Tobacco essence and perfume antibacterial material and preparation method thereof

Abstract

The invention discloses a tobacco flavor and perfume antibacterial material and a preparation method thereof, the tobacco flavor and perfume antibacterial material comprises an antibacterial active component and a carrier material, and the antibacterial active component is loaded on the carrier material; the antibacterial active component is Fe-coated Ag nanoparticles with Fe as a core and Ag as a shell, the mass fraction of Ag in the nano antibacterial material is 0.02%-2%, and the mass fraction of Fe is 0.5%-10%. The tobacco flavor and perfume antibacterial material provided by the invention can continuously exert an antibacterial effect, and is safe, non-toxic, low in content of effective antibacterial components, lasting in antibacterial property and convenient to recycle and reuse.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of essence and flavor antibacterial materials, and particularly relates to a tobacco essence and flavor antibacterial material and a preparation method thereof. BACKGROUND

[0002] Essence and flavor account for a rising proportion in the fine chemical industry year by year, and the use of tobacco essence and flavor accounts for 12% of the market share. Tobacco essence and flavor is an important raw material in the production and processing of cigarettes, which is composed of various flavors, appropriate solvents and other ingredients, and has the functions of improving tobacco odor, increasing toughness and improving combustion, and is related to the formation of the characteristic flavor of a cigarette brand. However, the essence and flavor contains a large amount of water and sugar and other substances, which is easy to be contaminated by microorganisms and cause phenomena such as sour smell and short shelf life, causing serious economic losses to enterprises.

[0003] Antibacterial agents are generally divided into inorganic antibacterial agents, organic antibacterial agents and natural antibacterial agents. The inorganic antibacterial agent utilizes the antibacterial ability of silver, copper and zinc metals, has a series of advantages such as broad-spectrum antibacterial, high temperature resistance, strong durability, excellent biocompatibility and degradation of formaldehyde, and is widely used in food, medicine, fabric, building materials, coatings and other fields. The bactericidal ability of silver in inorganic antibacterial agents is the strongest, which mainly produces antibacterial ability through the following ways: destroying cell wall / cell membrane, inhibiting bacterial respiratory chain, inducing genetic toxicity, inducing active oxygen free radicals, and inducing light catalytic protein damage.

[0004] Chinese patent 200410068909.7 discloses a preparation method and application of silver-loaded activated carbon. The silver-loaded activated carbon has the characteristics of simple process, small amount of impurity ions introduced, and is suitable for industrial scale production. The bactericidal agent and medical antibacterial material prepared by using the silver-loaded activated carbon can be applied to the preparation of sterilizing agents and medical antibacterial materials, including antibacterial machine woven cloth, non-woven fabric, felt and fiber and surgical dressings. Chinese patent 202110378195.3 discloses a preparation method of nano-titanium dioxide photocatalytic antibacterial material. The carbonized cigarette filter is obtained by high-temperature calcination of a cigarette filter, the carbonized cigarette filter is immersed in a titanium dioxide growth solution and stirred, the soaked carbonized cigarette filter is placed under high temperature and high pressure for reaction and then cooled, and the reaction product is washed and dried to obtain the carbonized cigarette filter loaded with nano-TiO2 antibacterial material. The present application also discloses a nano-titanium dioxide photocatalytic antibacterial material and its application. The carbonized cigarette filter and nano-TiO2 are harmless to the human body, can cause oxidation-reduction reaction with E. coli to inactivate it, have high inactivation efficiency, and can be applied to the prevention of E. coli infection in the human body.

[0005] In order to improve the safety performance of the product, the antibacterial material should avoid introducing substances harmful to human body in the design and production as far as possible, and the molecular sieve and silica gel and other materials are composed of completely harmless substances, which are very suitable for application in the research and development design of antibacterial products of food and daily chemical products. The antibacterial material combines the metal silver and iron with antibacterial capacity with the base material such as molecular sieve or silica gel, which can not only be efficiently applied to the sterilization treatment of tobacco flavor and fragrance, but also can realize the convenient recovery of the antibacterial material. SUMMARY

[0006] The technical problem to be solved by the present application is to provide a tobacco flavor and fragrance antibacterial material and a preparation method thereof, Fe@Ag nanoparticles are used as antibacterial active components, and 3A molecular sieve, 13X molecular sieve, alumina ball, activated carbon ball, silica gel ball and the like are used as carrier materials, and the tobacco flavor and fragrance antibacterial material is prepared by an impregnation process, so that an antibacterial material with excellent sterilization effect and convenient separation from flavor and fragrance is obtained, the antibacterial material preparation process is simple, and has good practical application prospect.

