CN108902177A - A kind of preparation method of argentiferous titanium dioxide anti-bacterial agent - Google Patents
A kind of preparation method of argentiferous titanium dioxide anti-bacterial agent Download PDFInfo
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- CN108902177A CN108902177A CN201810677629.8A CN201810677629A CN108902177A CN 108902177 A CN108902177 A CN 108902177A CN 201810677629 A CN201810677629 A CN 201810677629A CN 108902177 A CN108902177 A CN 108902177A
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- titanium dioxide
- argentiferous
- bacterial agent
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- silver
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
Abstract
The invention discloses a kind of preparation methods of argentiferous titanium dioxide anti-bacterial agent, including：(1) butyl titanate is added to absolute ethanol and is kept stirring until being added dropwise, dust technology is added dropwise again, 20~30min of magnetic agitation under 30~60 DEG C of water bath conditions obtains TiO 2 sol, and the ratio between the butyl titanate, volume of the dehydrated alcohol, the dust technology are 5:10~20:0.5~1.5；(2) silver nitrate solution is added into above-mentioned TiO 2 sol, 10~20min is stirred, the ammonium hydroxide for being added dropwise 3% extremely precipitates disappearance just, adds formalin, 2~3h of magnetic agitation under 50~60 DEG C of water bath condition obtains silver-TiO 2 sol mixture；(3) above-mentioned silver-TiO 2 sol mixture is centrifuged, gained precipitating is cleaned 3~5 times with ethanol water, and dry 10~20h, obtains argentiferous titanium dioxide anti-bacterial agent in 50~60 DEG C of baking oven.In argentiferous titanium dioxide anti-bacterial agent in the present invention, titanium dioxide can be loaded preferably and fix Nano silver grain, and Nano silver grain is made to have more efficient antibacterial activity.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation method of argentiferous titanium dioxide anti-bacterial agent.
Background technique
Antibacterial agent, to kill and suppress growth of microorganism the preparation for major function, is broadly divided into organic anti-bacterial as one kind
Agent and inorganic antiseptic two types.The features such as wherein organic antibacterial agent has low in cost, with strong points, but broad spectrum activity is poor,
The problems such as poor heat resistance.And inorganic antiseptic has many advantages, such as long-acting, broad-spectrum, is one of the research hotspot in the current field.
Inorganic antiseptic is divided into oxide semiconductor photoactivation antibacterial using titanium dioxide as representative and again using silver as representative
Heavy metal sterilize two major classes, titanium dioxide is from a wealth of sources, low in cost, but antimicrobial efficiency is low；And the heavy metals antibacterial such as silver is imitated
Fruit is good, but expensive, and usage amount is restricted.Therefore synthesis of titanium dioxide carries silver-colored economic benefits and social benefits inorganic antiseptic and causes numerous
The interest of person.Numerous studies discovery, when silver particles are evenly distributed in the complex antimicrobials of synthesis, uniform particle diameter, and in nanometer two
It is orderly adulterated in oxidation titanium oxide, anti-microbial property can be effectively improved.
For this reason, it is necessary to can solve in view of the above-mentioned problems, propose a kind of preparation method of argentiferous titanium dioxide anti-bacterial agent
Certainly problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of argentiferous titanium dioxide anti-bacterial agent, to overcome in the prior art
Deficiency.
To achieve the above object, the present invention provides the following technical solutions：
A kind of preparation method of argentiferous titanium dioxide anti-bacterial agent, including：
(1) butyl titanate is added to absolute ethanol and is kept stirring until be added dropwise, then dust technology is added dropwise, 30~
20~30min of magnetic agitation under 60 DEG C of water bath conditions obtains TiO 2 sol, the butyl titanate, the dehydrated alcohol, institute
Stating the ratio between volume of dust technology is 5:10~20:0.5~1.5；
(2) it is added silver nitrate solution into above-mentioned TiO 2 sol, stirs 10~20min, 3% ammonium hydroxide is added dropwise to heavy
It forms sediment and disappears just, add formalin, 2~3h of magnetic agitation under 50~60 DEG C of water bath condition obtains silver-titanium dioxide
Collosol intermixture；
(3) above-mentioned silver-TiO 2 sol mixture is centrifuged, gained precipitating cleans 3~5 with ethanol water
Secondary, dry 10~20h, obtains argentiferous titanium dioxide anti-bacterial agent in 50~60 DEG C of baking oven.
