CN104194424A - Preparation method of antimicrobial coating for metal of medical equipment - Google Patents
Preparation method of antimicrobial coating for metal of medical equipment Download PDFInfo
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Abstract
The invention relates to a preparation method of an antimicrobial coating for metal of medical equipment and belongs to the technical field of plating of metal materials. The preparation method comprises the following steps: after titanate is dissolved with a solvent, adding acid, water, silicon-contained compounds, dispersing agents, silver salt and synergists in sequence in the mixing process and uniformly stirring to prepare a titanium oxide coating; upwardly and uniformly taking out the medical equipment metal immersed into the titanium oxide coating, airing, blowing or drying; then, putting the coated metal into a muffle furnace to calcine; taking out, naturally cooling to a room temperature and obtaining the antimicrobial coating on the metal of the medical equipment. According to the preparation method, as the titanium oxide coating containing silver is adopted as an antimicrobial material, and the silicon-containing compounds and the synergists are added, the preparation method has the characteristics that the preparation method is simple, the operation is convenient, the cost is low, and the antibacterial effect is good, the falling-off of coating materials can be prevented during the use, and the prepared coating can be stored for a long time.
Description
Technical field
The invention belongs to the coating technology field to metallic substance, specifically, relate to a kind of preparation method of medical medicine equipment metal antibacterial coating.
Background technology
Metal ion all has strong and weak different antibacterial effects, wherein the sequence of germ resistance size is: Hg > Ag > Cd > Cu > Zn > Fe > Ni etc., inadequate but only there is germ resistance, also require it human body not to be damaged, and the security of metal ion sequence is: Ag > Co > Ni > Al > Zn > Cu=Fe > Mn > Sn > Ba > Mg > Ca, so with regard to security and the common result of considering of germ resistance, best with Ag ion, next is Cu system and Zn system.
Studies have shown that the anti-bacteria stainless steel that adds antibacterial metal to obtain by steel-making mode in molten steel, can obtain good antibacterial effect, and this anti-biotic material is easy to processing, excellent property.Anti-bacteria stainless steel mainly contains and adds copper anti-bacteria stainless steel and Jia Yin anti-bacteria stainless steel.
Add copper anti-bacteria stainless steel: be to add metallic copper in traditional stainless steel, and in manufacturing processed, take special thermal treatment, thereby make stainless steel on surface to the even trickle copper precipitate of inner disperse.
Add silver-colored anti-bacteria stainless steel: be to be under basic prerequisite, to add the anti-bacteria stainless steel that silver is refined at steel.Intestinal bacteria and streptococcus aureus are had to very high germ resistance.Even particularly through grinding, process and be exposed to after hot environment, sterilization rate still can reach more than 99%.Compared with adding silver-colored anti-bacteria stainless steel and adding the germ resistance of copper anti-bacteria stainless steel, after surface grinding, can not affect its germ resistance even if add silver-colored anti-bacteria stainless steel yet, just have decline and add copper anti-bacteria stainless steel germ resistance after surface grinding.Therefore,, with adding the various devices that silver-colored anti-bacteria stainless steel is made, after welding, also can guarantee its germ resistance and erosion resistance.It can be widely used in all respects that require germ resistance effect such as kitchen utensils, washing machine, home appliances, medical apparatus.
But these two kinds of anti-bacteria stainless steels are all add silver or copper and obtain in molten steel in when steel-making, for only having for the metal that the medical medicine equipment of anti-microbial property uses on surface, cost is very high.For this reason, be necessary to develop a kind of the antimicrobial coating in metallic surface with anti-microbial property, and the titania coating of argentiferous of the present invention just have easy construction, with low cost, effective feature.
Titanium oxide is a kind of N-shaped semiconductor material, and when it is subject to after the optical excitation of energy higher than energy gap, the electron production energy level transition in titanium oxide, forms redox photocatalytic effect on the surface of titanium oxide, can be by organic substance decomposing.Titanium oxide is a kind of good stability, good biocompatibility, nontoxic, the pollution-free and material of long-acting use repeatedly.In patent 201210568067.6, a kind of " oral cavity CoCr alloy material surface is prepared the method for silver-containing antibacterial coating " disclosed, the raw material that it adopts is titanic acid ester and silver salt.In patent 201010153504.9, a kind of " a kind of silver-colored titania-doped film and preparation method thereof " disclosed.These two kinds of methods are not all added silicon compound, and the specific surface area of the coating obtaining is all little.