[0007] The technical problem to be solved by the present application is solved by the following technical scheme:

[0008] A tobacco flavor and fragrance antibacterial material, comprising an antibacterial active component and a carrier material, wherein the antibacterial active component is carried on the carrier material; the antibacterial active component is Fe@Ag nanoparticles with Fe as the core and Ag as the shell, wherein the mass fraction of Ag in the nano antibacterial material is 0.02%-2%, and the mass fraction of Fe is 0.5%-10%.

[0009] Preferably, in the above technical scheme, the carrier material is selected from at least one of 3A molecular sieve, 4A molecular sieve, 13X molecular sieve, alumina ball, activated carbon ball and silica gel ball.

[0010] Preferably, in the above technical scheme, the Ag is derived from a soluble Ag salt, and the Fe is derived from a soluble metal Fe salt.

[0011] Preferably, in the above technical scheme, the Ag salt is selected from at least one of silver nitrate, silver diamminonitrate and silver sulfate; and the Fe salt is selected from at least one of ferric chloride hexahydrate, ferric nitrate nonahydrate and ferric sulfate nonahydrate.

[0012] A preparation method of a tobacco flavor and fragrance antibacterial material, comprising the following steps:

[0013] (1) Fe@Ag NPs preparation:

[0014] A certain amount of soluble Ag salt and soluble Fe salt are dispersed in an appropriate amount of oleylamine and tri-n-octylphosphine at room temperature;

[0015] The mixed solution is heated to 245 DEG C at a temperature increasing rate of 5 DEG C / min under an argon atmosphere and kept for 60 min, and the solution color changes;

[0016] Isopropanol is added to the above mixed solution, and the nanoparticles containing impurities are separated by centrifugation;

[0017] The nanoparticles are redispersed and purified in a mixed solution of n-hexane, ethanol and isopropanol to obtain an antibacterial active component (Fe@Ag NPs);

[0018] (2) Preparation of an antibacterial material for tobacco flavoring and perfuming materials:

[0019] The Fe@Ag NPs are dispersed in ethanol, a certain amount of carrier material is added to the above mixed solution, and the solution is impregnated under microwave conditions for 20-40 min to obtain an antibacterial material for tobacco flavoring and perfuming materials.

[0020] Preferably, in the above technical solution, the carrier material is selected from at least one of 3A molecular sieve, 4A molecular sieve, 13X molecular sieve, alumina ball, activated carbon ball and silica gel ball.

[0021] Preferably, in the above technical solution, the molar ratio of Ag to Fe is 1:10-1:20, and the volume ratio of oleylamine to tri-n-octylphosphine is 20:0.3.

[0022] Preferably, in the above technical solution, the amount of isopropanol is 1-3 times that of the mixed solution, and the volume ratio of n-hexane, ethanol and isopropanol is 1:(0.5-2):(0.5-1).

[0023] Preferably, in the above technical solution, the impregnation temperature is 20 DEG C, 40 DEG C, 60 DEG C or 80 DEG C, and the impregnation time is 8 h, 10 h or 12 h.

[0024] The above technical solution of the present application has the following beneficial effects:

[0025] The antibacterial material for tobacco flavoring and perfuming materials provided in the present application can continuously exert antibacterial effect, is safe and non-toxic, has low content of effective antibacterial components, has durable antibacterial property and is convenient for recycling and reuse. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 The scanning electron microscope (SEM) image of the antibacterial material for tobacco flavoring and perfuming materials. DETAILED DESCRIPTION

[0027] Various exemplary embodiments of the present application will now be described in detail. It should be noted that the relative arrangement of components and steps, numerical expressions, and numerical values set forth in these embodiments are not intended to limit the scope of the present application unless otherwise specifically stated.

[0028] The experimental methods used in the following examples are conventional methods, and the materials and reagents used are commercially available unless otherwise specified. The equipment used in the experiments is well known to those skilled in the art unless otherwise specified.

