Preparation method and application of coating essential oil-loaded zeolite molecular sieve with water burst release performance

Abstract

The invention relates to a preparation method and application of a coating essential oil-loaded zeolite molecular sieve with water burst release performance. Specifically, the essential oil-loaded zeolite molecular sieve is provided, and the essential oil-loaded zeolite molecular sieve is prepared from essential oil and a zeolite molecular sieve, the coating essential oil-loaded zeolite molecular sieve further comprises a coating, the coating is prepared by coating with a coating solution, and the coated essential oil-loaded zeolite molecular sieve is a coating essential oil-loaded zeolite molecular sieve. The coating essential oil-loaded zeolite molecular sieve with the water burst release performance is very slow in release under the condition of normal temperature, can realize uniform release under certain temperature and humidity, has the burst release performance under the condition of water, and can be used for preparing the coating essential oil-loaded zeolite molecular sieve with the water burst release performance. The coating essential oil-loaded zeolite molecular sieve prepared by the invention provides very beneficial help for the application of the coating essential oil-loaded zeolite molecular sieve in products such as paper diapers and the like. Meanwhile, the preparation method of the coating essential oil-loaded zeolite molecular sieve is simple, the raw materials are easy to obtain, the cost is low, and the coating essential oil-loaded zeolite molecular sieve is very suitable for commercial production.

Description

Technical Field

[0001] The invention relates to a preparation method of a coated essential oil-carrying zeolite molecular sieve with burst release performance upon contact with water and application thereof. Background Art

[0002] Chinese herbal essential oil is a general term for volatile aromatic oily liquids that can be distilled with steam. It has a variety of pharmacological activities such as aromatic flavor correction, sedation, anti-inflammatory and antibacterial. However, essential oils have disadvantages such as unstable physical and chemical properties, strong volatility, and easy oxidation and degradation, which limit their wide use in many fields. If essential oils or essential oil formulas are loaded and solidified through corresponding technologies, the stability of essential oils is improved, the release rate of essential oils is controlled, and the essential oils can be released slowly, their application range in the fields of health and textiles can be expanded, and their aromatic properties can be used to achieve aromatherapy, flavor correction and deodorization.

[0003] Some methods for solidifying essential oils have been provided in the prior art. For example, patent CN202210752507.7 discloses an emulsion encapsulation technology, which encapsulates plant essential oils with antibacterial and bactericidal effects, composites them with porous carrier bio-based activated carbon, and evenly distributes them on the surface of paper to achieve a sustained-release bactericidal effect and improve the bioavailability of active substances. However, the porous materials of this type of technology need to be prepared by themselves, and the essential oils are emulsified and corresponding additives are added, which increases the process cost and time cost.

[0004] Patent CN201811609259.0 discloses a method for preventing and controlling post-harvest Alternaria of grapes using a sepiolite / essential oil composite material. As a rare non-metal, sepiolite has a rich pore structure and can adsorb essential oils to delay their release. However, such porous materials need to be acid-activated before use, and the process is complicated and cumbersome. In summary, although some methods for curing essential oils are mentioned in the prior art, there are still problems such as many steps in the preparation method and difficulty in obtaining the raw materials used, which seriously affects the curing efficiency of the essential oils.

[0005] Technical difficulty of zeolite molecular sieve solidification of essential oils: Zeolite molecular sieve is a porous solid material, because of its numerous interconnected channels inside, while providing space for adsorption and solidification of essential oils, it also limits its loading method to a certain extent. The pore size of zeolite molecular sieve is between 0.3-1nm, and the pore size is relatively small. At present, the commonly used methods for porous materials to adsorb essential oils mainly include essential oil solution immersion method (immersing the porous material in a solution containing essential oils) and pure essential oil immersion method, and the adsorption process is completed by long-term contact between the essential oil and the porous material. Both methods involve subsequent drying and other treatments of the porous material adsorbed with essential oils, which are complex processes, time-consuming, and the drying process will cause essential oil loss and high cost. This patent adopts a stirring method to promote the essential oil to enter the internal pores of the zeolite through the action of external forces. Compared with the traditional method of immersing in essential oil solutions or pure essential oils, it shortens the time and improves efficiency. In addition, the volatility of the essential oil that has entered the internal pores of the zeolite is restricted to a certain extent due to the influence of steric hindrance and van der Waals forces, thereby achieving the effect of delaying the release of essential oils. Summary of the invention

[0006] In order to solve the above problems, the present invention provides a method for preparing a coated essential oil-loaded zeolite molecular sieve having a burst release property upon contact with water.

