Preparation of silver-loaded glass antibacterial material and application of silver-loaded glass antibacterial material in tobacco flavors and fragrances

Abstract

The invention discloses preparation of a silver-loaded glass antibacterial material and application of the silver-loaded glass antibacterial material in tobacco flavors and fragrances, the silver-loaded glass antibacterial material comprises a glass powder material, a silver-loaded molecular sieve material and a binder, the mass ratio of the glass powder material to the silver-loaded molecular sieve material to the binder is (85-90): (10-15): (5-10), and the preparation method of the silver-loaded glass antibacterial material comprises the following steps: (1) preparing the glass powder material; (2) preparing a silver-loaded molecular sieve material; and (3) preparing the silver-loaded glass antibacterial material. In the silver-loaded glass antibacterial material, the metal silver is uniformly dispersed on the surface of the glass material, and the molecular sieve provides a metal silver loading site effect, so that the antibacterial effect can be continuously exerted. The silver-loaded glass antibacterial material disclosed by the invention is suitable for tobacco flavors and fragrances, is safe and non-toxic, has lasting antibacterial property and is convenient to recycle and reuse.

Description

Technical Field

[0001] The invention relates to the technical field of tobacco flavors and fragrances, and in particular to the preparation of a silver-loaded glass antibacterial material and the application of the silver-loaded glass antibacterial material in tobacco flavors and fragrances. Background Art

[0002] With the rapid economic development of countries around the world, consumption levels have also been continuously improving, and the flavor and fragrance industry has also developed rapidly. The sales of flavors and fragrances account for an increasingly large proportion of the world's fine chemical industry, among which the use of tobacco flavors and fragrances accounts for 12% of the market share. Tobacco flavors are made of a variety of spices, appropriate amounts of solvents and other ingredients. They are important raw materials in the production and processing of cigarettes. They have the functions of improving tobacco odor, increasing toughness and improving combustion, and are related to the composition of the characteristic flavor of cigarette brands. However, because added flavors contain a large amount of water and sugars and other substances, their quality stability is poor and difficult to control. They are easily contaminated by microorganisms and produce sourness and odor, which shortens the shelf life and causes serious economic losses to companies.

[0003] Antimicrobial agents are generally divided into inorganic antimicrobial agents, organic antimicrobial agents and natural antimicrobial agents. Inorganic antimicrobial agents use the antimicrobial ability of metals such as silver, copper and zinc. They have a series of advantages such as broad-spectrum antimicrobial, high temperature resistance, strong durability, excellent biocompatibility and formaldehyde degradation. They are widely used in various fields such as food, medicine, fabrics, building materials, and coatings. Among inorganic antimicrobial agents, silver has the strongest bactericidal ability, which mainly produces antimicrobial ability by destroying cell walls / cell membranes, inhibiting bacterial respiratory chains, inducing genetic toxicity, inducing reactive oxygen free radicals, and inducing photocatalytic protein damage.

[0004] In order to improve the safety performance of products, antibacterial materials should avoid introducing harmful substances to the human body as much as possible during design and production. Glass materials are composed of completely harmless substances, which makes them very suitable for use in the research and development of antibacterial products for food and daily necessities. Silver-loaded glass antibacterial materials combine metallic silver with glass base materials, and can achieve convenient recycling of antibacterial materials on the basis of being able to sterilize tobacco flavors and fragrances. Summary of the invention

[0005] The technical problem to be solved by the present invention is to provide a preparation method of a silver-loaded glass antibacterial material and its application in tobacco flavors and fragrances, which overcomes the disadvantage that tobacco flavors and fragrances have a shortened shelf life due to microbial contamination. The present application uses glass material as a carrier of metallic silver, and is expected to obtain an antibacterial material with excellent bactericidal effect, no harm, and easy to separate from flavors and fragrances.

[0006] The technical problem to be solved by the present invention is achieved through the following technical solutions:

[0007] A silver-loaded glass antibacterial material comprises a glass powder material, a silver-loaded molecular sieve material and a binder, wherein the mass ratio of the three is (85-90):(10-15):(5-10). The silver-loaded glass antibacterial material is prepared by uniformly mixing the glass powder material, the silver-loaded molecular sieve material and the binder, grinding the mixture and feeding it into a granulator for extrusion molding.

[0008] Preferably, in the above technical solution, the granulator pressure is 30-50Mpa, maintained for 5-10min, and the binder is pseudo-boehmite with a moisture content of 8±2%.