Summary of the invention
The object of the present invention is to provide a kind of antimicrobial coating of medical medicine equipment metal.
Another object of the present invention is the preparation method of the antimicrobial coating that a kind of medical medicine equipment metal is provided.
For realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme.
At medical medicine equipment metallic surface, apply after the titanium oxide antimicrobial coating of argentiferous, be first dried and calcine again.Described method comprises following two steps.
(1) by titanic acid ester with after dissolution with solvents, in whipping process, add successively acid, water, silicon-containing compound, dispersion agent, silver salt and synergistic agent, stir evenly and make titanium oxide coating.
(2) the medical medicine equipment metal that will be immersed in step (1) gained titanium oxide coating upwards evenly proposes, dry, dry up or 30-80 DEG C of oven dry, this process can be repeatedly to obtain the coating (thickness is generally 10 microns below) of different coating thicknesses; Then, the above-mentioned metal after film is placed in to retort furnace, in 100-300 DEG C of calcining 1-60 hour; After taking-up, naturally cool to room temperature, obtain the antimicrobial coating of medical medicine equipment metal.
According to method step (1) Suo Shu, described metatitanic acid fat is one or more in butyl (tetra) titanate, titanium propanolate, titanium ethanolate, and in coating, shared massfraction is 0.1-10%.
According to method step (1) Suo Shu, described solvent is one or more in methyl alcohol, ethanol, propyl alcohol, butanols, acetone, and in coating, shared massfraction is 65-99%.
According to method step (1) Suo Shu, described acid is one or more in hydrochloric acid, hydrofluoric acid, nitric acid, formic acid, acetic acid, citric acid, tartrate, and in coating, shared massfraction is 0.1-10%.
According to method step (1) Suo Shu, described silicon-containing compound is one or more in tetraethyl silicate, METHYL TRICHLORO SILANE, Union carbide A-162, methyltrimethoxy silane, propyl trimethoxy silicane and vinyltriethoxysilane, and in coating, shared massfraction is 0.1-10%; Adding of silicon-containing compound can strengthen the adhesivity of film to parent metal material, and bigger serface is provided, thereby improves antibacterial speed.
According to method step (1) Suo Shu, described dispersion agent is at least one in triazole, benzotriazole, methyl benzotriazazole, and in coating, shared massfraction is 0.001-1%.It can ensure not turn black after coating is subject to irradiate light in storage or use procedure, does not produce precipitation.
According to method step (1) Suo Shu, described silver salt is Silver Nitrate, and in coating, shared massfraction is 0.001-1%.
According to method step (1) Suo Shu, described synergistic agent is at least one in zirconium nitrate, zirconium oxychloride, nickelous nitrate, zinc nitrate, zinc chloride, Platinic chloride, in coating, shared massfraction is 0.01-5%, they can improve the antibacterial effect of film, have especially strengthened coating antibacterial effect in the dark.
The present invention adopts the titanium oxide-coating film of argentiferous as anti-biotic material, and add silicon-containing compound and synergistic agent, have that preparation method is simple, easy to operate, cost is low, the feature of good anti-bacterial effect, can prevent that class coating material from use coming off, and made coating can be preserved for a long time.
Embodiment
Below in conjunction with specific embodiment, such scheme is described further.It should be understood that these embodiment are not limited to limit example of the present invention for the present invention is described.The implementation condition adopting in embodiment can be done further adjustment according to practical situation, and not marked implementation condition is generally the condition in routine test.
Embodiment 1.
Preparation titanium oxide coating: under stirring, add successively ethanol, butanols, butyl (tetra) titanate, nitric acid, tetraethyl silicate, triazole, Silver Nitrate and zinc nitrate, addition is respectively 70%, 21.435%, 5%, 1.5%, 2%, 0.01%, 0.05%, 0.005%, stirs 5h and makes titanium oxide coating.
Medical medicine equipment immersion metal after 5 minutes, is then upwards evenly proposed to this metal with the speed of 1-5cm/min in titanium oxide coating, and 80 DEG C are dried 1 hour.Then, this metal is placed in to retort furnace, in 150 DEG C of calcinings 4 hours.After taking-up, naturally cool to room temperature, obtain medical medicine equipment metal antibacterial coating.This coatingsurface is smooth, is still underlying metal material color, do not turn black, good anti-bacterial effect, to streptococcus aureus, colibacillary antibiotic rate more than 99.98%.