Preferably, in step (1), the ratio between the butyl titanate, volume of the dehydrated alcohol, the dust technology are 5:
15:1。
Preferably, in step (2), the concentration of the silver nitrate solution is 0.01~0.05mol/L.
Preferably, in step (2), the concentration of the formalin is 0.1~1mol/L.
Preferably, in the argentiferous titanium dioxide anti-bacterial agent, the partial size of the titanium dioxide is 2~3 μm.
Preferably, in the argentiferous titanium dioxide anti-bacterial agent, the mass fraction of the silver is 1.0~2.5%, the dioxy
The mass fraction for changing titanium is 97.5~99%.
Compared with the prior art, the advantages of the present invention are as follows：In argentiferous titanium dioxide anti-bacterial agent in the present invention, titanium dioxide
Titanium can be loaded preferably and fix Nano silver grain, to significantly improve the stability of Nano silver grain, make Nano silver grain
With more efficient antibacterial activity.
Specific embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of argentiferous titanium dioxide anti-bacterial agent, including：
(1) butyl titanate is added to absolute ethanol and is kept stirring until be added dropwise, then dust technology is added dropwise, 30~
20~30min of magnetic agitation under 60 DEG C of water bath conditions obtains TiO 2 sol, the butyl titanate, the dehydrated alcohol, institute
Stating the ratio between volume of dust technology is 5:10~20:0.5~1.5；
(2) it is added silver nitrate solution into above-mentioned TiO 2 sol, stirs 10~20min, 3% ammonium hydroxide is added dropwise to heavy
It forms sediment and disappears just, add formalin, 2~3h of magnetic agitation under 50~60 DEG C of water bath condition obtains silver-titanium dioxide
Collosol intermixture；
(3) above-mentioned silver-TiO 2 sol mixture is centrifuged, gained precipitating cleans 3~5 with ethanol water
Secondary, dry 10~20h, obtains argentiferous titanium dioxide anti-bacterial agent in 50~60 DEG C of baking oven.
In above-mentioned steps (1), the ratio between the butyl titanate, volume of the dehydrated alcohol, the dust technology are 5:15:1.
In above-mentioned steps (2), the concentration of the silver nitrate solution is 0.01~0.05mol/L, it is preferred that the silver nitrate
The concentration of solution is 0.03mol/L；The concentration of the formalin be 0.1~1mol/L, it is preferred that the formalin it is dense
Degree is 0.6mol/L.
In the argentiferous titanium dioxide anti-bacterial agent being prepared according to the above method, the partial size of the titanium dioxide is 2~3 μ
M, wherein the mass fraction of the silver is 1.0~2.5%, and the mass fraction of the titanium dioxide is 97.5~99%.
Following preparation methods that argentiferous titanium dioxide anti-bacterial agent in the present invention is illustrated with specifically embodiment.
Embodiment 1
(1) butyl titanate is added to absolute ethanol and is kept stirring until being added dropwise, then dust technology is added dropwise, at 30 DEG C
Magnetic agitation 20min under water bath condition obtains TiO 2 sol, the butyl titanate, the dehydrated alcohol, the dust technology
The ratio between volume be 5:10:0.5；
(2) silver nitrate solution of 0.01mol/L is added into above-mentioned TiO 2 sol, stirs 10min, is added dropwise 3%
Ammonium hydroxide adds the formalin of 0.1mol/L, magnetic agitation 2h, obtains under 50 DEG C of water bath condition to disappearance just is precipitated
Silver-TiO 2 sol mixture；
(3) above-mentioned silver-TiO 2 sol mixture is centrifuged, gained precipitating cleans 3~5 with ethanol water
Secondary, dry 10h, obtains argentiferous titanium dioxide anti-bacterial agent in 50 DEG C of baking oven.