[0007] One aspect of the present invention provides an essential oil-carrying zeolite molecular sieve, wherein the essential oil-carrying zeolite molecular sieve is made of essential oil and zeolite molecular sieve;

[0008] Preferably, the essential oil-carrying zeolite molecular sieve further comprises a coating, and the coating is prepared by coating with a coating liquid, and the coated essential oil-carrying zeolite molecular sieve is a coated essential oil-carrying zeolite molecular sieve.

[0009] In the technical solution of the present invention, the essential oil-carrying zeolite molecular sieve is obtained by the following method:

[0010] S1) weighing essential oil and zeolite molecular sieve; the mass ratio of the essential oil to the zeolite molecular sieve is 1:1.5-1:7; preferably 1:2, 1:3, 1:4, 1:5, 1:6, 1:7;

[0011] S2) placing the zeolite molecular sieve in a stirring device and stirring, and dropping or spraying the essential oil onto the zeolite molecular sieve surface and stirring evenly;

[0012] Preferably, it also comprises step S3)

[0013] S3) mixing and stirring the essential oil-carrying zeolite molecular sieve obtained in step S2) with the coating liquid to obtain a coated essential oil-carrying zeolite molecular sieve.

[0014] In the technical solution of the present invention, the essential oil is a single essential oil or a compound essential oil.

[0015] In the technical scheme of the present invention, the essential oil is selected from natural essential oils with volatility extracted from plants, preferably the active ingredient in the natural essential oil has a molecular diameter smaller than the pore size of the zeolite, and more preferably the active ingredient in the natural essential oil has a molecular diameter of 0.01-1 nm. For example, selected from peppermint oil, jasmine oil, citronella oil, perilla oil, sandalwood oil, cassia oil, rose oil, borneol, storax, patchouli oil, tangerine peel oil, basil oil, wormwood oil, eucalyptus oil, star anise oil, white cardamom oil, white mustard oil, cubeb oil, atractylodes oil, cardamom oil, tsaoko oil, agarwood oil, chuanxiong oil, angelica oil, clove oil, zedoary oil, saposhnikovia oil, citrus oil, dried ginger oil, galangal oil, chuanxiong oil, rhodiola rosea oil, prickly ash oil, small Fennel oil, Centella asiatica oil, mustard oil, Nepeta oil, orange peel oil, Forsythia oil, Myrrh oil, Elsholtzia densiflora oil, Notopterygium oil, Nutmeg oil, Cinnamon oil, Frankincense oil, Amomum oil, Cnidium monnieri oil, Ginger oil, Acorus calamus oil, turpentine oil, Turmeric oil, Evodia rutaecarpa oil, Asarum oil, Torreya grandis oil, Cyperus rotundus oil, Magnolia oil, Alpinia oxyphylla oil, Aucklandia suspensa oil, Citrus aurantium oil, Salvia miltiorrhiza oil, Wintergreen oil, Fennel oil, Lemon oil, Artemisia annua oil, Amomum oil or a combination thereof.

[0016] In the technical solution of the present invention, the zeolite molecular sieve is selected from zeolite molecular sieves in the form of strips, spheres, and activated powders.

[0017] In the technical solution of the present invention, the size of the zeolite molecular sieve is 0.01mm-6mm, preferably 0.4mm, 0.8mm, 1.6mm, 2.5mm, 3.0mm, 3.2mm, 4.0mm, and 5.0mm.

[0018] In the technical solution of the present invention, the zeolite molecular sieve is selected from one or more of 4A zeolite molecular sieve, 5A zeolite molecular sieve, 13X zeolite molecular sieve, 13X-HP zeolite molecular sieve and 13X zeolite activated powder.

[0019] In the technical solution of the present invention, the coating solution is selected from one or more of PEG 200, PEG 400, PEG 600, or PEG2000 and HPMC E5 dissolved in deionized water to prepare a coating solution with a concentration of 2.5-3.5%.

