adding 0.5-2 parts of hydrochloric acid into the bentonite mixed solution, and treating for 0.5-2 hours; continuously adding 4-8 parts of hydrogen peroxide aqueous solution, and treating for 0.5-2 hours; finally adding 6-12 parts of sodium chloride aqueous solution, treating for 0.5-1 h, centrifuging, taking out the lower layer precipitate, washing, drying and crushing to obtain sodium-exchanged montmorillonite;
(2) Re-dispersing the sodium-exchanged montmorillonite in 15-36 parts of water, and sequentially mixing and dispersing the sodium-exchanged montmorillonite and the water through mechanical stirring and ultrasonic treatment to form uniform montmorillonite mixed solution; adding 0.45-1.35 parts of octyl trimethyl ammonium chloride into the montmorillonite mixed solution for reaction; centrifuging the montmorillonite mixed solution after the reaction is finished, taking the lower layer precipitate, washing with water, drying and crushing to obtain modified montmorillonite;
(3) Taking 3-6 parts of lavender essential oil, 0.5-2 parts of rose essential oil, 0.6-3 parts of chamomile essential oil and 1.2-3 parts of lemon balm essential oil, and mixing the essential oils to form composite relieving essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 2-4 h in the vacuum container; and then placing the modified montmorillonite in a vacuum container for standing for 12-48 hours for adsorption to obtain the modified montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
Preferably, the parameters and steps of the mechanical stirring in the steps (1) and (2) are respectively independent: mixing at stirring speed of 300-600 rpm for 0.5-2 hr.
Preferably, the parameters and steps of the ultrasonic treatment in the steps (1) and (2) are respectively independent: the ultrasonic power is 550-850W, the ultrasonic frequency is 28-40 kHz, and the ultrasonic treatment is 15-60 min.
Preferably, the concentration of the hydrochloric acid in the step (1) is 1-2 mol/L.
Preferably, the concentration of the aqueous hydrogen peroxide solution in the step (1) is 1 to 3mol/L.
Preferably, the concentration of the aqueous sodium chloride solution in the step (1) is 0.5 to 1mol/L.
Preferably, the reaction in step (2) is carried out at a temperature of 60 to 75℃for a period of 0.5 to 1 hour.
Preferably, the internal temperature of the vacuum vessel in the step (3) is 35 to 40 ℃.
Preferably, in the step (3), the corresponding relationship between the mass of the compound type relief essential oil and the volume of the vacuum container is: every 1kg of compound type soothing essential oil is placed in a volume of 2-4 m 3 Is provided.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the invention.
The invention has the following description and functions of partial raw materials in the formula:
bentonite: the invention relates to a nonmetallic mineral product which takes montmorillonite as a main mineral component, which is used as a raw material for extracting and preparing sodium exchange montmorillonite.
Octyl trimethyl ammonium chloride: a chemical substance with molecular formula of C 11 H 26 ClN is used as a modifier of sodium-exchanged montmorillonite, enters between sodium-exchanged montmorillonite crystal layers through strong electrostatic interaction, and forms steric hindrance by long carbon chains to increase the crystal layer spacing.
Lavender essential oil: the lavender essential oil is prepared by extracting lavender, has the effects of clearing heat and detoxicating, cleaning skin, removing freckles and whitening, clearing brain and tonifying brain, diminishing inflammation and relieving pain, dispelling wind and dispelling cold, is a good beauty product for females, and can be used for treating the problems of acne, acne marks, acne scars, blackheads, susceptibility to skin, unbalanced skin water and oil, large pores and the like. The lavender can be used for external massage to relieve muscle soreness and improve rheumatic arthritis. Lavender essential oil aromatherapy can be used for relieving pressure and mood, and treating insomnia. Lavender essential oil also has effects of relieving headache, relieving freckle, promoting blood circulation, and removing toxin.
Rose essential oil: the rose essential oil has natural fragrance, and can make people feel mental comfort, pleasure and pleasure, relieve anxiety and depression, relieve pressure and promote sleep. The oleum Rosae Rugosae has antiinflammatory, antibacterial, infectious disease preventing, antiinflammatory, antispasmodic, and cell metabolism and cell regeneration promoting effects.
Chamomile essential oil: the chamomile essential oil is distilled from flowers, has excellent pacifying effect, and can relax anxiety, tension, anger and fear, so that people relax and feel happy. The anxiety is relieved, the mind is calm, and the health care tea is helpful for insomnia.
