Preparation method of AgNPS-( SBA-15) molecular sieve antibacterial material and anti-deterioration treatment method of tobacco charging essence

Abstract

The invention discloses a preparation method of an AgNPS-(SBA-15) molecular sieve antibacterial material and an anti-deterioration treatment method of tobacco charging essence, and the preparation method of the AgNPS-(SBA-15) molecular sieve antibacterial material comprises the following steps: mixing 3-aminopropyltriethoxysilane and SBA-15 in a toluene solution, and placing in an oil bath for reflux stirring; performing suction filtration and washing; placing the filtered sample in a Soxhlet extractor, performing reflux extraction with dichloromethane, and performing vacuum drying to obtain pretreated SBA-15; dissolving silver nitrate in distilled water under the assistance of ultrasonic waves, and slowly dropwise adding ammonia water until a transparent solution is formed; and adding the pretreated SBA-15 molecular sieve, continuously stirring, adding stearic acid, stirring and dissolving, slowly adding a hydrazine hydrate solution into the solution, continuously reacting for 1 hour after dropwise adding, filtering, cleaning, and carrying out vacuum drying to obtain the AgNPS-(SBA-15) molecular sieve antibacterial material. The AgNPS-(SBA-15) molecular sieve antibacterial material provided by the invention can be used for quickly sterilizing the cigarette flavoring essence, so that the shelf life of the flavoring essence is prolonged, and the quality stability of the flavoring essence is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of tobacco, and in particular to an AgNP S -(SBA-15) molecular sieve antibacterial material preparation and tobacco flavoring anti-deterioration treatment method. Background Art

[0002] Nanosilver refers to single silver particles with a particle size of less than 100nm prepared by certain chemical or physical methods. Nanosilver antibacterial materials have the advantages of both inorganic antibacterial materials and nano antibacterial materials, with large specific surface area, high surface reactivity, and multiple surface active centers. Its antibacterial ability is more than 200 times that of micron-sized silver particles. However, due to its small particle size, AgNPs are prone to agglomeration when there is a lack of surfactants or stabilizers on the surface, and cannot exert good antibacterial activity. Therefore, it is necessary to compound nanosilver with a variety of antibacterial agents and carriers through physical adsorption or chemical grafting to improve its dispersibility.

[0003] Molecular sieve is a kind of aluminosilicate compound with cubic lattice, which has uniform microporous structure and uniform pore diameter. These pores can adsorb molecules smaller than their diameter into the pore cavity, and have preferential adsorption capacity for polar molecules and unsaturated molecules. Molecular sieve has been widely used because of its advantages that other adsorbents do not have, such as high adsorption capacity and strong thermal stability.

[0004] Tobacco flavoring mainly uses water as solvent system, and its main components are invert sugar and natural extracts. It is easy to undergo microbial fermentation, mildew, bubbles and other deterioration phenomena, which has become a potential threat to the stability of cigarette products. Flavoring is a heat-sensitive product. Excessive temperature will change the color and flavor of flavoring. Therefore, non-heating sterilization technology / low-temperature long-time cold sterilization technology is used to ensure product quality without changing the product flavor.

[0005] Therefore, the present invention aims to solve the problem that silver nanoparticles are prone to spontaneously aggregate into large particles and affect their antibacterial properties. S -(SBA-15) molecular sieve antibacterial material and its preparation method, and use the antibacterial material to quickly sterilize the added flavor to extend the shelf life of the added flavor and improve the quality stability of the added flavor. Summary of the invention

[0006] The technical problem to be solved by the present invention is to provide a AgNP S -(SBA-15) molecular sieve antibacterial material preparation and tobacco flavoring anti-deterioration treatment method, and apply it to tobacco flavoring for sterilization treatment, with the characteristics of simple operation, high efficiency and green, and can be used repeatedly, and the quality of the flavoring remains unchanged and stable after treatment.