[0020] In the technical solution of the present invention, the stirring equipment is a ball mill or a stirrer.

[0021] In the technical solution of the present invention, the mass of the coating is 1%-15% of the total mass of the essential oil and the zeolite molecular sieve, preferably 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%.

[0022] Another aspect of the present invention provides a method for preparing the above essential oil-carrying zeolite molecular sieve, the preparation method comprising the following steps:

[0023] S1) weighing essential oil and zeolite molecular sieve; the mass ratio of the essential oil to the zeolite molecular sieve is 1:1.5-1:7; preferably 1:2, 1:3, 1:4, 1:5, 1:6, 1:7;

[0024] S2) placing the zeolite molecular sieve in a stirring device and stirring, and dropping or spraying the essential oil onto the zeolite molecular sieve surface and stirring evenly;

[0025] Preferably, it also comprises step S3)

[0026] S3) mixing and stirring the essential oil-carrying zeolite molecular sieve obtained in step S2) with the coating liquid to obtain a coated essential oil-carrying zeolite molecular sieve.

[0027] In another aspect, the present invention provides a daily necessity containing essential oil, wherein the daily necessity is selected from diapers, sanitary napkins, masks, protective clothing, and insoles.

[0028] Another aspect of the present invention provides the use of the essential oil-carrying zeolite molecular sieve in the preparation of antibacterial drugs, skin care products, cosmetics, daily necessities, and fragrance products.

[0029] Another aspect of the present invention provides a method for controlling the rate of essential oil release of an essential oil-carrying zeolite molecular sieve under high temperature and high humidity conditions, the method comprising a process of coating the surface of the essential oil-carrying zeolite molecular sieve to form a coating layer, wherein the release rate is y, in units of % / min, x is the coating weight gain percentage, and the high temperature and high humidity are conditions of 36°C and 60% humidity;

[0030] y = -0.0106x + 0.4803;

[0031] The coating weight gain percentage is the percentage of the coating layer weight to the weight of the uncoated essential oil-loaded zeolite molecular sieve.

[0032] In the technical solution of the present invention, the antibacterial agent is anti-Escherichia coli, Staphylococcus aureus, and Candida albicans.

[0033] Beneficial Effects

[0034] 1) The method of the present invention utilizes zeolite molecular sieve to solidify Chinese medicine essential oil for the first time. Zeolite molecular sieve is a silicate inorganic compound with a porous structure, which has rich internal pores, large specific surface, and good adsorption. Through physical adsorption, the essential oil is adsorbed into its internal pore structure, and the barrier effect of the pore structure is used to achieve the purpose of delaying the release of the essential oil, and the essential oil is adsorbed and solidified, which solves the shortcomings of the essential oil being volatile and unstable in physicochemical properties. In addition, zeolite molecular sieve has the advantages of good thermal stability and antibacterial effect. If it is applied to sanitary products and combined with the corresponding Chinese medicine essential oil, it can synergistically exert the drug effect.

[0035] 2) The present invention also combines the coating liquid to coat the zeolite molecular sieve loaded with essential oils, and further delays the release of the essential oils through the coating of the coating liquid. The different weight gain ratios of the coating determine the different degrees of encapsulation, thereby making the release speed of the essential oils different, which can meet the use requirements of different scenarios.

[0036] 3) The coating material of the present invention is liquid and does not require other solvation treatment. A stirring method can be used to achieve rapid coating. Compared with cyclodextrin inclusion, nanoemulsion, microcapsule, Pickering emulsification and liposome nanotechnology, it has the advantages of being simple and easy to operate, convenient for industrial production, and free of organic solvent residues. It also does not require a drying process, can avoid the loss of essential oils due to heating conditions, and is easy to scale up production.

[0037] 4) The coated essential oil-loaded zeolite molecular sieve of the present invention releases very slowly at room temperature, but can achieve uniform release at a certain temperature and humidity, and has a burst release performance when exposed to water, which provides very beneficial help for the application of the coated essential oil-loaded zeolite molecular sieve prepared by the present invention in products such as diapers.

[0038] 5) The coated essential oil-carrying zeolite molecular sieve of the present invention realizes quantitative regulation of the release rate through coating, and the burst release ratio can be regulated through coating.