Embodiment 2
(1) butyl titanate is added to absolute ethanol and is kept stirring until being added dropwise, then dust technology is added dropwise, at 50 DEG C
Magnetic agitation 25min under water bath condition obtains TiO 2 sol, the butyl titanate, the dehydrated alcohol, the dust technology
The ratio between volume be 5:15:1；
(2) silver nitrate solution of 0.03mol/L is added into above-mentioned TiO 2 sol, stirs 15min, is added dropwise 3%
Ammonium hydroxide adds the formalin of 0.6mol/L, magnetic agitation 2.5h, obtains under 55 DEG C of water bath condition to disappearance just is precipitated
To silver-TiO 2 sol mixture；
(3) above-mentioned silver-TiO 2 sol mixture is centrifuged, gained precipitating cleans 3~5 with ethanol water
Secondary, dry 15h, obtains argentiferous titanium dioxide anti-bacterial agent in 55 DEG C of baking oven.
Embodiment 3
(1) butyl titanate is added to absolute ethanol and is kept stirring until being added dropwise, then dust technology is added dropwise, at 60 DEG C
Magnetic agitation 30min under water bath condition obtains TiO 2 sol, the butyl titanate, the dehydrated alcohol, the dust technology
The ratio between volume be 5:20:1.5；
(2) silver nitrate solution of 0.05mol/L is added into above-mentioned TiO 2 sol, stirs 20min, is added dropwise 3%
Ammonium hydroxide adds the formalin of 1mol/L, magnetic agitation 3h, obtains under 60 DEG C of water bath condition to disappearance just is precipitated
Silver-TiO 2 sol mixture；
(3) above-mentioned silver-TiO 2 sol mixture is centrifuged, gained precipitating cleans 3~5 with ethanol water
Secondary, dry 20h, obtains argentiferous titanium dioxide anti-bacterial agent in 60 DEG C of baking oven.
In the argentiferous titanium dioxide anti-bacterial agent being prepared according to the method in above-described embodiment, the mass fraction of the silver
It is 1.0~2.5%, the mass fraction of the titanium dioxide is 97.5~99%.
It carries out electron-microscope scanning test to argentiferous titanium dioxide anti-bacterial agent obtained in the present invention to learn, dioxy in the antibacterial agent
The partial size for changing titanium is 2~3 μm, and titanium dioxide can preferably load and fix Nano silver grain, so as to significantly improve
The stability of Nano silver grain makes Nano silver grain have more efficient antibacterial activity.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (6)
1. a kind of preparation method of argentiferous titanium dioxide anti-bacterial agent, which is characterized in that including：
(1) butyl titanate is added to absolute ethanol and is kept stirring until being added dropwise, then dust technology is added dropwise, at 30~60 DEG C
20~30min of magnetic agitation under water bath condition, obtains TiO 2 sol, the butyl titanate, the dehydrated alcohol, described dilute
The ratio between volume of nitric acid is 5:10~20:0.5~1.5；
(2) be added silver nitrate solution into above-mentioned TiO 2 sol, stir 10~20min, be added dropwise 3% ammonium hydroxide it is proper to precipitating
It is good to disappear, formalin is added, 2~3h of magnetic agitation under 50~60 DEG C of water bath condition obtains silver-TiO 2 sol
Mixture；
(3) above-mentioned silver-TiO 2 sol mixture being centrifuged, gained precipitating is cleaned 3~5 times with ethanol water, in
Dry 10~20h, obtains argentiferous titanium dioxide anti-bacterial agent in 50~60 DEG C of baking oven.
2. the preparation method of argentiferous titanium dioxide anti-bacterial agent according to claim 1, which is characterized in that in step (1), institute
Stating the ratio between volume of butyl titanate, the dehydrated alcohol, the dust technology is 5:15:1.
3. the preparation method of argentiferous titanium dioxide anti-bacterial agent according to claim 1, which is characterized in that in step (2), institute
The concentration for stating silver nitrate solution is 0.01~0.05mol/L.