[0007] The technical problem to be solved by the present invention is achieved through the following technical solutions:

[0008] A kind of AgNP S -(SBA-15) molecular sieve antibacterial material preparation method, comprising the following steps:

[0009] (1) Pretreatment of SBA-15 molecular sieve: 3-aminopropyltriethoxysilane and SBA-15 were mixed in a toluene solution, placed in an oil bath at 130-160°C and refluxed with stirring for 10-15 hours; filtered and washed with toluene; the filtered sample was placed in a Soxhlet extractor and refluxed with dichloromethane for 10-16 hours; filtered and vacuum dried to obtain pretreated SBA-15;

[0010] (2) AgNP S -(SBA-15) molecular sieve antibacterial material preparation: silver nitrate was dissolved in distilled water under the assistance of ultrasound, and ammonia water was slowly added until a transparent solution was formed; the pretreated SBA-15 molecular sieve was added and stirred for 30 minutes, stearic acid was added and stirred to dissolve, and hydrazine hydrate solution was slowly added to the above solution. After the addition was completed, the reaction was continued for 1 hour, filtered and washed with 95% ethanol, and vacuum dried to obtain AgNP S -(SBA-15) molecular sieve antibacterial material.

[0011] Preferably, in the above technical solution, in step (1), the mass ratio of 3-aminopropyltriethoxysilane and SBA-15 in toluene solution is 1:(10-15).

[0012] Preferably, in the above technical solution, in step (2), the molar ratio of silver nitrate to ammonia water is 1:(2.5-3).

[0013] Preferably, in the above technical solution, in step (2), the mass ratio of stearic acid to hydrazine hydrate solution is 1:(2-3).

[0014] Preferably, in the above technical solution, in step (2), the mass ratio of silver nitrate to pretreated SBA-15 molecular sieve is 1:(10-15).

[0015] A kind of AgNP S -(SBA-15) molecular sieve antibacterial material, the AgNP S -(SBA-15) molecular sieve antibacterial material is prepared according to the above preparation method.

[0016] A method using the above-mentioned AgNP S -(SBA-15) molecular sieve antibacterial material to prevent deterioration of tobacco flavoring essence, comprising the following steps:

[0017] S1. Prepare the added flavor according to the formula requirements of the cigarette flavor and fragrance product, pour the prepared added flavor into the stirring kettle and stir continuously for 30 minutes;

[0018] S2, AgNP S -(SBA-15) molecular sieve antibacterial material is filled into a homemade filter box, and the filter box is connected to the discharge pipeline port of the stirring tank;

[0019] S3. After the stirring is completed, open the discharge valve at the bottom of the stirring kettle, and pour the tobacco flavoring into the product packaging barrel through the filter box and store it in a sealed manner.

[0020] A kind of AgNP according to above S -Application of (SBA-15) molecular sieve antibacterial material in preventing tobacco flavoring from spoiling.

[0021] The above technical solution of the present invention has the following beneficial effects:

[0022] The AgNPs provided in this application S -(SBA-15) molecular sieve antibacterial material has a simple preparation method. This material can quickly sterilize tobacco flavors to extend the shelf life of flavors and improve the quality stability of flavors. It is also highly efficient, green and reusable. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.

[0024] Figure 1 For the AgNP of this application S -Schematic diagram of the usage status of (SBA-15) molecular sieve antibacterial material. DETAILED DESCRIPTION

[0025] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that the relative arrangement of components and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present invention unless otherwise specifically stated.

[0026] Unless otherwise specified, the reagents used in this application are all commercially available or obtained through commercial channels, or can be prepared by referring to existing chemical methods.