[0039] 6) Both zeolite itself and zeolite loaded with essential oil have antibacterial effects, and the two have a synergistic effect in antibacterial effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 This is the release curve of the peppermint oil-loaded zeolite molecular sieve in Example 1.

[0041] Figure 2 is the loss rate of essential oil in the coating process with different coating solutions.

[0042] Figure 3 The release curves of essential oil-loaded zeolite peppermint oil at different coating ratios.

[0043] Figure 4 The relationship between release rate and coating ratio.

[0044] Figure 5 Results of the loss of essential oils after 24 hours of storage of different coated essential oil-loaded zeolite molecular sieves. (Data are expressed as mean ± standard error; ** represents P < 0.01.)

[0045] Figure 6 Evaluation of the inhibitory effect of the coated essential oil-loaded zeolite group on Escherichia coli (the zeolite addition amounts from left to right are 14.1 mg, 28.2 mg, and 70.5 mg).

[0046] Figure 7 Evaluation of the inhibitory effect of the essential oil-coated zeolite group on Staphylococcus aureus (the zeolite addition amounts from left to right are 14.1 mg, 28.2 mg, and 70.5 mg).

[0047] Figure 8 Evaluation of the inhibitory effect of the essential oil-coated zeolite group on Candida albicans (the zeolite addition amounts from left to right are 14.1 mg, 28.2 mg, and 70.5 mg).

[0048] Fig. 9 Evaluation of the inhibitory effect of the essential oil group on Escherichia coli (the amount of essential oil added from left to right is 3.2 mg, 6.4 mg, and 16.0 mg).

[0049] Fig.10 Evaluation of the inhibitory effect of the essential oil group on Staphylococcus aureus (the amount of essential oil added from left to right is 3.2 mg, 6.4 mg, and 16.0 mg).

[0050] Fig.11 Evaluation of the inhibitory effect of the essential oil group on Candida albicans (the amount of essential oil added from left to right is 3.2 mg, 6.4 mg, and 16.0 mg). DETAILED DESCRIPTION

[0051] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and understandable, the specific implementation modes of the present invention are described in detail below, but it should not be understood as limiting the applicable scope of the present invention.

[0052] Specific preparation process:

[0053] (1) Preparation of essential oil-loaded zeolite: Weigh appropriate amounts of essential oil (or essential oil formula) and zeolite molecular sieve according to mass ratio, place the zeolite molecular sieve in a stirring device, dropwise or spray the essential oil (or essential oil formula) into the stirring device, rotate at 200 r / min, and stir for 5 min to obtain the zeolite;

[0054] (2) Preparation of coated essential oil-loaded zeolite: Weigh appropriate amounts of the essential oil-loaded zeolite and coating liquid according to the coating ratio, place the essential oil-loaded zeolite in a stirring device, and drop or spray the coating liquid into the stirring device for 3 minutes.

[0055] The solidification of essential oil can be achieved through the above two-step stirring process. First, the essential oil is adsorbed and solidified by porous materials, and then it is wrapped and solidified again through coating technology, thereby improving the stability of the essential oil. By adjusting the coating ratio, the release rate of the essential oil can also be controlled.

[0056] Example 1 Preparation of essential oil-carrying zeolite molecular sieve

[0057] Weigh peppermint oil and zeolite molecular sieve 13X-HP (spherical 0.4-0.8 mm) at a mass ratio of essential oil to zeolite of 1:3;

[0058] First, put zeolite molecular sieve 13X-HP into a mixer and stir;

[0059] Slowly drop peppermint oil into the zeolite molecular sieve 13X-HP in the mixer, keep the speed at 200r / min, and stir for 5 minutes to obtain the essential oil-loaded zeolite molecular sieve.

[0060] Evaluation of the sustained-release effect of essential oil-carrying zeolite molecular sieve: Weigh 25 mg of peppermint oil and 100 mg of essential oil-carrying zeolite molecular sieve parallel samples in open weighing bottles, place them in an environment with a temperature of 25°C and a humidity of 40% ± 5%, take samples at 0, 12, 24, 36, 48, and 72 hours, perform gas chromatography analysis, and calculate the release amount. The release rate is calculated as follows:

[0061] w T (%) = (w0-w b ) / w0×100% (4)

[0062] Where: w0 is the initial content of essential oil in the essential oil zeolite, w b It is a method to determine the content of essential oil in essential oil zeolite within a certain period of time.