4. the preparation method of argentiferous titanium dioxide anti-bacterial agent according to claim 1, which is characterized in that in step (2), institute
The concentration for stating formalin is 0.1~1mol/L.
5. the preparation method of argentiferous titanium dioxide anti-bacterial agent according to claim 1, which is characterized in that the argentiferous dioxy
Change in titanium antibacterial agent, the partial size of the titanium dioxide is 2~3 μm.
6. the preparation method of argentiferous titanium dioxide anti-bacterial agent according to claim 1, which is characterized in that the argentiferous dioxy
Change in titanium antibacterial agent, the mass fraction of the silver is 1.0~2.5%, and the mass fraction of the titanium dioxide is 97.5~99%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110670194A (en) * | 2019-10-14 | 2020-01-10 | 湖南科力嘉纺织股份有限公司 | Preparation method of antibacterial yarn |
| CN112075454A (en) * | 2020-10-13 | 2020-12-15 | 成都市图腾环保科技有限公司 | Composite silver titanium dioxide inorganic antibacterial agent |
| CN113621181A (en) * | 2021-08-03 | 2021-11-09 | 安徽江淮汽车集团股份有限公司 | Preparation method of antibacterial agent, thermoplastic resin composite material and preparation method thereof |
| CN113712046A (en) * | 2021-05-26 | 2021-11-30 | 北京崇高纳米科技有限公司 | Organic-inorganic compound for long-acting protection of microorganisms and preparation method thereof |
| CN115651439A (en) * | 2022-11-11 | 2023-01-31 | 安徽江淮汽车集团股份有限公司 | Automobile health cabin antibacterial coating and preparation method thereof |
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| CN101731270A (en) * | 2009-12-17 | 2010-06-16 | 浙江大学 | Method for preparing novel titanium dioxide silver-doped antibacterial agent |
| CN103203466A (en) * | 2013-03-25 | 2013-07-17 | 中国人民解放军济南军区第四0一医院 | Method for preparing nano silver different in grain diameter |
| CN104258851A (en) * | 2014-10-18 | 2015-01-07 | 中山市创科科研技术服务有限公司 | Preparation method of silver doped titanium dioxide nano sol |
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2018
- 2018-06-27 CN CN201810677629.8A patent/CN108902177A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101731270A (en) * | 2009-12-17 | 2010-06-16 | 浙江大学 | Method for preparing novel titanium dioxide silver-doped antibacterial agent |
| CN103203466A (en) * | 2013-03-25 | 2013-07-17 | 中国人民解放军济南军区第四0一医院 | Method for preparing nano silver different in grain diameter |
| CN104258851A (en) * | 2014-10-18 | 2015-01-07 | 中山市创科科研技术服务有限公司 | Preparation method of silver doped titanium dioxide nano sol |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110670194A (en) * | 2019-10-14 | 2020-01-10 | 湖南科力嘉纺织股份有限公司 | Preparation method of antibacterial yarn |
| CN112075454A (en) * | 2020-10-13 | 2020-12-15 | 成都市图腾环保科技有限公司 | Composite silver titanium dioxide inorganic antibacterial agent |
| CN113712046A (en) * | 2021-05-26 | 2021-11-30 | 北京崇高纳米科技有限公司 | Organic-inorganic compound for long-acting protection of microorganisms and preparation method thereof |
| CN113712046B (en) * | 2021-05-26 | 2023-10-24 | 北京崇高纳米科技有限公司 | Organic-inorganic compound capable of protecting microorganisms for long time and preparation method thereof |
| CN113621181A (en) * | 2021-08-03 | 2021-11-09 | 安徽江淮汽车集团股份有限公司 | Preparation method of antibacterial agent, thermoplastic resin composite material and preparation method thereof |
| CN115651439A (en) * | 2022-11-11 | 2023-01-31 | 安徽江淮汽车集团股份有限公司 | Automobile health cabin antibacterial coating and preparation method thereof |
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Application publication date: 20181130 |