CN100551242C - Silver supported ammonium modified nano zeolite antibacterial agent and preparation method thereof - Google Patents
Silver supported ammonium modified nano zeolite antibacterial agent and preparation method thereof Download PDFInfo
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- CN100551242C CN100551242C CNB2006101520329A CN200610152032A CN100551242C CN 100551242 C CN100551242 C CN 100551242C CN B2006101520329 A CNB2006101520329 A CN B2006101520329A CN 200610152032 A CN200610152032 A CN 200610152032A CN 100551242 C CN100551242 C CN 100551242C
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Abstract
Silver supported ammonium modified nano zeolite antibacterial agent and preparation method thereof relates to a kind of antibacterial agent, the preparation method who especially relates to a kind of silver supported ammonium modified nano zeolite antibacterial agent and adopt the ionic liquid phase exchange process.A kind of bacteriostasis rate height is provided, is applied to produce the smooth smooth daily-use sanitary anti-bacteria ceramic of glaze etc., heat-treatment temperature range is up to 1100 ℃ of silver supported ammonium modified nano zeolite antibacterial agents that still possess effective anti-microbial property and preparation method thereof.Be made up of ammonium modified nano zeolite and silver, ammonium modified nano zeolite is 91%～99%, and silver nitrate is 1%～9%.With nano zeolite powder and ammonium chloride solution hybrid reaction, the water suction filtration, wash generate with the no white precipitate of liquor argenti nitratis ophthalmicus check to filtrate till, dry again, make ammonium modified nano zeolite through grinding.Again ammonium modified nano zeolite is scattered in the water, adds AgNO
3,, make silver supported ammonium modified nano zeolite antibacterial agent after the grinding with deionized water suction filtration, the oven dry of washing back.
Description
Technical field
The present invention relates to a kind of antibacterial agent, the preparation method who especially relates to a kind of silver supported ammonium modified nano zeolite antibacterial agent and adopt the ionic liquid phase exchange process.
Background technology
Along with people to the research of environmental microorganism and improving constantly of the level of understanding, when utilizing the microorganism helpfulness, also very vigilant its harmfulness as pathogen.It is reported that dead about 5,200 ten thousand people of whole world year nineteen ninety-five wherein because of the death toll that bacterial infection causes is 1,700 ten thousand, account for 1/3.The food poisoning of the nationwide that the pathogenicity Escherichia coli 0-157 of Japan's generation in 1996 causes was once once causing global fear.In addition, microorganism also can cause the decomposition, rotten and corrupt of various industrial materials, cosmetics and pharmaceuticals etc., thereby the life-span of product is shortened.In the modern society that scientific and technological progress, social development and living standards of the people improve constantly, healthy living environment becomes human pursuing one's goal day by day, and environmental protection problem also more and more comes into one's own.Anti-biotic material is the important component part of environment-friendly materials, thereby exploitation and production and people's lives goods closely bound up, that can suppress or eliminate noxious bacteria, has become one of modern science and technology field important subject.The major defect that existing carrying silver antimicrobials exists: the one, silver nitrate is that antibacterial product dissociates that the silver nitrate ion that is reduced into the simple substance silver nitrate under solar radiation or after being heated to uniform temperature easily and grey or brown and influence the outward appearance of goods; The 2nd, Ag-carried antibacterial goods cost is higher.Zhoushan Tomorrow Nanomaterials Co., Ltd discloses a kind of preparation method of nano silver-supported antibacterial powder in publication number is the application for a patent for invention of CN1344494, comprise silver nitrate in the raw material, earlier nano silicon-based oxide is modulated into pasty state with water, add stabilizing agent, mix with silver nitrate aqueous solution then synthetic, after dehydration and drying form.Shanghai Normal University discloses a kind of silver-carried antibacterial agent with nanometer porous in publication number is the application for a patent for invention of CN1817138, be made up of carrier and silver nitrate, and specific surface area is 500～1500cm
3/ g, the aperture is 2～10nm, pore volume is 0.5～1.5cm
3/ g.
Summary of the invention
The objective of the invention is at the existing shortcoming of existing carrying silver antimicrobials and preparation method thereof, a kind of bacteriostasis rate height is provided, be applied to produce the smooth smooth daily-use sanitary anti-bacteria ceramic of glaze etc., heat-treatment temperature range is up to 1100 ℃ of silver supported ammonium modified nano zeolite antibacterial agents that still possess effective anti-microbial property and preparation method thereof.
For the good anti-biotic material of obtained performance, technical scheme of the present invention is to adopt the ionic liquid phase exchange process to prepare silver supported ammonium modified nano zeolite antibacterial agent.
Silver supported ammonium modified nano zeolite antibacterial agent of the present invention is made up of ammonium modified nano zeolite and silver, cubage by mass percentage, and ammonium modified nano zeolite is 91%～99%, silver nitrate is 1%～9%.