[0063] The results show that ( Figure 1 ), after 72 hours of release, the release rate of peppermint oil itself was 66.75%, and the release rate of essential oil-loaded zeolite molecular sieve was 32.06%. The results show that the zeolite molecular sieve solidification can slow down the release of essential oil. The release curves at different time points are detailed in Figure 1 It can be seen that the release rate of peppermint oil solidified by zeolite molecular sieve is not only slowed down, but also stable, without sudden release.

[0064] Example 2 Screening of coating solution

[0065] Water-soluble coating materials hydroxypropyl methylcellulose E5 (HPMC E5) and polyethylene glycol 2000 (PEG 2000), and liquid coating materials PEG 400 and PEG 600 were used as coating solutions for screening. The loss rate of peppermint oil during the coating process was used as an indicator to screen the coating solutions.

[0066] (1) Coating pan coating method

[0067] Dissolve PEG 2000 and HPMC E5 in deionized water to prepare a coating solution with a concentration of 3%; accurately weigh the essential oil-carrying zeolite and the coating solution according to the coating weight gain of 5% (g / g); place the essential oil-carrying zeolite in a coating machine; spray the coating solution evenly on the surface of the essential oil-carrying zeolite at an appropriate position with a spray gun for coating; the coating machine rotates at 50 r / min; and slowly dries with hot air at 50°C.

[0068] (2) Stirring coating method

[0069] Taking PEG 400 and PEG 600 as coating liquid, accurately weigh the essential oil-loaded zeolite and the coating liquid according to the coating weight gain of 5% (g / g), put the essential oil-loaded zeolite in a beaker, slowly add the coating liquid dropwise to the essential oil-loaded zeolite, seal with plastic wrap, and stir for 3 minutes.

[0070] The loss rate of peppermint oil during coating by different coating methods is as follows Figure 2 As shown in the figure, in the coating pan coating method, the loss caused by HPMC E5 as the coating material is less than that caused by PEG 2000; in the stirring coating method, the loss caused by PEG 400 as the coating material is less than that caused by PEG 600. Compared with the two coating methods, due to heating, the coating pan coating method will cause a larger loss rate, with a minimum value of 6.75%. In comparison, the maximum loss rate of the stirring coating method is only 4.24%, which is significantly less than that of the coating pan coating method. Therefore, PEG 400 stirring coating is preferred to prepare coated essential oil-loaded zeolite molecular sieves.

[0071] Example 3 Preparation of coated essential oil-carrying zeolite molecular sieve

[0072] Weigh peppermint oil and zeolite molecular sieve 13X-HP (spherical 0.4-0.8 mm) at a mass ratio of essential oil to zeolite of 1:3, and first put the zeolite molecular sieve 13X-HP into a blender for stirring;

[0073] Slowly drip peppermint oil into the zeolite molecular sieve 13X-HP in the mixer, keep the speed at 200r / min, and stir for 5min to obtain the essential oil-loaded zeolite molecular sieve;

[0074] Weigh the coating liquid PEG 400, the mass of which is 1%, 5%, 8%, 10% and 12% of the mass of the essential oil-carrying zeolite molecular sieve; drop or spray the coating liquid into the essential oil-carrying zeolite molecular sieve in the mixer, keep the speed at 200 r / min, and stir for 3 minutes to obtain the coated essential oil-carrying zeolite molecular sieve.

[0075] Weigh 100 mg of the above-prepared coated essential oil zeolite molecular sieve into an open weighing bottle and place it in an environment with a temperature of 36°C and a humidity of 60% to simulate the release of essential oil in the use environment of disposable sanitary products such as diapers. Samples were taken from the gas phase every 30 minutes for content determination. At the same time, artificial urine was added at the 150th minute to simulate the release of diapers after encountering artificial urine. The results showed that ( Figure 3 ), after 180 minutes of release, the total release rate of 12% coated essential oil zeolite was 59.22% after 180 minutes, while the total release rate of 1% coated essential oil zeolite was 78.79%. The results show that the release of essential oil can be delayed by coating, and the higher the coating weight gain ratio, the better the effect of delaying the release of essential oil. Therefore, different weight gain ratios of coated essential oil zeolite molecular sieves can meet the requirements of different products for the release time of essential oil.