[0009] A method for preparing a silver-loaded glass antibacterial material comprises the following steps:

[0010] (1) Preparation of glass powder material: SiO2, Al2O3 and Na2O3 are placed in a mixer according to a certain mass ratio and mixed evenly to obtain a mixture; the mixture is added to a high temperature device, heated to 1400°C and calcined for 2-3 hours to obtain a melt; after the melt is mixed evenly, the melt is quenched with water to obtain a glass body; after the glass body is dried, it is placed in a ball mill for ball milling, and sieved to obtain a glass powder material;

[0011] (2) Preparation of silver-loaded molecular sieve material: The molecular sieve and silver nitrate solution are uniformly mixed, and the temperature is raised to 500° C. and calcined for 1-2 hours in a high-temperature device under the protection of an inert gas to obtain the silver-loaded molecular sieve material;

[0012] (3) Preparation of silver-loaded glass antibacterial material: After the glass powder material, silver-loaded molecular sieve material and binder are fully and evenly ground, they are prepared into spherical particles in a granulator to obtain the silver-loaded glass antibacterial material.

[0013] Preferably, in the above technical solution, in step (1), the mass ratio of silicon dioxide, aluminum oxide and sodium oxide is (85-95): (10-30): (5-15).

[0014] Preferably, in the above technical solution, in step (1), the mixed material is added into a high temperature device, and the heating program is: 25-1400°C, 150-250min, and constant temperature for 80-120min; the water used for water quenching is deionized water.

[0015] Preferably, in the above technical solution, in step (1), the ball milling process is as follows: add 1 part of the glass powder material, 2 parts of deionized water, and 10 parts of grinding balls into a ball mill, and ball mill at a speed of 300-600r / min for 2-4h.

[0016] Preferably, in the above technical scheme, in step (2), the molecular sieve is a mesoporous molecular sieve with a particle size less than 100 mesh and a pore size of 30-60 nm; the concentration of the silver nitrate solution is 0.2-0.9 mol / L, and the volume ratio of the molecular sieve to the silver nitrate solution is 1:(10-20); the heating program is: 25-120°C, 90-100 min, constant temperature 20-30 min; 120-500°C, 180-220 min, insulation 70-110 min; the inert gas is nitrogen with a purity greater than 99.9%.

[0017] Preferably, in the above technical solution, in step (3), the mass ratio of the glass powder material, the silver-loaded molecular sieve material and the binder is (85-90):(10-15):(5-10); and the binder is pseudo-boehmite.

[0018] A preparation method of a silver-loaded glass antibacterial material and its application in tobacco flavors. The silver-loaded glass antibacterial material is a silver-loaded glass antibacterial material prepared according to the preparation method.

[0019] An application of silver-loaded glass antibacterial material in tobacco flavors, the application is as follows: the tobacco flavors and fragrances prepared according to the product formula are transferred into a turnover tank, 1 / 4 volume of silver-loaded glass antibacterial material microspheres are loaded into the tank, stirred for 0.5-1h, and then left to stand for more than 1h. The processed finished tobacco flavors and fragrances are then poured into the finished product tank to complete the sterilization.

[0020] The above technical solution of the present invention has the following beneficial effects:

[0021] In the silver-loaded glass antibacterial material of the present invention, metallic silver is evenly dispersed on the surface of the glass material, and the molecular sieve provides the role of loading metallic silver sites, which can continuously exert the antibacterial effect.

[0022] The silver-loaded glass antibacterial material of the invention is suitable for tobacco flavors and fragrances, is safe and non-toxic, has a lasting antibacterial property and is easy to recycle and reuse. DETAILED DESCRIPTION

[0023] Various exemplary embodiments of the present invention 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 do not limit the scope of the present invention unless specifically stated otherwise.

[0024] 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.

[0025] Example 1

[0026] (1) Preparation of silver-loaded glass antibacterial material:

[0027] In parts by weight, 85 parts of silicon dioxide, 30 parts of aluminum oxide, and 15 parts of sodium oxide are mixed, put into a blender and mixed evenly to obtain a mixture; the mixture is added into a high-temperature device, heated to 1400°C and calcined for 2 hours to obtain a melt, and after the melt is mixed evenly, the melt is water quenched and cooled to obtain a glass body; after the glass body is dried, it is put into a ball mill and ball-milled at a speed of 300 r / min for 4 hours, and the glass powder material is obtained after sieving.