Silver supported ammonium modified nano zeolite antibacterial agent preparation method of the present invention comprises the steps:
1) preparation ammonium modified nano zeolite
Earlier with nano zeolite powder and ammonium chloride solution hybrid reaction, by quality than nano zeolite powder: ammonium chloride solution is 1: (5～15), the water suction filtration, wash check no white precipitate generation with liquor argenti nitratis ophthalmicus to filtrate till;
With washed filtrate product oven dry, make ammonium modified nano zeolite again through grinding.
2) preparation silver supported ammonium modified nano zeolite antibacterial agent
Earlier ammonium modified nano zeolite is scattered in the water, adds AgNO
3, to press ammonium modified nano zeolite and calculate with different mass percentage content with silver nitrate, ammonium modified nano zeolite is 91%～99%, silver nitrate is 1%～9%, with deionized water suction filtration, the oven dry of washing back;
After grinding, make silver supported ammonium modified nano zeolite antibacterial agent again.
The concentration of the ammonium chloride solution that adopts is preferably 2～5mol/L, best magnetic agitation 3～9h in hybrid reaction, the water suction filtration, wash to filtrate with the no white precipitate generation of liquor argenti nitratis ophthalmicus check till.Again washed filtrate product is placed 70～90 ℃ of oven dry,, cross 150～250 mesh sieves, make ammonium modified nano zeolite through grinding.
The mode that when ammonium modified nano zeolite is scattered in the water, preferably adopts ultrasonic to disperse.Add AgNO
3After, preferably magnetic agitation 3～9h uses deionized water suction filtration, washing, 70～90 ℃ of oven dry; Through grinding, cross 150～250 mesh sieves again, make silver supported ammonium modified nano zeolite antibacterial agent.
The silver supported ammonium modified nano zeolite antibacterial agent of gained is applied to produce the smooth smooth daily-use sanitary anti-bacteria ceramic of glaze, still possesses effective anti-microbial property during heat treatment temperature height to 1100 ℃.Antibacterial ring experiment shows: along with the increase of silver carrying amount, silver supported ammonium modified nano zeolite antibacterial agent improves gradually to colibacillary anti-microbial property.Bacteriostasis rate experiment shows, when calculating the silver supported ammonium modified nano zeolite antibacterial agent addition by mass percentage and be 5%, can reach 99.9% to colibacillary bacteriostasis rate.The antibiotic persistence test result of the anti-bacteria ceramic that silver supported ammonium modified nano zeolite antibacterial agent is made shows that this anti-bacteria ceramic has good durability.Adopt the microscopic appearance of electron microscope observation zeolite powder, the grain diameter of zeolite powder is about 30nm, and particle size distribution is more even.Because nano particle has nanometer size effect and skin effect, so the type zeolite helps increasing the load capacity of ammonium radical ion and silver nitrate ion as the antibacterial agent carrier, thereby improves the anti-microbial property of preparation gained antibacterial agent.
Embodiment
Embodiment 1
Prepare ammonium modified nano zeolite earlier: with the ammonium chloride solution hybrid reaction of zeolite powder and 3mol/L, by quality than zeolite powder: ammonium chloride solution is 1: 10, behind the magnetic agitation 5h, with the deionized water suction filtration, wash to filtrate with the no white precipitate generation of liquor argenti nitratis ophthalmicus check till; Washed filtrate product is placed 75 ℃ of oven dry,, make ammonium modified nano zeolite through grinding 200 mesh sieves.Prepare silver supported ammonium modified nano zeolite antibacterial agent again: adopt ultrasonic to be scattered in the deionized water ammonium modified nano zeolite, add AgNO
3, by mass percentage the cubage ammonium modified nano zeolite be 99% and silver nitrate be 1%, behind the magnetic agitation 6h, with deionized water suction filtration, washing, 80 ℃ of oven dry; Through grinding, cross 200 mesh sieves, make silver supported ammonium modified nano zeolite.
Embodiment 2
Similar to Example 1, its difference is preparation ammonium modified nano zeolite earlier, ammonium chloride solution hybrid reaction with zeolite powder and 3mol/L, by quality than zeolite powder: ammonium chloride solution is 1: 15, behind the magnetic agitation 6h, with the deionized water suction filtration, wash to filtrate with the no white precipitate generation of liquor argenti nitratis ophthalmicus check till; Washed filtrate product is placed 80 ℃ of oven dry,, make ammonium modified nano zeolite through grinding 180 mesh sieves.Prepare silver supported ammonium modified nano zeolite antibacterial agent again, adopt ultrasonic to be scattered in the deionized water ammonium modified nano zeolite, add AgNO
3, cubage by mass percentage, ammonium modified nano zeolite is 95%, silver nitrate is 5%, behind the magnetic agitation 5h, with deionized water suction filtration, washing, 75 ℃ of oven dry; Through grinding, cross 180 mesh sieves, make silver supported ammonium modified nano zeolite.