[0076] Furthermore, the average release rate (% / min) of the uncoated, 1% coated, 5% coated, and 12% coated essential oil-loaded zeolites from 0 to 150 min (without water) was taken as the ordinate, and the coating weight gain percentage (%) was taken as the abscissa, and the regression equation was obtained by fitting the curve. The results show that (Table 1 and Figure 4 ), the release rate has a good linear relationship with the coating weight gain percentage, release rate: y = -0.0106x + 0.4803, R 2 =0.9579. The higher the coating weight gain ratio, the lower the release rate of the essential oil-carrying zeolite. Through the research of the present invention, the inventors found that the release rate of the coated essential oil-carrying zeolite molecular sieve of the present invention can be controlled by adjusting the coating weight gain percentage. When a different release rate is required, the required coating amount can be calculated according to the above linear equation to achieve the purpose of adjusting the release rate.

[0077] Table 1 Average release rate of essential oil-loaded zeolites with different coating ratios

[0078]

[0079] Example 4 Analysis of the Burst Release of Essential Oil-Carrying Zeolite Molecular Sieve Coated

[0080] Weigh peppermint oil and zeolite molecular sieve 13X-HP (spherical 0.4-0.8 mm) at a mass ratio of essential oil to zeolite of 1:3, and first put the zeolite molecular sieve 13X-HP into a blender for stirring;

[0081] Slowly drip peppermint oil into the zeolite molecular sieve 13X-HP in the mixer, keep the speed at 200r / min, and stir for 5min to obtain the essential oil-loaded zeolite molecular sieve;

[0082] Weigh the coating liquid PEG 400, the mass of which is 1%, 2%, 5%, 10% and 12% of the mass of the essential oil-carrying zeolite molecular sieve; drop or spray the coating liquid into the essential oil-carrying zeolite molecular sieve in the mixer, keep the speed at 200 r / min, and stir for 3 minutes to obtain the coated essential oil-carrying zeolite molecular sieve.

[0083] Weigh 100 mg of each of the above-prepared coated essential oil-carrying zeolite molecular sieves in an open weighing bottle, place it in an environment of 36°C and 60% humidity to simulate the release of essential oil in the use environment of disposable sanitary products such as diapers, and sample the gas phase every 30 minutes for content determination. At the same time, artificial urine was added at the 150th minute to determine the release of essential oil 30 minutes after contact with urine. By comparing the release of the essential oil-carrying zeolite molecular sieve 30 minutes before and after contact with urine, its burst release was evaluated.

[0084] Burst release ratio = (essential oil release rate 30 minutes after encountering urine / essential oil release rate 30 minutes before encountering urine) × 100%

[0085] The results show (Table 2) that the essential oil-carrying zeolite molecular sieve of the present invention can not only realize stable release under high humidity, but also can perform burst release after encountering urine, which makes it fully meet the application in products such as diapers, and can not only slowly release essential oils in conventional use, prevent diaper rash caused by long-term use of diapers, but also release a large amount of essential oils when a large amount of urine appears to protect the user's buttocks skin from being soaked in urine for a long time, causing skin damage, while achieving an antibacterial effect. After coating, the burst release ability of the essential oil-carrying zeolite can be adjusted by adjusting the coating ratio. As the coating ratio decreases, the burst release ratio increases, and the burst release ability shows an enhanced trend.

[0086] Table 2 Burst release ratio of essential oil-loaded zeolite with different coating ratios

[0087]

[0088] Example 5: Release of essential oil-coated zeolite molecular sieve at room temperature

[0089] Preparation of coated and uncoated essential oil-loaded zeolite molecular sieves: The essential oil-loaded zeolite molecular sieve was prepared by the method of Example 1, and the coated essential oil-loaded zeolite molecular sieve was prepared by the method of Example 3, wherein the coating weight gain was 5%.

[0090] The release at room temperature was evaluated by the loss rate of essential oils in coated and uncoated zeolite molecular sieves loaded with essential oils during storage. Accurately weigh 1g of coated and uncoated zeolite molecular sieves loaded with essential oils and place them at room temperature for 24 hours. The content of essential oils in the coated and uncoated zeolite molecular sieves loaded with essential oils after 24 hours of storage was determined, and the loss rate of essential oils before and after storage was calculated.