Essential oil of melissa officinalis: the herba Melissae axillaris essential oil has functions of smoothing and tranquilizing, and can relieve shock, panic and hysteria. However, the bergamot essential oil-like refreshing effect can be realized, so that the dropoff feeling can be reduced, and people can positively ascend; can also sooth people from the pain caused by accidents. The herba Melissae axillaris essential oil has tranquilization effect, can relieve hypertension by acting on circulatory system, and can slow down heart beat to calm emotion; nourish the heart, relieve cramps and hypodynamia. It also has sedative effects on hyperpnea, which also makes it a good drug for the treatment of shock or convulsions.
The invention has the beneficial effects that:
compared with the prior art, the compound type relaxing essential oil is prepared from the lavender essential oil, the rose essential oil, the chamomile essential oil and the melissa essential oil, and can play an excellent relaxing effect by taking the compound type relaxing essential oil as an active ingredient of a fragrance, and can relax anxiety and tension, so that people relax and feel peaceful.
Compared with the prior art, the natural plant essential oil is diffused to form saturated steam under the vacuum condition, the montmorillonite is used for adsorbing the gaseous essential oil, no additional organic solvent is used in the preparation process of the perfume, and the adverse effect caused by the organic solvent is eliminated.
Compared with the prior art, the method uses octyl trimethyl ammonium chloride to treat the sodium-exchanged montmorillonite so as to increase the interlayer spacing of the sodium-exchanged montmorillonite; under the strong electrostatic interaction of the sodium exchange montmorillonite surface, octyl trimethyl ammonium chloride enters between crystal layers, and the space between the crystal layers is increased through the steric hindrance formed by long carbon chains, so that favorable conditions are created for the montmorillonite to adsorb essential oil molecules.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
The comparative example and the examples of the present invention have the following parameters of part of raw materials:
octyl trimethyl ammonium chloride, CAS number: 10108-86-8;
bentonite, 200 mesh, provided by the company of Benzengzhi county, wanxing bentonite Limited liability.
Example 1
A fragrance with relieving effect is prepared by the following method:
(1) Dispersing 5kg of bentonite in 30kg of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 1.5kg of hydrochloric acid into the bentonite mixed solution, and treating for 0.5h; continuously adding 6kg of hydrogen peroxide aqueous solution, treating for 1h, centrifuging, taking the lower layer precipitate, washing with water, drying, and pulverizing to obtain impurity-removed montmorillonite;
(2) Mixing 4.5kg of lavender essential oil, 1.5kg of rose essential oil and 1.8kg of chamomile essential oil to form composite soothing essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 4 hours in the vacuum container; and then placing the impurity-removed montmorillonite in a vacuum container, standing for 36h for adsorption to obtain the impurity-removed montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
The parameters of the mechanical stirring in the step (1) and the steps are as follows: mix for 0.5h at a stirring rate of 450 rpm.
The parameters of the ultrasonic treatment in the step (1) are as follows: ultrasonic power is 550W, ultrasonic frequency is 28kHz, and ultrasonic treatment is carried out for 30min.
The concentration of the hydrochloric acid in the step (1) is 1mol/L.
The concentration of the aqueous hydrogen peroxide solution in the step (1) is 3mol/L.
The internal temperature of the vacuum vessel in the step (2) is 40 ℃.
The corresponding relation between the mass of the compound type relieving essential oil and the volume of the vacuum container in the step (2) is as follows: every 1kg of compound type soothing essential oil is placed in a volume of 2m 3 Is provided.
Example 2
A fragrance with relieving effect is prepared by the following method:
(1) Dispersing 5kg of bentonite in 30kg of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 1.5kg of hydrochloric acid into the bentonite mixed solution, and treating for 0.5h; continuously adding 6kg of hydrogen peroxide aqueous solution, treating for 1h, centrifuging, taking the lower layer precipitate, washing with water, drying, and pulverizing to obtain impurity-removed montmorillonite;
(2) Mixing 4.5kg of lavender essential oil, 1.5kg of rose essential oil and 1.2kg of lemon balm essential oil to form composite type relieving essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 4 hours in the vacuum container; and then placing the impurity-removed montmorillonite in a vacuum container, standing for 36h for adsorption to obtain the impurity-removed montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
The parameters of the mechanical stirring in the step (1) and the steps are as follows: mix for 0.5h at a stirring rate of 450 rpm.