[0029] Example 1

[0030] First, 0.0786 g of silver nitrate and 2.4134 g of iron chloride hexahydrate were dispersed in 20 ml of oleylamine and 0.3 ml of tri-n-octylphosphine at room temperature;

[0031] Second, the mixed solution was heated to 245°C at a heating rate of 5°C / min under an argon atmosphere and maintained for 60 min, and the color of the solution changed;

[0032] Then, isopropyl alcohol (1-3 times the amount of the mixed solution) was added to the above mixture, and the impurity-containing nanoparticles were separated by centrifugation;

[0033] Finally, the antibacterial active component (Fe@Ag NPs) was obtained by redispersion and purification in a mixed solution of n-hexane, ethanol, and isopropyl alcohol (volume ratio of 1:(0.5-2):(0.5-1)) and was ready for use.

[0034] The antibacterial active component (Fe@Ag NPs) was dispersed in ethanol, 10.0 g of 3A molecular sieves was added to the above mixture, and the mixture was immersed at 20°C for 12 h to obtain the tobacco flavoring material.

[0035] Example 2

[0036] First, 0.0786 g of silver nitrate and 2.4134 g of iron chloride hexahydrate were dispersed in 20 ml of oleylamine and 0.3 ml of tri-n-octylphosphine at room temperature;

[0037] Second, the mixed solution was heated to 245°C at a heating rate of 5°C / min under an argon atmosphere and maintained for 60 min, and the color of the solution changed;

[0038] Then, isopropyl alcohol (1-3 times the amount of the mixed solution) was added to the above mixture, and the impurity-containing nanoparticles were separated by centrifugation;

[0039] Finally, the antibacterial active component (Fe@Ag NPs) was obtained by redispersion and purification in a mixed solution of n-hexane, ethanol, and isopropyl alcohol (volume ratio of 1:(0.5-2):(0.5-1)) and was ready for use.

[0040] The antibacterial active component (Fe@Ag NPs) is dispersed in ethanol, 10.0 g of 4A molecular sieve is added to the above mixture, and the mixture is soaked at 40℃ for 12 h to obtain the tobacco flavoring material with antibacterial activity.

[0041] Example 3

[0042] First, 0.0786 g of silver nitrate and 3.5704 g of iron sulfate heptahydrate are dispersed in 20 ml of oleylamine and 0.3 ml of tri-n-octylphosphine at room temperature;

[0043] Secondly, the mixed solution is heated to 245℃ at a heating rate of 5℃ / min under an argon atmosphere and kept for 60 min, and the color of the solution changes;

[0044] Then, isopropyl alcohol (1-3 times the amount of the mixture) is added to the above mixture, and the impurity-containing nanoparticles are separated by centrifugation;

[0045] Finally, the antibacterial active component (Fe@Ag NPs) is dispersed and purified in a mixed solution of n-hexane, ethanol and isopropyl alcohol (volume ratio 1:(0.5-2):(0.5-1)) for standby.

[0046] The antibacterial active component (Fe@Ag NPs) is dispersed in ethanol, 10.0 g of 4A molecular sieve is added to the above mixture, and the mixture is soaked at 40℃ for 12 h to obtain the tobacco flavoring material with antibacterial activity.

[0047] Example 4

[0048] First, 0.0786 g of silver nitrate and 2.4134 g of iron chloride hexahydrate are dispersed in 20 ml of oleylamine and 0.3 ml of tri-n-octylphosphine at room temperature;

[0049] Secondly, the mixed solution is heated to 245℃ at a heating rate of 5℃ / min under an argon atmosphere and kept for 60 min, and the color of the solution changes;

[0050] Then, isopropyl alcohol is added to the above mixture, and the impurity-containing nanoparticles are separated by centrifugation;

[0051] Finally, the antibacterial active component (Fe@Ag NPs) is dispersed and purified in a mixed solution of n-hexane, ethanol and isopropyl alcohol for standby.

[0052] The antibacterial active component (Fe@Ag NPs) is dispersed in ethanol, 10.0 g of 4A molecular sieve is added to the above mixture, and the mixture is soaked at 40℃ for 12 h to obtain the tobacco flavoring material with antibacterial activity.