[0027] Example 1

[0028] A kind of AgNP S -(SBA-15) molecular sieve antibacterial material preparation method, comprising the following steps:

[0029] (1) SBA-15 molecular sieve pretreatment:

[0030] 3-aminopropyltriethoxysilane and SBA-15 were mixed in a toluene solution with a mass ratio of 1:10; the mixture was placed in an oil bath at 130°C with reflux and stirring for 10 hours; the mixture was filtered and washed with toluene; the filtered sample was placed in a Soxhlet extractor and refluxed with dichloromethane for 10 hours; the mixture was filtered and dried under vacuum to obtain the pretreated SBA-15.

[0031] (2) AgNP S -(SBA-15) molecular sieve antibacterial material preparation:

[0032] Silver nitrate was dissolved in distilled water with the assistance of ultrasound, and ammonia water was slowly added until a transparent solution was formed, and the molar ratio of silver nitrate to ammonia water was 1:2.5; the pretreated SBA-15 molecular sieve was added and continued to be stirred for 30 minutes, stearic acid was added and stirred to dissolve, and hydrazine hydrate solution was slowly added to the above solution, and the mass ratio of stearic acid to hydrazine hydrate solution was 1:3; after the addition was completed, the reaction was continued for one hour, filtered and washed with 95% ethanol, and vacuum dried to obtain AgNP S -(SBA-15) molecular sieve antibacterial material. The mass ratio of silver nitrate to pretreated SBA-15 molecular sieve is 1:10.

[0033] Sterilization treatment in tobacco flavoring (anti-deterioration treatment method):

[0034] S1. Prepare Hongqiqu (Hard Silver) flavoring essence (provided by Henan China Tobacco Zhumadian Cigarette) according to the formula requirements of cigarette flavors and fragrances, pour the prepared flavoring essence into a stirring kettle and stir continuously for 30 minutes;

[0035] S2, AgNP S -(SBA-15) molecular sieve antibacterial material is filled into the homemade filter box, and the filter box is connected to the outlet pipeline port of the stirring tank (such as Figure 1 );

[0036] S3. After the stirring is completed, open the discharge valve at the bottom of the stirring kettle, and pour the added flavor into the product packaging barrel through the filter box and seal it for storage. Take a sample and mark it as added flavor 1#.

[0037] Example 2

[0038] A kind of AgNP S -(SBA-15) molecular sieve antibacterial material preparation method, comprising the following steps:

[0039] (1) SBA-15 molecular sieve pretreatment:

[0040] 3-aminopropyltriethoxysilane and SBA-15 were mixed in a toluene solution, with the mass ratio of 3-aminopropyltriethoxysilane and SBA-15 in the toluene solution being 1:15; the mixture was placed in an oil bath at 160°C and refluxed with stirring for 15 hours; the mixture was filtered and washed with toluene; the filtered sample was placed in a Soxhlet extractor and refluxed with dichloromethane for 16 hours; the mixture was filtered and vacuum dried to obtain the pretreated SBA-15.

[0041] (2) AgNP S -(SBA-15) molecular sieve antibacterial material preparation:

[0042] Silver nitrate was dissolved in distilled water with the assistance of ultrasound, and ammonia water was slowly added until a transparent solution was formed, and the molar ratio of silver nitrate to ammonia water was 1:3; the pretreated SBA-15 molecular sieve was added and continued to be stirred for 30 minutes, stearic acid was added and stirred to dissolve, and hydrazine hydrate solution was slowly added to the above solution, and the mass ratio of stearic acid to hydrazine hydrate solution was 1:2; after the addition was completed, the reaction was continued for one hour, filtered and washed with 95% ethanol, and vacuum dried to obtain AgNP S -(SBA-15) molecular sieve antibacterial material. The mass ratio of silver nitrate to pretreated SBA-15 molecular sieve is 1:15.