The parameters of the ultrasonic treatment in the step (1) are as follows: ultrasonic power is 550W, ultrasonic frequency is 28kHz, and ultrasonic treatment is carried out for 30min.
The concentration of the hydrochloric acid in the step (1) is 1mol/L.
The concentration of the aqueous hydrogen peroxide solution in the step (1) is 3mol/L.
The internal temperature of the vacuum vessel in the step (2) is 40 ℃.
The corresponding relation between the mass of the compound type relieving essential oil and the volume of the vacuum container in the step (2) is as follows: every 1kg of compound type soothing essential oil is placed in a volume of 2m 3 Is provided.
Example 3
A fragrance with relieving effect is prepared by the following method:
(1) Dispersing 5kg of bentonite in 30kg of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 1.5kg of hydrochloric acid into the bentonite mixed solution, and treating for 0.5h; continuously adding 6kg of hydrogen peroxide aqueous solution, treating for 1h, centrifuging, taking the lower layer precipitate, washing with water, drying, and pulverizing to obtain impurity-removed montmorillonite;
(2) Mixing 4.5kg of lavender essential oil, 1.8kg of chamomile essential oil and 1.2kg of lemon balm essential oil to form composite type relieving essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 4 hours in the vacuum container; and then placing the impurity-removed montmorillonite in a vacuum container, standing for 36h for adsorption to obtain the impurity-removed montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
The parameters of the mechanical stirring in the step (1) and the steps are as follows: mix for 0.5h at a stirring rate of 450 rpm.
The parameters of the ultrasonic treatment in the step (1) are as follows: ultrasonic power is 550W, ultrasonic frequency is 28kHz, and ultrasonic treatment is carried out for 30min.
The concentration of the hydrochloric acid in the step (1) is 1mol/L.
The concentration of the aqueous hydrogen peroxide solution in the step (1) is 3mol/L.
The internal temperature of the vacuum vessel in the step (2) is 40 ℃.
The corresponding relation between the mass of the compound type relieving essential oil and the volume of the vacuum container in the step (2) is as follows: every 1kg of compound type soothing essential oil is placed in a volume of 2m 3 Is provided.
Example 4
A fragrance with relieving effect is prepared by the following method:
(1) Dispersing 5kg of bentonite in 30kg of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 1.5kg of hydrochloric acid into the bentonite mixed solution, and treating for 0.5h; continuously adding 6kg of hydrogen peroxide aqueous solution, treating for 1h, centrifuging, taking the lower layer precipitate, washing with water, drying, and pulverizing to obtain impurity-removed montmorillonite;
(2) Taking 1.5kg of rose essential oil, 1.8kg of chamomile essential oil and 1.2kg of lemon balm essential oil, and mixing the essential oils to form composite soothing essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 4 hours in the vacuum container; and then placing the impurity-removed montmorillonite in a vacuum container, standing for 36h for adsorption to obtain the impurity-removed montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
The parameters of the mechanical stirring in the step (1) and the steps are as follows: mix for 0.5h at a stirring rate of 450 rpm.
The parameters of the ultrasonic treatment in the step (1) are as follows: ultrasonic power is 550W, ultrasonic frequency is 28kHz, and ultrasonic treatment is carried out for 30min.
The concentration of the hydrochloric acid in the step (1) is 1mol/L.
The concentration of the aqueous hydrogen peroxide solution in the step (1) is 3mol/L.
The internal temperature of the vacuum vessel in the step (2) is 40 ℃.
The corresponding relation between the mass of the compound type relieving essential oil and the volume of the vacuum container in the step (2) is as follows: every 1kg of compound type soothing essential oil is placed in a volume of 2m 3 Is provided.
Example 5
A fragrance with relieving effect is prepared by the following method:
(1) Dispersing 5kg of bentonite in 30kg of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 1.5kg of hydrochloric acid into the bentonite mixed solution, and treating for 0.5h; continuously adding 6kg of hydrogen peroxide aqueous solution, treating for 1h, centrifuging, taking the lower layer precipitate, washing with water, drying, and pulverizing to obtain impurity-removed montmorillonite;
(2) Mixing 4.5kg of lavender essential oil, 1.5kg of rose essential oil, 1.8kg of chamomile essential oil and 1.2kg of lemon balm essential oil to form composite type relieving essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 4 hours in the vacuum container; and then placing the impurity-removed montmorillonite in a vacuum container, standing for 36h for adsorption to obtain the impurity-removed montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
The parameters of the mechanical stirring in the step (1) and the steps are as follows: mix for 0.5h at a stirring rate of 450 rpm.