The examining report of titanium oxide antimicrobial coating.
Detect unit: microbiological analysis inspection center of Guangdong Province.
Client: Wo Xin source, Shenyang commerce and trade company limited.
Report number: 2013FM4650.
Detection method: JIS Z 2801:2010.
Analyzing and testing result.
Titanium oxide antimicrobial coating is applied to the examining report of medical suture needle.
Detect unit: Hangzhou medicine equipment quality surveillance inspection center of State Food and Drug Administration.
Survey report numbering: G20140230.
Sample title: medical medicine equipment metallic coating sewing needle.
Specification: △ 1/2 7 × 17.
Sample size: 17.
Shou Jian unit/production unit: Wo Xin source, Shenyang commerce and trade company limited.
Test basis: YY0043-2005.
Interventions Requested: 4.1.1 pierces through power, 4.1.2 cutting force, 4.2.1 hardness, 4.2.2 elasticity, 4.2.3 toughness, 4.3.3 surfaceness.
Detected result is as follows.
Test result: test sample institute inspection project meets the requirement of YY0043-2005 " medical suture needle " standard.
Titanium oxide antimicrobial coating is applied to the examining report of knife blade.
Detect unit: Hangzhou medicine equipment quality surveillance inspection center of State Food and Drug Administration.
Survey report numbering: G20140229.
Sample title: medical medicine equipment metallic coating knife blade.
Specification: 11#.
Sample size: 18.
Shou Jian unit/production unit: Wo Xin source, Shenyang commerce and trade company limited.
Test basis: YY0174-2005 " knife blade " standard.
Interventions Requested: 4.2.1 outward appearance (roughness), 4.3 sharpness, 4.4.1 blade hardness, 4.4.2 blade elasticity.
Detected result is as follows.
Test result: test sample institute inspection project meets the requirement of YY0174-2005 " knife blade " standard.
Embodiment 2.
Preparation titanium oxide coating: under stirring, add successively ethanol, Virahol, butanols, metatitanic acid isopropyl alcohol ester, hydrochloric acid, METHYL TRICHLORO SILANE, benzotriazole, Silver Nitrate and zirconium nitrate, addition is respectively 60%, 21%, 12.96%, 4%, 0.5%, 1.5%, 0.005%, 0.005%, 0.03%, stirs 7h and makes titanium oxide coating.
Medical medicine equipment immersion metal after 10 minutes, is then upwards evenly proposed to this metal with the speed of 1-5cm/min in titanium oxide coating, and blower fan blows 1.5 hours.After dry, this metal is placed in to retort furnace, in 120 DEG C of calcinings 8 hours.After taking-up, naturally cool to room temperature, obtain medical medicine equipment metal antibacterial coating.This coatingsurface is smooth, is still underlying metal material color, do not turn black, and good anti-bacterial effect.
Embodiment 3.
Preparation titanium oxide coating: under stirring, add successively methyl alcohol, butanols, butyl (tetra) titanate, hydrochloric acid, tetraethyl silicate, methyl benzotriazazole, Silver Nitrate and zirconium oxychloride, addition is respectively 80%, 13.454%, 3%, 1.5%, 2%, 0.003%, 0.003%, 0.04%, stirs 5h and makes titanium oxide coating.
Medical medicine equipment immersion metal after 10 minutes, is then upwards evenly proposed to this metal with the speed of 1-5cm/min in titanium oxide coating, and 50 DEG C are dried 3 hours.After dry, this metal is placed in to retort furnace, in 230 DEG C of calcinings 1 hour.After taking-up, naturally cool to room temperature, obtain medical medicine equipment metal antibacterial coating.This coatingsurface is smooth, is still underlying metal material color, do not turn black, and good anti-bacterial effect.
Embodiment 4.
Preparation titanium oxide coating: under stirring, add successively ethanol, butyl (tetra) titanate, nitric acid, citric acid, vinyltriethoxysilane, benzotriazole, Silver Nitrate, nickelous nitrate and Platinic chloride, addition is respectively 92.9395%, 2.5%, 1.5%, 0.05%, 3%, 0.003%, 0.0035%, 0.003%, 0.001%, stirs 5h and makes titanium oxide coating.