[0043] Sterilization treatment in tobacco flavoring (anti-deterioration treatment method):

[0044] S1. Prepare Hongqiqu (Hard Silver) flavoring essence (provided by Henan China Tobacco Zhumadian Cigarette) according to the formula requirements of cigarette flavors and fragrances, pour the prepared flavoring essence into a stirring kettle and stir continuously for 30 minutes;

[0045] S2, AgNP S -(SBA-15) molecular sieve antibacterial material is filled into the homemade filter box, and the filter box is connected to the outlet pipeline port of the stirring tank (such as Figure 1 );

[0046] S3. After the stirring is completed, open the discharge valve at the bottom of the stirring kettle, and pour the added flavor into the product packaging barrel through the filter box and seal it for storage. Take a sample and mark it as added flavor 2#.

[0047] Example 3

[0048] A kind of AgNP S -(SBA-15) molecular sieve antibacterial material preparation method, comprising the following steps:

[0049] (1) SBA-15 molecular sieve pretreatment:

[0050] 3-aminopropyltriethoxysilane and SBA-15 were mixed in a toluene solution, with the mass ratio of 3-aminopropyltriethoxysilane and SBA-15 in the toluene solution being 1:10; the mixture was placed in an oil bath at 140°C and refluxed with stirring for 12 hours; the mixture was filtered and washed with toluene; the filtered sample was placed in a Soxhlet extractor and refluxed with dichloromethane for 15 hours; the mixture was filtered and vacuum dried to obtain the pretreated SBA-15.

[0051] (2) AgNP S -(SBA-15) molecular sieve antibacterial material preparation:

[0052] Silver nitrate was dissolved in distilled water with the assistance of ultrasound, and ammonia water was slowly added until a transparent solution was formed, and the molar ratio of silver nitrate to ammonia water was 1:3; the pretreated SBA-15 molecular sieve was added and continued to be stirred for 30 minutes, stearic acid was added and stirred to dissolve, and hydrazine hydrate solution was slowly added to the above solution, and the mass ratio of stearic acid to hydrazine hydrate solution was 1:2.5; after the addition was completed, the reaction was continued for one hour, filtered and washed with 95% ethanol, and vacuum dried to obtain AgNP S -(SBA-15) molecular sieve antibacterial material. The mass ratio of silver nitrate to pretreated SBA-15 molecular sieve is 1:15.

[0053] Sterilization treatment in tobacco flavoring (anti-deterioration treatment method):

[0054] S1. Prepare Hongqiqu (Hard Silver) flavoring essence (provided by Henan China Tobacco Zhumadian Cigarette) according to the formula requirements of cigarette flavors and fragrances, pour the prepared flavoring essence into a stirring kettle and stir continuously for 30 minutes;

[0055] S2, AgNP S -(SBA-15) molecular sieve antibacterial material is filled into the homemade filter box, and the filter box is connected to the outlet pipeline port of the stirring tank (such as Figure 1 );

[0056] S3. After the stirring is completed, open the discharge valve at the bottom of the stirring kettle, and pour the added flavor into the product packaging barrel through the filter box and seal it for storage. Take a sample and mark it as added flavor 3#.

[0057] Of course, the added flavors of the present application may also adopt the flavor and fragrance formula of the heated cigarette formula commonly used in the art, and are not limited to the above-mentioned products. The present application only uses this as an example for experimental description.

[0058] The added flavors prepared in Examples 1 to 3 were added to the cigarette shreds by spraying at a ratio of 2.65wt% in the adding process, and were recorded as cigarettes 1#, 2# and 3#; at the same time, the shredded tobacco added with the control sample added with flavors and fragrances was used as a blank control group, recorded as the control sample; cigarette products were made by conventional methods in the art, and the moisture was balanced (humidity 60%±2%, temperature 25±1°C) for 24h, and then sensory evaluation was carried out according to "YC / T 415-2011 Sensory Evaluation Method for Tobacco Products", and the results are shown in Table 1.

[0059] Table 1 Results of sensory quality evaluation of cigarettes

[0060]

[0061] It can be seen from the evaluation results in Table 1 that the present invention S -When the flavoring treated with (SBA-15) molecular sieve antibacterial material is added to cigarettes, the aroma quality and aftertaste of the cigarettes are slightly improved, while other indicators remain unchanged, indicating that the intrinsic quality of the flavoring treated has not changed and the product quality is stable.