The parameters of the ultrasonic treatment in the step (1) are as follows: ultrasonic power is 550W, ultrasonic frequency is 28kHz, and ultrasonic treatment is carried out for 30min.
The concentration of the hydrochloric acid in the step (1) is 1mol/L.
The concentration of the aqueous hydrogen peroxide solution in the step (1) is 3mol/L.
The internal temperature of the vacuum vessel in the step (2) is 40 ℃.
The corresponding relation between the mass of the compound type relieving essential oil and the volume of the vacuum container in the step (2) is as follows: every 1kg of compound type soothing essential oil is placed in a volume of 2m 3 Is provided.
Example 6
A fragrance with relieving effect is prepared by the following method:
(1) Dispersing 5kg of bentonite in 30kg of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 1.5kg of hydrochloric acid into the bentonite mixed solution, and treating for 0.5h; continuously adding 6kg of hydrogen peroxide water solution, and treating for 1h; finally, adding 8kg of sodium chloride aqueous solution, treating for 1h, centrifuging, taking out the lower layer precipitate, washing with water, drying, and crushing to obtain sodium-exchanged montmorillonite;
(2) Mixing 4.5kg of lavender essential oil, 1.5kg of rose essential oil, 1.8kg of chamomile essential oil and 1.2kg of lemon balm essential oil to form composite type relieving essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 4 hours in the vacuum container; and then placing the sodium-exchanged montmorillonite in a vacuum container for standing for 36h for adsorption to obtain the sodium-exchanged montmorillonite adsorbed with the compound soothing essential oil, namely the fragrance with the soothing effect.
The parameters of the mechanical stirring in the step (1) and the steps are as follows: mix for 0.5h at a stirring rate of 450 rpm.
The parameters of the ultrasonic treatment in the step (1) are as follows: ultrasonic power is 550W, ultrasonic frequency is 28kHz, and ultrasonic treatment is carried out for 30min.
The concentration of the hydrochloric acid in the step (1) is 1mol/L.
The concentration of the aqueous hydrogen peroxide solution in the step (1) is 3mol/L.
The concentration of the sodium chloride aqueous solution in the step (1) is 1mol/L.
The internal temperature of the vacuum vessel in the step (2) is 40 ℃.
The corresponding relation between the mass of the compound type relieving essential oil and the volume of the vacuum container in the step (2) is as follows: every 1kg of compound type soothing essential oil is placed in a volume of 2m 3 Is provided.
Example 7
A fragrance with relieving effect is prepared by the following method:
(1) Dispersing 5kg of bentonite in 30kg of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 1.5kg of hydrochloric acid into the bentonite mixed solution, and treating for 0.5h; continuously adding 6kg of hydrogen peroxide water solution, and treating for 1h; finally, adding 8kg of sodium chloride aqueous solution, treating for 1h, centrifuging, taking out the lower layer precipitate, washing with water, drying, and crushing to obtain sodium-exchanged montmorillonite;
(2) Re-dispersing the sodium-exchanged montmorillonite in 21kg of water, and sequentially mixing and dispersing the sodium-exchanged montmorillonite and the water by mechanical stirring and ultrasonic treatment to form uniform montmorillonite mixed solution; adding 0.9kg of octyl trimethyl ammonium chloride into the montmorillonite mixed solution for reaction; centrifuging the montmorillonite mixed solution after the reaction is finished, taking the lower layer precipitate, washing with water, drying and crushing to obtain modified montmorillonite;
(3) Mixing 4.5kg of lavender essential oil, 1.5kg of rose essential oil, 1.8kg of chamomile essential oil and 1.2kg of lemon balm essential oil to form composite type relieving essential oil; placing the compound type soothing essential oil in a vacuum container, and standing for 4 hours in the vacuum container; and then placing the modified montmorillonite in a vacuum container for standing for 36h for adsorption to obtain the modified montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
The parameters and steps of the mechanical stirring in the steps (1) and (2) are as follows: mix for 0.5h at a stirring rate of 450 rpm.
The parameters and steps of the ultrasonic treatment in the steps (1) and (2) are as follows: ultrasonic power is 550W, ultrasonic frequency is 28kHz, and ultrasonic treatment is carried out for 30min.
The concentration of the hydrochloric acid in the step (1) is 1mol/L.