[0028] By volume, 1 part of molecular sieve is uniformly mixed with 15 parts of silver nitrate solution, and the mixture is heated to 500° C. and calcined for 1 hour in a high-temperature device under the protection of an inert gas to obtain a silver-loaded molecular sieve material.

[0029] By weight, 90 parts of glass powder material, 10 parts of silver-loaded molecular sieve material and 5 parts of binder are fully ground and uniformly prepared into spherical particles in a granulator to obtain the silver-loaded glass antibacterial material.

[0030] (2) Antibacterial pretreatment of tobacco flavors and fragrance solvents:

[0031] Solvents for preparing tobacco flavors and fragrances, such as water and propylene glycol, are pumped into solvent tanks respectively. Before entering the solvent tanks, they pass through a treatment tank loaded with silver-loaded glass antibacterial material microspheres at a treatment rate of 60-100 kg / min.

[0032] (3) Treatment of finished tobacco flavors and fragrances:

[0033] The finished golden leaf (mango) flavors and fragrances (provided by Henan China Tobacco Zhumadian Cigarette Factory) prepared according to the product formula were transferred into the turnover tank, and 1 / 4 volume of silver-loaded glass antibacterial material microspheres were placed in the tank. After stirring for 0.5-1h, it was left to stand for more than 1h. Then the treated finished tobacco flavors and fragrances were poured into the finished product tank. The treated finished tobacco flavors and fragrances were tested for antibacterial properties, and the results are shown in Table 1.

[0034] (4) Recycling of antibacterial materials:

[0035] The silver-loaded glass antibacterial material microspheres in the turnover tank are regularly filtered and recovered, ultrasonically cleaned with water and propylene glycol for 20-30 minutes respectively, and can be used again after drying.

[0036] Table 1 Antibacterial test results

[0037]

[0038] Example 2

[0039] (1) Preparation of silver-loaded glass antibacterial material:

[0040] In parts by weight, 95 parts of silicon dioxide, 10 parts of aluminum oxide, and 5 parts of sodium oxide are mixed, put into a blender and mixed evenly to obtain a mixture; the mixture is added into a high-temperature device, heated to 1400°C and calcined for 3 hours to obtain a melt, and after the melt is mixed evenly, the melt is water quenched and cooled to obtain a glass body; after the glass body is dried, it is put into a ball mill and ball-milled at a speed of 600 r / min for 2 hours, and the glass powder material is obtained after sieving.

[0041] By volume, 1 part of molecular sieve is uniformly mixed with 20 parts of silver nitrate solution, and the mixture is heated to 500° C. and calcined for 2 hours in a high-temperature device under the protection of an inert gas to obtain a silver-loaded molecular sieve material.

[0042] By weight, 85 parts of glass powder material, 15 parts of silver-loaded molecular sieve material and 10 parts of binder are fully ground and uniformly prepared into spherical particles in a granulator to obtain the silver-loaded glass antibacterial material.

[0043] (2) Antibacterial pretreatment of tobacco flavors and fragrance solvents:

[0044] Solvents for preparing tobacco flavors and fragrances, such as water and propylene glycol, are pumped into solvent tanks respectively. Before entering the solvent tanks, they pass through a treatment tank loaded with silver-loaded glass antibacterial material microspheres at a treatment rate of 60-100 kg / min.

[0045] (3) Treatment of finished tobacco flavors and fragrances:

[0046] The finished Golden Leaf (New Galaxy) flavors and fragrances (provided by Henan China Tobacco Zhumadian Cigarette Factory) prepared according to the product formula were transferred into the turnover tank, and 1 / 4 volume of silver-loaded glass antibacterial material microspheres were placed in the tank. After stirring for 0.5-1h, it was left to stand for more than 1h. Then the treated finished tobacco flavors and fragrances were poured into the finished product tank. The treated finished tobacco flavors and fragrances were tested for antibacterial properties, and the results are shown in Table 2.

[0047] (4) Recycling of antibacterial materials:

[0048] The silver-loaded glass antibacterial material microspheres in the turnover tank are regularly filtered and recovered, ultrasonically cleaned with water and propylene glycol for 20-30 minutes respectively, and can be used again after drying.