Embodiment 3
Similar to Example 1, its difference is preparation ammonium modified nano zeolite earlier, ammonium chloride solution hybrid reaction with zeolite powder and 2mol/L, by quality than zeolite powder: ammonium chloride solution is 1: 5, behind the magnetic agitation 3h, with the deionized water suction filtration, wash to filtrate with the no white precipitate generation of liquor argenti nitratis ophthalmicus check till; Washed filtrate product is placed 70 ℃ of oven dry,, make ammonium modified nano zeolite through grinding 150 mesh sieves.Prepare silver supported ammonium modified nano zeolite antibacterial agent again, adopt ultrasonic to be scattered in the deionized water ammonium modified nano zeolite, add AgNO
3, cubage by mass percentage, ammonium modified nano zeolite is 94%, silver nitrate is 6%, behind the magnetic agitation 3h, with deionized water suction filtration, washing, 70 ℃ of oven dry; Through grinding, cross 150 mesh sieves, make silver supported ammonium modified nano zeolite.
Embodiment 4
Similar to Example 1, its difference is preparation ammonium modified nano zeolite earlier, ammonium chloride solution hybrid reaction with zeolite powder and 5mol/L, by quality than zeolite powder: ammonium chloride solution is 1: 5, behind the magnetic agitation 9h, with the deionized water suction filtration, wash to filtrate with the no white precipitate generation of liquor argenti nitratis ophthalmicus check till; Washed filtrate product is placed 90 ℃ of oven dry,, make ammonium modified nano zeolite through grinding 250 mesh sieves.Prepare silver supported ammonium modified nano zeolite antibacterial agent again, adopt ultrasonic to be scattered in the deionized water ammonium modified nano zeolite, add AgNO
3, cubage by mass percentage, ammonium modified nano zeolite is 93%, silver nitrate is 7%, behind the magnetic agitation 9h, with deionized water suction filtration, washing, 90 ℃ of oven dry; Through grinding, cross 250 mesh sieves, make silver supported ammonium modified nano zeolite.
Embodiment 5: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 96% by mass percentage, silver nitrate is 4%, at 800 ℃ of following thermal treatment 1h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 9.3mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 2.5%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 98.10%.
Embodiment 6: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 98% by mass percentage, silver nitrate is 2%, at 900 ℃ of following thermal treatment 1h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 9.7mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 10.0%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 100%.
Embodiment 7: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 96% by mass percentage, silver nitrate is 4%, at 800 ℃ of following thermal treatment 1h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 10.2mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 7.5%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 99.98%.
Embodiment 8: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 99% by mass percentage, silver nitrate is 1%, at 1000 ℃ of following thermal treatment 1h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 8.8mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 10.0%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 100%.
Embodiment 9: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 91% by mass percentage, silver nitrate is 9%, at 1100 ℃ of following thermal treatment 1h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 9.5mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 5.0%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 92.5%.
Embodiment 10: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 97% by mass percentage, silver nitrate is 3%, at 900 ℃ of following thermal treatment 2h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 8.5mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 4.0%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 93.5%.
Embodiment 11: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 92% by mass percentage, silver nitrate is 8%, at 1000 ℃ of following thermal treatment 0.5h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 9.2mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 6.0%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 91.5%.
Embodiment 12: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 91% by mass percentage, silver nitrate is 9%, at 1000 ℃ of following thermal treatment 0.5h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 9.6mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 6.0%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 93.5%.
Embodiment 13: silver nitrate and ammonium modified nano zeolite hybrid reaction, wherein the cubage ammonium modified nano zeolite is 95% by mass percentage, silver nitrate is 5%, at 1100 ℃ of following thermal treatment 0.5h, make the ammonium modified nano zeolite antimicrobial powder, the antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of acquisition is 9.5mm; When silver supported ammonium modified zeolite antibacterial agent percentage composition was 6.0%, the bacteriostasis rate of the anti-bacteria ceramic that makes was 91.5%.
With silver nitrate and ammonium modified nano zeolite with different proportioning hybrid reactions, wherein calculate silver nitrate content by mass percentage and be respectively 1%, 2%, 3% and 4%, make the ammonium modified nano zeolite antimicrobial powder, obtain the anti-microbial property (seeing table 1 for details) of the antibacterial agent of variable concentrations preparation; Adopting different heat treatment temperatures is that 2% antimicrobial powder that makes is handled to the mass percentage content by silver nitrate, and obtaining the different heat treatment temperature influences situation (seeing table 2 for details) to the anti-microbial property of antibacterial agent; The bacteriostasis rate of the anti-bacteria ceramic that table 3 makes for different silver supported ammonium modified zeolite antibacterial agent percentage compositions.