The concentration of the aqueous hydrogen peroxide solution in the step (1) is 3mol/L.
The concentration of the sodium chloride aqueous solution in the step (1) is 1mol/L.
The temperature of the reaction in the step (2) was 75 ℃, and the reaction was carried out for 1 hour.
The internal temperature of the vacuum vessel in the step (3) is 40 ℃.
The corresponding relation between the mass of the compound type relieving essential oil and the volume of the vacuum container in the step (3) is as follows: every 1kg of compound type soothing essential oil is placed in a volume of 2m 3 Is provided.
Test example 1
Sensory evaluation is carried out on the using effect of the fragrance with relieving effect, 20 sensory test evaluators are selected in each group, and the training of the evaluators meets the specific requirements in GBT 15549-1995 on the aspects of sensory analysis methodology detection and smell identification and the entry and training of the evaluators. 50g of incense with relieving effect is takenAtmosphere is placed at 5m 3 Allowing a official test evaluator to enter a test room after standing for 30min, and grading after waiting for 30min in the room; the room temperature was 25℃and the relative humidity was 50%. Sensory evaluation the fragrance with soothing effect was tested for its intensity of smell, soothing degree, and duration of smell; the strong smell degree is 5 minutes, and the fractions of-2, -1, 0, 1 and 2 respectively represent no obvious smell, lighter smell, proper smell, stronger smell and over-strong smell; the relaxation degree is 10 minutes, and the integer of 1-10 is used for representing the relaxation feeling of an evaluator after the fragrance is used, and the higher the score is, the stronger the relaxation feeling is; the duration of the smell was recorded in hours, and the maximum time the evaluator could feel the smell, i.e. the time the smell intensity reached-2 minutes. The test results were arithmetically averaged and rounded off. The sensory evaluation test results of the fragrance having a soothing effect are shown in table 1.
TABLE 1
Degree of richness (branch) Degree of relaxation (divide) Duration (h)
Example 1 1 4 16
Example 2 1 5 17
Example 3 1 4 17
Example 4 2 5 18
Example 5 -1 6 19
Example 6 -1 7 27
Example 7 0 9 31
As can be seen from the test results of the above examples, example 7 has the best use effect. Example 7 has proper smell, is not thick or light, and can create the most comfortable atmosphere for the testers; furthermore, example 7 also had the longest duration, which was superior to the other examples. The reason for this phenomenon may be that example 7 uses lavender essential oil, rose essential oil, chamomile essential oil, lemon balm essential oil, which can exert excellent soothing effect, relax anxiety and tension, relax and feel peaceful; in addition, example 7 sodium-exchanged montmorillonite was treated with octyl trimethyl ammonium chloride to increase the interlayer spacing thereof; under the strong electrostatic interaction of the sodium exchange montmorillonite surface, octyl trimethyl ammonium chloride enters between crystal layers, and the space between the crystal layers is increased through the steric hindrance formed by long carbon chains, so that favorable conditions are created for the montmorillonite to adsorb essential oil molecules.
Test example 2
The unit adsorption amount of various montmorillonite to essential oil in the fragrance with relieving effect is tested. A weighing instrument is arranged below a device with montmorillonite in a vacuum container, the initial mass of montmorillonite for adsorption and the final mass after adsorption are recorded, and the unit adsorption amount is calculated according to the following formula:
wherein a is the unit adsorption quantity, and the unit is mg/g; m is m 1 The initial mass is expressed in g; m is m 2 The unit is g for the mass after adsorption.
The results of the unit adsorption amount of the essential oil by each montmorillonite in the fragrance with relieving effect are shown in Table 2.
TABLE 2
Adsorption per unit (mg/g)
Example 5 142
Example 6 203
Example 7 278
The higher the unit adsorption amount, the more the montmorillonite adsorbs the essential oil. As can be seen from the comparison of the above examples, example 7 using the modified montmorillonite has the best adsorption effect. The reason for this phenomenon may be that the sodium-exchanged montmorillonite surface has strong electrostatic interactions, which facilitate adsorption of montmorillonite and essential oil molecules; in addition, hydroxyl exists on the surface of the sodium-exchanged montmorillonite, so that hydrogen bonds can be formed between the sodium-exchanged montmorillonite and essential oil, and adsorbed essential oil is reserved in the montmorillonite; the sodium-exchanged montmorillonite can be treated by octyl trimethyl ammonium chloride to increase the interlayer spacing; under the strong electrostatic interaction of the surface of the sodium-exchanged montmorillonite, octyl trimethyl ammonium chloride enters between crystal layers, the space between the crystal layers is increased through the steric hindrance formed by long carbon chains, and the adsorption area of the sodium-exchanged montmorillonite is increased.