[0049] Table 2 Antibacterial test results

[0050]

[0051] Example 3

[0052] (1) Preparation of silver-loaded glass antibacterial material:

[0053] In parts by weight, 88 parts of silicon dioxide, 18 parts of aluminum oxide, and 12 parts of sodium oxide are mixed, put into a blender and mixed evenly to obtain a mixture; the mixture is added into a high-temperature device, heated to 1400°C and calcined for 2.5 hours to obtain a melt, and after the melt is mixed evenly, the melt is water quenched and cooled to obtain a glass body; after the glass body is dried, it is put into a ball mill and ball-milled at a speed of 500 r / min for 3 hours, and the glass powder material is obtained after sieving.

[0054] By volume, 1 part of molecular sieve is mixed evenly with 12 parts of silver nitrate solution, and the mixture is heated to 500° C. and calcined for 1.5 hours in a high-temperature device under the protection of an inert gas to obtain a silver-loaded molecular sieve material.

[0055] By weight, 87 parts of glass powder material, 13 parts of silver-loaded molecular sieve material and 8 parts of binder are fully ground and uniformly prepared into spherical particles in a granulator to obtain the silver-loaded glass antibacterial material.

[0056] (2) Antibacterial pretreatment of tobacco flavors and fragrance solvents:

[0057] Solvents for preparing tobacco flavors and fragrances, such as water and propylene glycol, are pumped into solvent tanks respectively. Before entering the solvent tanks, they pass through a treatment tank loaded with silver-loaded glass antibacterial material microspheres at a treatment rate of 60-100 kg / min.

[0058] (3) Treatment of finished tobacco flavors and fragrances:

[0059] The finished Golden Leaf (Tianxingjian) flavors and fragrances (provided by Henan Zhongyan Zhumadian Cigarette Factory) prepared according to the product formula were transferred into the turnover tank, and 1 / 4 volume of silver-loaded glass antibacterial material microspheres were placed in the tank. After stirring for 0.5-1h, it was left to stand for more than 1h. Then the treated finished tobacco flavors and fragrances were poured into the finished product tank. The treated finished tobacco flavors and fragrances were tested for antibacterial properties, and the results are shown in Table 3.

[0060] (4) Recycling of antibacterial materials:

[0061] The silver-loaded glass antibacterial material microspheres in the turnover tank are regularly filtered and recovered, ultrasonically cleaned with water and propylene glycol for 20-30 minutes respectively, and can be used again after drying.

[0062] Table 3 Antibacterial test results

[0063]

[0064] Example 4

[0065] (1) Preparation of silver-loaded glass antibacterial material:

[0066] In parts by weight, 93 parts of silicon dioxide, 24 parts of aluminum oxide, and 7 parts of sodium oxide are mixed, put into a blender and mixed evenly to obtain a mixture; the mixture is added into a high-temperature device, heated to 1400°C and calcined for 2.2 hours to obtain a melt, and after the melt is mixed evenly, the melt is water quenched and cooled to obtain a glass body; after the glass body is dried, it is put into a ball mill and ball-milled at a speed of 400 r / min for 2.8 hours, and the glass powder material is obtained after sieving.

[0067] Calculated by volume, 1 part of molecular sieve and 13 parts of silver nitrate solution are mixed evenly, and the mixture is heated to 500° C. and calcined for 1 hour in a high-temperature device under the protection of inert gas to obtain a silver-loaded molecular sieve material.

[0068] By weight, 86 parts of glass powder material, 14 parts of silver-loaded molecular sieve material and 13 parts of binder are fully ground and uniformly prepared into spherical particles in a granulator to obtain the silver-loaded glass antibacterial material.

[0069] (2) Antibacterial pretreatment of tobacco flavors and fragrance solvents:

[0070] Solvents for preparing tobacco flavors and fragrances, such as water and propylene glycol, are pumped into solvent tanks respectively. Before entering the solvent tanks, they pass through a treatment tank loaded with silver-loaded glass antibacterial material microspheres at a treatment rate of 60-100 kg / min.

[0071] (3) Treatment of finished tobacco flavors and fragrances:

[0072] The finished golden leaf (hard silver) flavors and fragrances (provided by Henan Zhongyan Zhumadian Cigarette Factory) prepared according to the product formula were transferred into the turnover tank, and 1 / 4 volume of silver-loaded glass antibacterial material microspheres were placed in the tank. After stirring for 0.5-1h, it was left to stand for more than 1h. Then the treated finished tobacco flavors and fragrances were poured into the finished product tank. The treated finished tobacco flavors and fragrances were tested for antibacterial properties, and the results are shown in Table 4.