Medical medicine equipment immersion metal after 10 minutes, is then upwards evenly proposed to this metal with the speed of 1-5cm/min in titanium oxide coating, and 50 DEG C are dried 3 hours.After dry, this metal is placed in to retort furnace, in 240 DEG C of calcinings 1 hour.After taking-up, naturally cool to room temperature, obtain medical medicine equipment metal antibacterial coating.This coatingsurface is smooth, is still underlying metal material color, do not turn black, and good anti-bacterial effect.
Claims (9)
1. a preparation method for medical medicine equipment metal antibacterial coating, is characterized in that: preparation method of the present invention comprises following two steps,
(1) by titanic acid ester with after dissolution with solvents, in whipping process, add successively acid, water, silicon-containing compound, dispersion agent, silver salt and synergistic agent, stir evenly and make titanium oxide coating;
(2) the medical medicine equipment metal that will be immersed in step (1) gained titanium oxide coating upwards evenly proposes, dry, dry up or 30-80 DEG C of oven dry, this process can be repeatedly to obtain the coating (thickness is generally 10 microns below) of different coating thicknesses; Then, the above-mentioned metal after film is placed in to retort furnace, in 100-300 degree calcining 1-60 hour; After taking-up, naturally cool to room temperature, obtain the antimicrobial coating of medical medicine equipment metal.
2. the preparation method of medical medicine equipment metal antibacterial coating claimed in claim 1, is characterized in that: described phthalic acid ester is one or more in butyl (tetra) titanate, titanium propanolate, titanium ethanolate, and in coating, shared massfraction is 0.1-10%.
3. the preparation method of medical medicine equipment metal antibacterial coating claimed in claim 1, is characterized in that: described solvent is one or more in methyl alcohol, ethanol, propyl alcohol, butanols, acetone, and in coating, shared massfraction is 65-99%.
4. the preparation method of medical medicine equipment metal antibacterial coating claimed in claim 1, it is characterized in that: described acid is one or more in hydrochloric acid, hydrofluoric acid, nitric acid, formic acid, acetic acid, citric acid, tartrate, in coating, shared massfraction is 0.1-10%.
5. preparation method claimed in claim 1, it is characterized in that: described silicon-containing compound is one or more in tetraethyl silicate, METHYL TRICHLORO SILANE, Union carbide A-162, methyltrimethoxy silane, propyl trimethoxy silicane and vinyltriethoxysilane, in coating, shared massfraction is 0.1-10%; Adding of silicon-containing compound can strengthen the adhesivity of film to parent metal material, and bigger serface is provided, thereby improves antibacterial speed.
6. the preparation method of medical medicine equipment metal antibacterial coating claimed in claim 1, is characterized in that: described dispersion agent is at least one in triazole, benzotriazole, methyl benzotriazazole, and in coating, shared massfraction is 0.001-1%; It can ensure not turn black after coating is subject to irradiate light in storage or use procedure, does not produce precipitation.
7. the preparation method of medical medicine equipment metal antibacterial coating claimed in claim 1, is characterized in that: described silver salt can be Silver Nitrate, and in coating, shared ratio is 0.001-1%.
8. the preparation method of medical medicine equipment metal antibacterial coating claimed in claim 1, it is characterized in that: described synergistic agent is at least one in zirconium nitrate, zirconium oxychloride, nickelous nitrate, zinc nitrate, zinc chloride, Platinic chloride, in coating, shared massfraction is 0.01-5%, they can improve the antibacterial effect of film, have especially strengthened coating antibacterial effect in the dark.
9. the preparation method of the medical medicine equipment metal antibacterial coating described in claim 1-8, it is characterized in that: preparation titanium oxide coating: follow stirring, add successively ethanol, butanols, butyl (tetra) titanate, nitric acid, tetraethyl silicate, triazole, Silver Nitrate and zinc nitrate, addition is respectively 70%, 21.435%, 5%, 1.5%, 2%, 0.01%, 0.05%, 0.05%, stirs 5h and makes titanium oxide coating;
Medical medicine equipment immersion metal after 5 minutes, is then upwards evenly proposed to this metal with the speed of 1-5cm/min in titanium oxide coating, and 80 DEG C are dried 1 hour; Then, this metal is placed in to retort furnace, in 150 DEG C of calcinings 4 hours; After taking-up, naturally cool to room temperature, obtain medical medicine equipment metal antibacterial coating; This coatingsurface is smooth, is still underlying metal material color, do not turn black, good anti-bacterial effect, to streptococcus aureus, colibacillary antibiotic rate more than 99.98%.