[0053] Application Example 1

[0054] First, 1 / 4 of the tobacco flavoring antibacterial material is loaded in the treatment tank, secondly, the prepared tobacco flavoring is added into the treatment tank, stirred for 1h, and then placed for 1h; then, the tobacco flavoring is separated out for antibacterial test, and the antibacterial results of yeast and mold are shown in Tables 1 and 2; finally, the nanometer antibacterial material is recycled for reuse, and the antibacterial performance of the antibacterial material when reused is shown in Table 3.

[0055] Table 1: Test results of nanometer antibacterial material

[0056]

[0057]

[0058] Table 2: Test results of nanometer antibacterial material

[0059]

[0060] Table 3: Cycle test results of nanometer antibacterial material

[0061]

[0062] From Tables 1-3, it can be seen that the tobacco flavoring antibacterial material has a significant antibacterial effect on yeast and mold, and the antibacterial rate reaches 99.9% in 48 hours; and after 20 cycles, the antibacterial rate on mold still reaches 99.8%, showing excellent and durable antibacterial performance, and good reusability.

[0063] Although the present application has been disclosed as above with examples, it is not intended to limit the present application, and any person skilled in the art can make various selections and modifications without departing from the spirit and scope of the present application, and therefore the protection scope of the present application is defined by the claims and equivalent forms thereof.

Claims

1. A tobacco flavourant antibacterial material characterised in that, The antibacterial active component and the carrier material, the antibacterial active component is carried on the carrier material; the antibacterial active component is Fe@Ag nanoparticles with Fe as the core and Ag as the shell, wherein the mass fraction of Ag in the nano-antibacterial material is 0.02%-2%, and the mass fraction of Fe is 0.5%-10%.

2. A tobacco flavourant antimicrobial material according to claim 1 characterised in that, The carrier material is selected from at least one of 3A molecular sieve, 4A molecular sieve, 13X molecular sieve, alumina ball, activated carbon ball and silica gel ball.

3. The tobacco flavourant antimicrobial material of claim 1, wherein, The Ag is derived from a soluble Ag salt, and the Fe is derived from a soluble metal Fe salt.

4. A tobacco flavourant antimicrobial material according to claim 3, characterised in that, The Ag salt is selected from at least one of silver nitrate, silver diamminonitrate and silver sulfate; and the Fe salt is selected from at least one of ferric chloride hexahydrate, ferric nitrate nonahydrate and ferric sulfate nonahydrate.

5. A method of preparing a tobacco flavourant antibacterial material according to any one of claims 1 to 4, characterised in that, The method comprises the following steps: (1) Fe@Ag NPs preparation: A certain amount of soluble Ag salt and soluble Fe salt are dispersed in an appropriate amount of oleylamine and tri-n-octylphosphine at room temperature; The mixed solution is heated to 245 DEG C at a heating rate of 5 DEG C / min under an argon atmosphere and kept for 60 min, and the solution color changes; Isopropyl alcohol is added to the above mixed solution to centrifugally separate the nanoparticles containing impurities; The nanoparticles are redispersed and purified in a mixed solution of n-hexane, ethanol and isopropyl alcohol to obtain the antibacterial active component (Fe@Ag NPs); (2) Preparation of tobacco flavoring antibacterial material: The Fe@Ag NPs are dispersed in ethanol, a certain amount of carrier material is added to the above mixed solution, and the mixture is immersed under microwave conditions for 20-40 min to obtain the tobacco flavoring antibacterial material.

6. The preparation method according to claim 5, characterized in that, The carrier material is selected from at least one of 3A molecular sieve, 4A molecular sieve, 13X molecular sieve, alumina ball, activated carbon ball and silica gel ball.

7. The preparation method according to claim 5, characterized in that, The molar ratio of Ag to Fe is 1:10-1:20; and the volume ratio of oleylamine to tri-n-octylphosphine is 20:0.

3.

8. The preparation method according to claim 5, characterized in that, The amount of isopropyl alcohol is 1-3 times that of the mixed solution; and the volume ratio of n-hexane, ethanol and isopropyl alcohol is 1:(0.5-2):(0.5-1).

9. The preparation method according to claim 5, characterized in that, The immersion temperature is 20 DEG C, 40 DEG C, 60 DEG C or 80 DEG C; and the immersion time is 8 h, 10 h or 12 h.

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