The antibacterial ring of the silver supported ammonium modified zeolite antibacterial agent of the different silver nitrate content preparations of table 1
| The mass percent of silver nitrate content | Blank | 1％ | 2％ | 3％ | 4％ |
| Antibacterial ring (mm) | 0 | 9.3 | 9.7 | 10.0 | 10.2 |
The antibacterial ring of silver supported ammonium modified zeolite antibacterial agent during table 2 different heat treatment temperature
| Heat treatment temperature (℃) | Blank | 800 | 900 | 1000 | 1100 |
| Antibacterial ring (mm) | 0 | 10.3 | 9.7 | 8.8 | 2.5 |
The bacteriostasis rate of the anti-bacteria ceramic that the silver supported ammonium modified zeolite antibacterial agent of the different percentage compositions of table 3 makes
| Sample | When initial (cfu) | Behind the 24h (cfu) | Bacteriostasis rate (%) |
| Blank sample 2.5% sample 5.0% sample 7.5% sample 10.0% sample | 38.3×10 7 38.3×10 7 38.3×10 7 38.3×10 7 38.3×10 7 | 26.7×10 7×2 36.3×10 5×2 1.7×10 5×2 0.3×10 5×2 0×10 5×2 | - 98.10 99.91 99.98 100 |
Claims (2)
1. the preparation method of silver supported ammonium modified nano zeolite antibacterial agent is characterized in that the steps include:
1) preparation ammonium modified nano zeolite
Earlier with nano zeolite powder and ammonium chloride solution hybrid reaction, magnetic agitation 3～9h, by quality than nano zeolite powder: ammonium chloride solution is 1: 5～15, the water suction filtration, wash to filtrate with the no white precipitate generation of liquor argenti nitratis ophthalmicus check till, with washed filtrate product oven dry, the temperature of oven dry is 70～90 ℃ again, through grinding, cross 150～250 mesh sieves, make ammonium modified nano zeolite; The concentration of described ammonium chloride solution is 2～5mol/L;
2) preparation silver supported ammonium modified nano zeolite antibacterial agent
Earlier adopt ultrasonic to be scattered in the water ammonium modified nano zeolite, add AgNO
3, with deionized water suction filtration, washing,, grind the back and cross 150～250 mesh sieves 70～90 ℃ of oven dry down, make silver supported ammonium modified nano zeolite antibacterial agent, by mass percentage, ammonium modified nano zeolite is 91%～99%, silver nitrate is 1%～9%.
2. the preparation method of silver supported ammonium modified nano zeolite antibacterial agent as claimed in claim 1 is characterized in that adding AgNO
3After, magnetic agitation 3～9h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101028284B (en) * | 2007-03-27 | 2010-10-06 | 中国人民解放军第四军医大学 | Externally-applied zeolite hemostat and its preparation |
| CN102461561A (en) * | 2010-11-19 | 2012-05-23 | 北京佳盛世纪科技有限公司 | Zeolite-loaded silver antibacterial agent and preparation method thereof |
| CN102318645B (en) * | 2011-05-25 | 2014-04-16 | 华侨大学 | Silver-containing antibacterial agent and preparation method thereof |
| CN106668925A (en) * | 2016-12-23 | 2017-05-17 | 浙江大学常州工业技术研究院 | Antibacterial hemostatic material as well as preparation method and use thereof |
| CN107258812A (en) * | 2017-06-22 | 2017-10-20 | 安徽省德邦瓷业有限公司 | A kind of preparation method of composite modified zeolite with carrying silver for domestic ceramics glaze slip |
| CN108822664A (en) * | 2018-06-06 | 2018-11-16 | 东阳市善水环境工程有限公司 | A kind of bactericidal inner wall Paint preparation technology |
| CN109970341B (en) * | 2019-04-23 | 2022-03-08 | 潮州市华利达陶瓷制作有限公司 | Antifouling antibacterial ceramic glaze and preparation method thereof |
| CN111955614A (en) * | 2020-08-31 | 2020-11-20 | 眉山市丹福饲料有限公司 | Pig feed preparation process and pig feed prepared by same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4938958A (en) * | 1986-12-05 | 1990-07-03 | Shinagawa Fuel Co., Ltd. | Antibiotic zeolite |
| CN1685830A (en) * | 2005-04-29 | 2005-10-26 | 宁波华实纳米材料有限公司 | Nano silver antibacterial powder and its preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4938958A (en) * | 1986-12-05 | 1990-07-03 | Shinagawa Fuel Co., Ltd. | Antibiotic zeolite |
| CN1685830A (en) * | 2005-04-29 | 2005-10-26 | 宁波华实纳米材料有限公司 | Nano silver antibacterial powder and its preparation method |
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