Claims (9)

1. A method for preparing a fragrance with soothing effect, comprising the following steps:
(1) Dispersing bentonite in water to form uniform bentonite mixed solution; centrifuging the bentonite mixed solution after acid treatment, oxidation treatment and particle exchange treatment, and taking out the lower-layer sediment, washing, drying and crushing to obtain sodium-exchanged montmorillonite;
(2) Dispersing the sodium-exchanged montmorillonite in water to form uniform montmorillonite mixed solution; adding octyl trimethyl ammonium chloride into the montmorillonite mixed solution and reacting; centrifuging after the reaction is finished, taking the lower layer precipitate, washing with water, drying and crushing to obtain modified montmorillonite;
(3) Mixing lavender essential oil, rose essential oil, chamomile essential oil and lemon balm essential oil to form composite type relieving essential oil; placing the compound soothing essential oil in a vacuum environment, and forming saturated steam through diffusion; and then the modified montmorillonite is used for adsorbing saturated steam to obtain the fragrance with the relieving effect.
2. The method for preparing a fragrance having a soothing effect according to claim 1, comprising the steps of, in parts by weight:
(1) Dispersing 5-9 parts of bentonite in 30-54 parts of water, and sequentially mixing and dispersing the bentonite and the water through mechanical stirring and ultrasonic treatment to form uniform bentonite mixed solution; adding 0.5-2 parts of hydrochloric acid into the bentonite mixed solution, and treating for 0.5-2 hours; continuously adding 4-8 parts of hydrogen peroxide aqueous solution, and treating for 0.5-2 hours; finally adding 6-12 parts of sodium chloride aqueous solution, treating for 0.5-1 h, centrifuging, taking out the lower layer precipitate, washing, drying and crushing to obtain sodium-exchanged montmorillonite;
(2) Re-dispersing the sodium-exchanged montmorillonite in 15-36 parts of water, and sequentially mixing and dispersing the sodium-exchanged montmorillonite and the water through mechanical stirring and ultrasonic treatment to form uniform montmorillonite mixed solution; adding 0.45-1.35 parts of octyl trimethyl ammonium chloride into the montmorillonite mixed solution for reaction; centrifuging the montmorillonite mixed solution after the reaction is finished, taking the lower layer precipitate, washing with water, drying and crushing to obtain modified montmorillonite;
(3) Taking 3-6 parts of lavender essential oil, 0.5-2 parts of rose essential oil, 0.6-3 parts of chamomile essential oil and 1.2-3 parts of lemon balm essential oil, and mixing the essential oils to form composite relieving essential oil; placing the composite soothing essential oil in a vacuum container, and standing for 2-4 hours in the vacuum container; and then placing the modified montmorillonite in a vacuum container for standing for 12-48 hours for adsorption to obtain the modified montmorillonite adsorbed with the composite soothing essential oil, namely the fragrance with the soothing effect.
3. A process for the preparation of a fragrance having a soothing effect according to claim 2, characterized in that: the concentration of the hydrochloric acid in the step (1) is 1-2 mol/L.
4. A process for the preparation of a fragrance having a soothing effect according to claim 2, characterized in that: the concentration of the hydrogen peroxide aqueous solution in the step (1) is 1-3 mol/L.
5. A process for the preparation of a fragrance having a soothing effect according to claim 2, characterized in that: the concentration of the sodium chloride aqueous solution in the step (1) is 0.5-1 mol/L.
6. A process for the preparation of a fragrance having a soothing effect according to claim 2, characterized in that: the reaction temperature in the step (2) is 60-75 ℃, and the reaction time is 0.5-1 h.
7. A process for the preparation of a fragrance having a soothing effect according to claim 2, characterized in that: in the step (3), the internal temperature of the vacuum container is 35-40 ℃.
8. The method for preparing a fragrance with soothing function according to claim 2, wherein the mass of the compound soothing essential oil in the step (3) and the volume of the vacuum container are related as follows: placing 1kg of compound soothing essential oil in a volume of 2-4 m 3 Is a vacuum vessel of (a).
9. A fragrance having soothing action, characterized in that: the method according to any one of claims 1 to 8.
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