CN104304319B - A kind of preparation method of titanium dioxide silver base inorganic antibacterial agent - Google Patents
A kind of preparation method of titanium dioxide silver base inorganic antibacterial agent Download PDFInfo
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- CN104304319B CN104304319B CN201410473030.4A CN201410473030A CN104304319B CN 104304319 B CN104304319 B CN 104304319B CN 201410473030 A CN201410473030 A CN 201410473030A CN 104304319 B CN104304319 B CN 104304319B
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- silver
- titanium dioxide
- salt solution
- inorganic antibacterial
- antibacterial agent
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- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- MFPVDOIQNSMNEW-UHFFFAOYSA-N silver oxygen(2-) titanium(4+) Chemical compound [O--].[O--].[Ti+4].[Ag+] MFPVDOIQNSMNEW-UHFFFAOYSA-N 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 26
- 239000012266 salt solution Substances 0.000 claims abstract description 24
- 239000004332 silver Substances 0.000 claims abstract description 20
- 229910052709 silver Inorganic materials 0.000 claims abstract description 20
- NGBNXJUWQPLNGM-UHFFFAOYSA-N silver;azane Chemical compound N.[Ag+] NGBNXJUWQPLNGM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 7
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000009736 wetting Methods 0.000 claims description 9
- 230000002421 anti-septic effect Effects 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 20
- 239000002245 particle Substances 0.000 abstract description 12
- 230000000845 anti-microbial effect Effects 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract 1
- 230000006698 induction Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000006087 Brown hydroboration reaction Methods 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- QBNKFXYJSJOGEL-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Ti+4] QBNKFXYJSJOGEL-UHFFFAOYSA-N 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
Abstract
The invention discloses the preparation method of a kind of titanium dioxide silver base inorganic antibacterial agent.NaOH and ammoniacal liquor are added dropwise in silver salt solution successively, it is configured to certain density silver ammonium salt solution, and control ph, incipient wetness impregnation method is utilized to be added drop-wise in a certain amount of titanium dioxide powder by the silver-colored ammonium salt solution of configuration, and constantly vibrate, make it soak uniformly, after dropping, then obtain titanium dioxide silver base inorganic antibacterial agent through drying at room temperature, reduction.The present invention is simple to operate, preparation technology environmental protection, titanium dioxide surface hydroxyl electric charge is regulated by pH value, induction silver ammonium ion forms strong interaction with titanium dioxide surface, the reunion of silver particles in subsequent processes is effectively stoped to be grown up, silver particles high dispersion at titanium dioxide surface is effectively ensured, improves the anti-microbial property of TiO 2 carrying silver inorganic antibacterial material.
Description
Technical field
The present invention relates to the preparation method of a kind of inorganic composite materials, be specifically related to the preparation method of a kind of TiO 2 carrying silver particles.
Background technology
Antiseptic with the preparation killed and suppress growth of microorganism as major function, is broadly divided into organic antibacterial agent as a class
With inorganic antiseptic two types.The features such as wherein organic antibacterial agent has with low cost, with strong points, but broad spectrum activity is poor,
The problems such as poor heat resistance.And inorganic antiseptic has the advantages such as long-acting, broad-spectrum, it it is one of the study hotspot at present this field.
Inorganic antiseptic is divided into again the oxide semiconductor photoactivation with titanium dioxide as representative antibacterial and weight with silver as representative
The big class of metal sterilizing two, titanium dioxide wide material sources, with low cost, but antimicrobial efficiency is low；And the antibacterial effect of the heavy metals such as silver
The best, but expensive, and usage amount is restricted.Therefore synthesis of titanium dioxide carries silver economic benefits and social benefits inorganic antiseptic and causes crowd
The interest of many scholars.Numerous studies find, when in the complex antimicrobials of synthesis, silver particles is evenly distributed, and uniform particle diameter, and
Nanometer titanium dioxide titanium oxide adulterates in order, anti-microbial property can be effectively improved.
For improving anti-microbial property, substantial amounts of preparation method is applied to the preparation of titanium dioxide silver base inorganic antibacterial agent.But at present
Organic solvent and the complex process such as most synthetic methods need to add complexing agent in preparation process, stabilizer；And other works
The relatively simple preparation method of skill, such as wet chemistry method, the steps such as inevitably needs are overanxious, suction filtration produce a large amount of useless
Liquid, inadequate environmental protection.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of titanium dioxide silver base inorganic antibacterial agent, this preparation method is easy,
Silver particles uniform particle diameter in environmental protection, and the composite prepared, is evenly distributed, improves TiO 2 carrying silver nothing
The antimicrobial efficiency of machine anti-biotic material and performance.