[0091] Loss rate = (total content of peppermint oil after 0 hours of storage - total content of peppermint oil after 24 hours of storage) / total content of peppermint oil after 0 hours of storage

[0092] The results show that ( Figure 5 ) Compared with uncoated essential oil-loaded zeolite, the essential oil-loaded zeolite molecular sieves coated with both coating materials can effectively reduce the loss of peppermint oil during storage, and PEG 400 is better than PEG 600 as the coating material.

[0093] Example 6 Antibacterial performance test of essential oil-coated zeolite molecular sieve

[0094] Preparation of coated essential oil-loaded zeolite molecular sieve: The coated essential oil-loaded zeolite molecular sieve was prepared by the method of Example 3, wherein the coating weight gain was 10%, and the antibacterial performance of the essential oil-loaded zeolite molecular sieve was evaluated.

[0095] ① Investigation on the antibacterial properties of essential oil-loaded zeolite:

[0096] Prepare plate culture dishes containing Escherichia coli, Staphylococcus aureus and Candida albicans; use agar plate diffusion method to investigate the antibacterial effect of essential oil zeolite. Pour the coated essential oil zeolite molecular sieve in the center of the plate so that the stacked zeolite particles are circular with a diameter of 20 mm. The amount of sample added to each plate of the essential oil zeolite group is 14.1 mg, 28.2 mg and 70.5 mg, and each sample is parallel to 3 groups, and the size of the antibacterial zone of each group of plates is observed and compared.

[0097] ②Evaluation of antibacterial properties of essential oil formula:

[0098] Design of antibacterial dosage of essential oil formula: According to the composition ratio of coated essential oil zeolite molecular sieve, the dosage of essential oil in the formula is 3.20mg, 6.40mg and 16.01mg. The antibacterial performance of the essential oil formula was evaluated by agar plate diffusion method. Four Oxford cups were placed in a clockwise direction with sterile tweezers. The above amount of essential oil formula was added to three Oxford cups, and one Oxford cup was not added as a control. Mark the bottom of the dish with a marker. Compare the size of the antibacterial zone and compare it with the essential oil-loaded zeolite to evaluate the changes in the antibacterial performance of the essential oil after adsorption by the zeolite molecular sieve.

[0099] The results showed (Table 3, Figure 6-11), different doses of essential oil formula and essential oil-carrying zeolite have certain inhibitory effects on the growth of Escherichia coli, Staphylococcus aureus and Candida albicans, and as the dose of essential oil-carrying zeolite increases, the diameter of the inhibition zone gradually increases; in addition, for the same amount of essential oil and essential oil-carrying zeolite, the antibacterial effect of essential oil-carrying zeolite is stronger than that of the essential oil formula, and the sustained release function of essential oil-carrying zeolite makes its antibacterial performance better than that of the essential oil itself. The above results show that essential oil-carrying zeolite has a significant antibacterial effect, and is stronger than the same dose of essential oil.

[0100] Table 3 Agar plate diffusion method antibacterial test results

[0101]

Claims

1. A zeolite molecular sieve carrying essential oil, characterized in that: The essential oil-carrying zeolite molecular sieve is made of essential oil and zeolite molecular sieve; Preferably, the essential oil-carrying zeolite molecular sieve further comprises a coating, and the coating is prepared by coating with a coating liquid, and the coated essential oil-carrying zeolite molecular sieve is a coated essential oil-carrying zeolite molecular sieve.

2. The essential oil-carrying zeolite molecular sieve according to claim 1, characterized in that: The essential oil-carrying zeolite molecular sieve is obtained by the following method: S1) weighing essential oil and zeolite molecular sieve; the mass ratio of the essential oil to the zeolite molecular sieve is 1:1.5-1:7; preferably 1:2, 1:3, 1:4, 1:5, 1:6, 1:7; S2) placing the zeolite molecular sieve in a stirring device and stirring, and dropping or spraying the essential oil onto the zeolite molecular sieve surface and stirring evenly; Preferably, it also comprises step S3) S3) mixing and stirring the essential oil-carrying zeolite molecular sieve obtained in step S2) with the coating liquid to obtain a coated essential oil-carrying zeolite molecular sieve; Preferably, the stirring equipment is a ball mill or a stirrer.