[0073] (4) Recycling of antibacterial materials:

[0074] The silver-loaded glass antibacterial material microspheres in the turnover tank are regularly filtered and recovered, ultrasonically cleaned with water and propylene glycol for 20-30 minutes respectively, and can be used again after drying.

[0075] Table 4 Antibacterial test results

[0076]

[0077]

[0078] 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 silver-loaded glass antibacterial material, characterized in that: The invention comprises glass powder material, silver-loaded molecular sieve material and binder, wherein the mass ratio of the three is (85-90):(10-15):(5-10). The silver-loaded glass antibacterial material is prepared by uniformly mixing the glass powder material, the silver-loaded molecular sieve material and the binder, grinding the mixture and feeding it into a granulator for extrusion molding.

2. The silver-loaded glass antibacterial material according to claim 1, characterized in that: The granulator pressure is 30-50 MPa, maintained for 5-10 min, and the binder is pseudo-boehmite with a moisture content of 8±2%.

3. A method for preparing a silver-loaded glass antibacterial material, characterized in that: The following steps are involved: (1) Preparation of glass powder material: SiO2, Al2O3 and Na2O3 are placed in a mixer according to a certain mass ratio and mixed evenly to obtain a mixture; the mixture is added to a high temperature device, heated to 1400°C and calcined for 2-3 hours to obtain a melt; after the melt is mixed evenly, the melt is quenched with water to obtain a glass body; after the glass body is dried, it is placed in a ball mill for ball milling, and sieved to obtain a glass powder material; (2) Preparation of silver-loaded molecular sieve material: The molecular sieve and silver nitrate solution are uniformly mixed, and the temperature is raised to 500° C. and calcined for 1-2 hours in a high-temperature device under the protection of an inert gas to obtain the silver-loaded molecular sieve material; (3) Preparation of silver-loaded glass antibacterial material: After the glass powder material, silver-loaded molecular sieve material and binder are fully and evenly ground, they are prepared into spherical particles in a granulator to obtain the silver-loaded glass antibacterial material.

4. The method for preparing the silver-loaded glass antibacterial material according to claim 3, characterized in that: In step (1), the mass ratio of silicon dioxide, aluminum oxide and sodium oxide is (85-95):(10-30):(5-15).

5. The method for preparing the silver-loaded glass antibacterial material according to claim 3, characterized in that: In step (1), the mixed material is added into a high temperature device, and the temperature rise program is: 25-1400° C., 150-250 min, and constant temperature for 80-120 min; the water used for water quenching is deionized water.

6. The method for preparing the silver-loaded glass antibacterial material according to claim 3, characterized in that: In step (1), the ball milling process is as follows: add 1 part of the glass powder material, 2 parts of deionized water, and 10 parts of grinding balls into a ball mill, and ball mill at a rotation speed of 300-600 r / min for 2-4 hours.

7. The method for preparing the silver-loaded glass antibacterial material according to claim 3, characterized in that: In step (2), the molecular sieve is a mesoporous molecular sieve with a particle size less than 100 mesh and a pore size of 30-60 nm; the concentration of the silver nitrate solution is 0.2-0.9 mol / L, and the volume ratio of the molecular sieve to the silver nitrate solution is 1:(10-20); the heating program is: 25-120°C, 90-100 min, constant temperature 20-30 min; 120-500°C, 180-220 min, insulation 70-110 min; the inert gas is nitrogen with a purity greater than 99.9%.

8. The method for preparing the silver-loaded glass antibacterial material according to claim 3, characterized in that: In step (3), the mass ratio of glass powder material, silver-loaded molecular sieve material and binder is (85-90):(10-15):(5-10); the binder is pseudo-boehmite.

9. A method for preparing a silver-loaded glass antibacterial material and its application in tobacco flavors, characterized in that: The silver-loaded glass antibacterial material is a silver-loaded glass antibacterial material prepared according to any one of the preparation methods described in claims 3-8.

10. Application of silver-loaded glass antibacterial material in tobacco flavor, characterized in that: The application is: transfer the tobacco flavors and fragrances prepared according to the product formula into the turnover tank, put 1 / 4 volume of silver-loaded glass antibacterial material microspheres into the tank, stir for 0.5-1h, and let it stand for more than 1h. Then pour the processed finished tobacco flavors and fragrances into the finished product tank to complete the sterilization.

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