For reaching above-mentioned purpose, the preparation method of titanium dioxide silver base inorganic antibacterial agent of the present invention, its preparation method
As follows:
Dropping NaOH and ammoniacal liquor are to the silver-colored ammonium salt solution of configuration 0.002～0.2mol/L, pH value in silver salt solution the most successively
Control 11.3～12.6；
B. above-mentioned silver ammonium salt solution is constantly added dropwise in a certain amount of titanium dioxide powder, and constantly vibrates so that it is wetting
Uniformly, when solution dropping is complete, after titanium dioxide fully soaks, by little to sample at room temperature natural drying 24 hours～48
Time；
C. dry sample is irradiated 1 hour～6 hours under ultraviolet source, i.e. prepare TiO 2 carrying silver inorganic antibacterial
Agent.
Silver-colored ammonium salt solution described in step A uses after being first added dropwise to NaOH in silver salt solution generate white precipitate and drips ammonia again
Prepared by water；Wherein, silver salt is silver nitrate.
Titanium dioxide powder described in step B is nano titanium oxide.
Compared with prior art, the invention have the advantage that
1. the present invention is by regulation solution ph so that the titanium dioxide surface hydroxyl after wetting is electronegative, and silver ammonium is just
Ion forms monolayer adsorption at titanium dioxide surface, due to the strong interaction of silver ammonium ion with titanium dioxide surface, effectively
Prevent in follow-up During Hydrogen Reducing the reunion of silver particles and grow up, finally give in titanium dioxide surface high degree of dispersion
Silver particles.
The antiseptic silver particles size of gained the most of the present invention is little, and dispersive property is good, and preparation technology is simple, produces without waste liquid, green
Colour circle is protected, and improves the anti-microbial property of titanium dioxide carrying silver antimicrobials.
Accompanying drawing explanation
Fig. 1 be the titanium dioxide silver base inorganic antibacterial agent for preparing of the present invention scanning transmission electron microscope photo.
Detailed description of the invention
Embodiments of the present invention are further illustrated below by embodiment and accompanying drawing.
The preparation method of a kind of TiO 2 carrying silver composite, it specifically comprises the following steps that
A. NaOH and ammoniacal liquor is used to be added dropwise in silver nitrate solution the silver-colored ammonium of configuration 0.002～0.2mol/L successively molten
Liquid, pH value controls 11.3～12.6；
B. above-mentioned silver ammonium salt solution is constantly added dropwise in a certain amount of nano titanium oxide, and constantly vibrates so that it is wetting is all
Even, when solution dropping is complete, and titanium dioxide the most fully soaks, then by sample at room temperature natural drying 24 hours～48
Hour；
C. dry sample is irradiated 1 hour～6 hours under ultraviolet source, i.e. prepare TiO 2 carrying silver inorganic antibacterial
Agent.
Note: the salt of above-mentioned argentiferous and the input amount of titanium dioxide can according to titanium dioxide in antiseptic final products and silver
Content obtains than calculating, and the dripping quantity of solution calculates with complete wetting titanium dioxide.
Embodiment 1
It is added dropwise in silver nitrate solution with sodium hydroxide solution, after generation white precipitate is transformed into brown precipitate then, then drips
Adding ammoniacal liquor until precipitation disappears and pH value rises to 11.8, concentration is the silver-colored ammonium salt solution of 0.02mol/L.By 2.6mL silver
Ammonium salt solution is constantly added dropwise in 1.0g titanium dioxide powder, and constantly vibrates so that it is wetting is uniformly.When silver ammonium salt solution drips
Add complete, by sample at room temperature natural drying 48 hours.Then dry sample is irradiated 1 hour under ultraviolet source,
I.e. prepare titanium dioxide silver base inorganic antibacterial agent.Fig. 1 is its scanning transmission electron microscope figure, and as seen from Figure 1, Argent grain is two
Titania surface high degree of dispersion, is evenly distributed, and grain size is homogeneous, and average particle size particle size is 1.9nm.
Embodiment 2
It is added dropwise in silver nitrate solution with sodium hydroxide solution, after generation white precipitate is transformed into brown precipitate then, then drips
Adding ammoniacal liquor until precipitation disappears and pH value rises to 11.3, concentration is the silver-colored ammonium salt solution of 0.05mol/L.By 2.6mL silver
Ammonium salt solution is constantly added dropwise in 1.0g titanium dioxide powder, and constantly vibrates so that it is wetting is uniformly.When silver ammonium salt solution drips
Add complete, by sample at room temperature natural drying 36 hours.Then dry sample is irradiated 3 hours under ultraviolet source,
I.e. prepare titanium dioxide silver base inorganic antibacterial agent.
Embodiment 3:
It is added dropwise in silver nitrate solution with sodium hydroxide solution, after generation white precipitate is transformed into brown precipitate then, then drips
Adding ammoniacal liquor until precipitation disappears and pH value rises to 12.5, concentration is the silver-colored ammonium salt solution of 0.3mol/L.By 2.6mL silver ammonium
Solution is constantly added dropwise in 1.0g titanium dioxide powder, and constantly vibrates so that it is wetting is uniformly.When silver ammonium salt solution dropping
Complete, by sample at room temperature natural drying 48 hours.Then dry sample is irradiated 3 hours under ultraviolet source,
I.e. prepare titanium dioxide silver base inorganic antibacterial agent.