[0062] The added flavors prepared in Examples 1 to 3 and the untreated control samples were placed in a constant temperature and humidity chamber, and the changes of the four samples over the storage time were observed. The results are shown in Table 2.

[0063] Table 2 Changes of added flavors

[0064]

[0065]

[0066] It can be seen from Table 2 that the AgNPs of the present invention S -(SBA-15) molecular sieve antibacterial material treated flavoring, its shelf life is much longer than untreated flavoring, improving product quality stability.

[0067] Although the present invention has been disclosed as above by the embodiments, it is not intended to limit the present invention. Any person skilled in the art may make various choices and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention is limited by the claims and their equivalents.

Claims

1. A kind of AgNP S -(SBA-15) molecular sieve antibacterial material preparation method, characterized in that, The following steps are involved: (1) Pretreatment of SBA-15 molecular sieve: 3-aminopropyltriethoxysilane and SBA-15 were mixed in a toluene solution, placed in an oil bath at 130-160°C and refluxed with stirring for 10-15 hours; filtered and washed with toluene; the filtered sample was placed in a Soxhlet extractor and refluxed with dichloromethane for 10-16 hours; filtered and vacuum dried to obtain pretreated SBA-15; (2) AgNP S -(SBA-15) molecular sieve antibacterial material preparation: silver nitrate was dissolved in distilled water under the assistance of ultrasound, and ammonia water was slowly added until a transparent solution was formed; the pretreated SBA-15 molecular sieve was added and stirred for 30 minutes, stearic acid was added and stirred to dissolve, and hydrazine hydrate solution was slowly added to the above solution. After the addition was completed, the reaction was continued for 1 hour, filtered and washed with 95% ethanol, and vacuum dried to obtain AgNP S -(SBA-15) molecular sieve antibacterial material.

2. AgNP according to claim 1 S -(SBA-15) molecular sieve antibacterial material preparation method, characterized in that, In step (1), the mass ratio of 3-aminopropyltriethoxysilane to SBA-15 in toluene solution is 1:(10-15).

3. AgNP according to claim 1 S -(SBA-15) molecular sieve antibacterial material preparation method, characterized in that, In step (2), the molar ratio of silver nitrate to ammonia water is 1:(2.5-3).

4. AgNP according to claim 1 S -(SBA-15) molecular sieve antibacterial material preparation method, characterized in that, In step (2), the mass ratio of stearic acid to hydrazine hydrate solution is 1:(2-3).

5. AgNP according to claim 1 S -(SBA-15) molecular sieve antibacterial material preparation method, characterized in that, In step (2), the mass ratio of the silver nitrate solution to the pretreated SBA-15 molecular sieve is 1:(10-15).

6. A kind of AgNP S -(SBA-15) molecular sieve antibacterial material, characterized in that, The AgNP S -(SBA-15) molecular sieve antibacterial material is prepared according to any preparation method described in claims 1-5.

7. A method using the AgNP according to claim 6 S -(SBA-15) molecular sieve antibacterial material to prevent deterioration of tobacco flavoring, characterized in that: The following steps are involved: S1. Prepare the added flavor according to the formula requirements of the cigarette flavor and fragrance product, pour the prepared added flavor into the stirring kettle and stir continuously for 30 minutes; S2, AgNP S -(SBA-15) molecular sieve antibacterial material is filled into a homemade filter box, and the filter box is connected to the discharge pipeline port of the stirring tank; S3. After the stirring is completed, open the discharge valve at the bottom of the stirring kettle, and pour the tobacco flavoring into the product packaging barrel through the filter box and seal it for storage.

8. An AgNP according to claim 6 S -Application of (SBA-15) molecular sieve antibacterial material in preventing tobacco flavoring from spoiling.

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