3. The essential oil-carrying zeolite molecular sieve according to claim 1, characterized in that: The essential oil is a single essential oil or a compound essential oil; Preferably, the essential oil is selected from volatile natural essential oils extracted from plants. More preferably, the molecular diameter of the active ingredient in the natural essential oil is smaller than the pore diameter of the zeolite. More preferably, it is an active ingredient in natural essential oils with a molecular diameter of 0.01-1 nm.

4. The essential oil-carrying zeolite molecular sieve according to claim 1, characterized in that: The zeolite molecular sieve is selected from the zeolite molecular sieve in the form of strip, sphere and activated powder; Preferably, the zeolite molecules are screened from a size of 0.01 mm to 6 mm, preferably 0.4 mm, 0.8 mm, 1.6 mm, 2.5 mm, 3.0 mm, 3.2 mm, 4.0 mm, 5.0 mm; Preferably, the zeolite molecular sieve is selected from one or more of 4A zeolite molecular sieve, 5A zeolite molecular sieve, 13X zeolite molecular sieve, 13X-HP zeolite molecular sieve and 13X zeolite activated powder.

5. The essential oil-carrying zeolite molecular sieve according to claim 1, characterized in that: The coating solution is selected from one or more of PEG 200, PEG 400, PEG 600, or PEG 2000 and HPMC E5 dissolved in deionized water to prepare a coating solution with a concentration of 2.5-3.5%; Preferably, in the technical solution of the present invention, the mass of the coating is 1%-15% of the total mass of the essential oil and the zeolite molecular sieve.

6. The essential oil-carrying zeolite molecular sieve according to claim 1, characterized in that: The essential oil-carrying zeolite molecular sieve can release the essential oil at a rate of y. y = -0.0106x + 0.4803; Wherein, the release rate is y, in % / min, and x is the coating weight gain percentage; The release rate is under high temperature and high humidity conditions, wherein the high temperature and high humidity are under the conditions of temperature 36°C and humidity 60%; The coating weight gain percentage is the percentage of the coating layer weight to the weight of the uncoated essential oil-loaded zeolite molecular sieve.

7. A method for preparing the essential oil-carrying zeolite molecular sieve according to any one of claims 1 to 6, the method comprising the following steps: S1) weighing essential oil and zeolite molecular sieve; the mass ratio of the essential oil to the zeolite molecular sieve is 1:1.5-1:7; S2) placing the zeolite molecular sieve in a stirring device and stirring, and dropping or spraying the essential oil onto the zeolite molecular sieve surface and stirring evenly; Preferably, it also comprises step S3) S3) mixing and stirring the essential oil-carrying zeolite molecular sieve obtained in step S2) with the coating liquid to obtain the coated essential oil-carrying zeolite molecular sieve.

8. A daily necessity containing essential oil, wherein the daily necessity is selected from diapers, sanitary napkins, masks, protective clothing, and insoles; The daily necessities contain the essential oil-carrying zeolite molecular sieve according to any one of claims 1 to 6.

9. Use of the essential oil-carrying zeolite molecular sieve according to any one of claims 1 to 6 in the preparation of antibacterial drugs, skin care products, cosmetics, daily necessities, and fragrance products; Preferably, the antibacterial agent is anti-Escherichia coli, Staphylococcus aureus, and Candida albicans; Preferably, the daily necessities are selected from diapers, sanitary napkins, masks, protective clothing, and insoles.

10. A method for controlling the rate of essential oil release from the essential oil-carrying zeolite molecular sieve according to any one of claims 1 to 6 under high temperature and high humidity conditions, the method comprising coating the surface of the essential oil-carrying zeolite molecular sieve to control the amount of coating during the process of forming a coating layer, wherein the release rate is y, in units of % / min, x is the coating weight gain percentage, and the high temperature and high humidity are conditions of 36°C and 60% humidity; y = -0.0106x + 0.4803; The coating weight gain percentage is the percentage of the coating layer weight to the weight of the uncoated essential oil-carrying zeolite molecular sieve.

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