Embodiment 4:
It is added dropwise in silver nitrate solution with sodium hydroxide solution, after generation white precipitate is transformed into brown oxidation silver precipitation then,
Dripping ammoniacal liquor again until precipitation disappears and pH value rises to 12.0, concentration is the silver-colored ammonium salt solution of 0.1mol/L.By 2.6mL
Silver ammonium salt solution is constantly added dropwise in 1.0g titanium dioxide powder, and constantly vibrates so that it is wetting is uniformly.When silver ammonium salt solution
Drip complete, by sample at room temperature natural drying 36 hours.Then dry sample is irradiated under ultraviolet source 1 little
Time, i.e. prepare titanium dioxide silver base inorganic antibacterial agent.
Claims (3)
1. the preparation method of a titanium dioxide silver base inorganic antibacterial agent, it is characterised in that comprise the steps:
A. the silver-colored ammonium salt solution of configuration 0.002～0.2mol/L, pH value controls 11.3～12.6；
B. above-mentioned silver ammonium salt solution is constantly added dropwise in titanium dioxide powder, and constantly vibrates so that it is wetting is uniform,
When solution dropping is complete, after titanium dioxide fully soaks, by sample at room temperature natural drying 24 hours～48
Hour；
C. dry sample is irradiated 1 hour～6 hours under ultraviolet source, i.e. prepare TiO 2 carrying silver nothing
Machine antiseptic.
The preparation method of titanium dioxide silver base inorganic antibacterial agent the most according to claim 1, its feature exists
In, the silver-colored ammonium salt solution described in step A uses and is first added dropwise to NaOH in silver salt solution generate white precipitate
After drip ammoniacal liquor again and prepare；Wherein, silver salt is silver nitrate.
The preparation method of titanium dioxide silver base inorganic antibacterial agent the most according to claim 1, its feature exists
In, the titanium dioxide powder described in step B is nano titanium oxide.
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| CN201410473030.4A CN104304319B (en) | 2014-09-16 | 2014-09-16 | A kind of preparation method of titanium dioxide silver base inorganic antibacterial agent |
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| CN201410473030.4A CN104304319B (en) | 2014-09-16 | 2014-09-16 | A kind of preparation method of titanium dioxide silver base inorganic antibacterial agent |
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| CN104304319A CN104304319A (en) | 2015-01-28 |
| CN104304319B true CN104304319B (en) | 2016-08-17 |
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| CN105178008A (en) * | 2015-07-17 | 2015-12-23 | 浙江锦尚合成革有限公司 | Synthetic leather surface treatment agent and preparation method thereof |
| CN105133366A (en) * | 2015-07-17 | 2015-12-09 | 浙江锦尚合成革有限公司 | Environment-protective synthetic leather and preparation method thereof |
| CN105155293A (en) * | 2015-07-17 | 2015-12-16 | 浙江锦尚合成革有限公司 | Anti-microbial synthetic leather and preparation method thereof |
| CN105176053B (en) * | 2015-07-17 | 2018-06-19 | 浙江锦尚合成革有限公司 | A kind of synthetic leather slurry and preparation method thereof |
| CN106386870A (en) * | 2016-04-30 | 2017-02-15 | 安吉云界生物科技有限公司 | Nuisance-free plant disease preventive protection preparation and preparation method thereof |
| CN106256205A (en) * | 2016-09-26 | 2016-12-28 | 武汉市纳米金磁科技有限责任公司 | A kind of preparation method carrying silver titanium oxide antimicrobial powder |
| CN106577750A (en) * | 2016-11-29 | 2017-04-26 | 青岛海之星生物科技有限公司 | Preparing method for titanium-dioxide composite nanometer antibacterial material and product thereof |
| CN107441936A (en) * | 2017-08-31 | 2017-12-08 | 河海大学 | A kind of Ag TiO2/ SPES mixing milipore filters and its preparation method and application |
| CN108636101A (en) * | 2018-04-27 | 2018-10-12 | 广东自由能科技股份有限公司 | A kind of sterilizing deodoring agent and preparation method thereof and the application in aerosol |
| CN109896545B (en) * | 2019-03-14 | 2021-08-20 | 东北石油大学 | Hollow shell type titanium dioxide nano material, silver-loaded hollow shell type titanium dioxide nano material and preparation method thereof |
| CN111764168A (en) * | 2020-05-25 | 2020-10-13 | 浙江丑鸭实业有限公司 | Finishing process of antibacterial protective clothing |
| CN111454429A (en) * | 2020-06-10 | 2020-07-28 | 泉州玺堡家居科技有限公司 | MDI (diphenylmethane diisocyanate) tapping technology-based high-breathability slow-resilience cotton and preparation method thereof |
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Denomination of invention: Preparation method of an inorganic antibacterial agent loaded with silver on titanium dioxide Effective date of registration: 20201216 Granted publication date: 20160817 Pledgee: Jiangsu Zijin Rural Commercial Bank Co.,Ltd. Chengxi Branch Pledgor: Nanjing Fenghaohua Food Supply Chain Management Co.,Ltd. Registration number: Y2020980009450 |
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