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| CN106361412A (en) * | 2016-09-14 | 2017-02-01 | 泰山医学院 | Medical intelligent surgical knife |
| CN106581782A (en) * | 2016-12-13 | 2017-04-26 | 天津丰茂科技有限公司 | ALD technology-based energy saving method for producing oxidation layer on medical device |
| CN107236974A (en) * | 2017-06-13 | 2017-10-10 | 合肥聪亨新型建材科技有限公司 | A kind of preparation method of antibiotic property composite material coating |
| CN107822674A (en) * | 2017-12-25 | 2018-03-23 | 苏州塔比诺机电有限公司 | A kind of electro-mechanical surgical device |
| WO2018056900A1 (en) | 2016-09-20 | 2018-03-29 | Agency For Science, Technology And Research | Redox active metal/metal oxide composites for antimicrobial applications |
| CN107936630A (en) * | 2017-12-01 | 2018-04-20 | 河南省健琪医疗器械有限公司 | A kind of medical instrument special surface antimicrobial coating and its preparation process |
| CN107951545A (en) * | 2017-12-25 | 2018-04-24 | 苏州塔比诺机电有限公司 | A kind of aseptic electric operation device |
| CN107981701A (en) * | 2016-10-26 | 2018-05-04 | 佛山市顺德区美的电热电器制造有限公司 | Titanium-based carries silver-colored titanium dioxide composite antibacterial base material and preparation method thereof and titanium-based cookware and preparation method thereof |
| CN108950498A (en) * | 2018-09-04 | 2018-12-07 | 合肥久新不锈钢厨具有限公司 | A kind of preparation method of anti-bacteria stainless steel plate |
| CN112322160A (en) * | 2020-10-27 | 2021-02-05 | 郭竹春 | Environment-friendly formaldehyde-removing coating |
| WO2021097667A1 (en) * | 2019-11-19 | 2021-05-27 | 南京先进生物材料与过程装备研究院有限公司 | Biomedical material surface polymer-based coating |
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| CN106361412A (en) * | 2016-09-14 | 2017-02-01 | 泰山医学院 | Medical intelligent surgical knife |
| JP2019529711A (en) * | 2016-09-20 | 2019-10-17 | エージェンシー フォー サイエンス， テクノロジー アンド リサーチ | Redox-active metal / metal oxide composites for antibacterial applications |
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| JP2021165433A (en) * | 2016-09-20 | 2021-10-14 | エージェンシー フォー サイエンス， テクノロジー アンド リサーチ | Metal/metal oxide composition with oxidation-reduction activity for antibacterial application |
| CN109689932A (en) * | 2016-09-20 | 2019-04-26 | 新加坡科技研究局 | Redox active metal/metal oxide compound for antimicrobial application |
| CN107981701A (en) * | 2016-10-26 | 2018-05-04 | 佛山市顺德区美的电热电器制造有限公司 | Titanium-based carries silver-colored titanium dioxide composite antibacterial base material and preparation method thereof and titanium-based cookware and preparation method thereof |
| CN106581782A (en) * | 2016-12-13 | 2017-04-26 | 天津丰茂科技有限公司 | ALD technology-based energy saving method for producing oxidation layer on medical device |
| CN107236974A (en) * | 2017-06-13 | 2017-10-10 | 合肥聪亨新型建材科技有限公司 | A kind of preparation method of antibiotic property composite material coating |
| CN107936630A (en) * | 2017-12-01 | 2018-04-20 | 河南省健琪医疗器械有限公司 | A kind of medical instrument special surface antimicrobial coating and its preparation process |
| CN107822674A (en) * | 2017-12-25 | 2018-03-23 | 苏州塔比诺机电有限公司 | A kind of electro-mechanical surgical device |
| CN107951545A (en) * | 2017-12-25 | 2018-04-24 | 苏州塔比诺机电有限公司 | A kind of aseptic electric operation device |
| CN108950498A (en) * | 2018-09-04 | 2018-12-07 | 合肥久新不锈钢厨具有限公司 | A kind of preparation method of anti-bacteria stainless steel plate |
| WO2021097667A1 (en) * | 2019-11-19 | 2021-05-27 | 南京先进生物材料与过程装备研究院有限公司 | Biomedical material surface polymer-based coating |
| CN112322160A (en) * | 2020-10-27 | 2021-02-05 | 郭竹春 | Environment-friendly formaldehyde-removing coating |
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