CN104194424B - A kind of preparation method of medical medical apparatus and instruments metal antibacterial coating - Google Patents

A kind of preparation method of medical medical apparatus and instruments metal antibacterial coating Download PDF

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CN104194424B
CN104194424B CN201410480459.6A CN201410480459A CN104194424B CN 104194424 B CN104194424 B CN 104194424B CN 201410480459 A CN201410480459 A CN 201410480459A CN 104194424 B CN104194424 B CN 104194424B
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instruments
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周海燕
姜华
刘军
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Liu Jun
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SHENYANG WOXINYUAN TRADING Co Ltd
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Abstract

The preparation method of a kind of medical medical apparatus and instruments metal antibacterial coating belongs to the coating technology field to metal material, specifically, relates to the preparation method of a kind of medical medical apparatus and instruments metal antibacterial coating.After titanate esters is first dissolved with solvent by the present invention, whipping process is sequentially added into acid, water, silicon-containing compound, dispersant, silver salt and synergist, stirs evenly prepared titanium oxide coating.Again the medical medical apparatus and instruments metal being immersed in titanium oxide coating is the most uniformly proposed, dry, dry up or dry;Then, the above-mentioned metal after film is placed in Muffle furnace calcining;Naturally cool to room temperature after taking-up, obtain the antimicrobial coating of medical medical apparatus and instruments metal.The present invention uses the titanium oxide-coating film of argentiferous as anti-biotic material, and add silicon-containing compound and synergist, have preparation method be simple and convenient to operate, the feature of low cost, good anti-bacterial effect, be possible to prevent class coating material in use to come off, and made coating can preserve for a long time.

Description

A kind of preparation method of medical medical apparatus and instruments metal antibacterial coating
Technical field
The invention belongs to the coating technology field to metal material, specifically, relate to the preparation method of a kind of medical medical apparatus and instruments metal antibacterial coating.
Background technology
Metal ion is respectively provided with strong and weak different antibacterial effect, wherein antibiotic property size is ordered as: Hg > Ag > Cd > Cu > Zn > Fe > Ni etc., but it is inadequate for only having antibiotic property, also require that human body is not damaged by it, and the safety of metal ion is ordered as: Ag > Co > Ni > Al > Zn > Cu=Fe > Mn > Sn > Ba > Mg > Ca, so the result that safety and antibiotic property are considered jointly, best with Ag ion, next to that Cu system and Zn system.
Research proves to add in molten steel the anti-bacteria stainless steel that antibacterial metal is obtained by steel-making mode, can obtain good antibacterial effect, and this anti-biotic material is prone to processing, function admirable.Anti-bacteria stainless steel mainly has 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 tradition rustless steel, and in the fabrication process, take special heat treatment so that rustless steel from surface to the copper precipitate that inside disperse is the trickleest.
Add silver anti-bacteria stainless steel: be the anti-bacteria stainless steel adding silver under premise based on steel and refining.Escherichia coli and staphylococcus aureus had the highest antibiotic property.Even if particularly after grinding, processing and be exposed to hot environment, sterilization rate still can reach more than 99%.Add silver anti-bacteria stainless steel compared with the antibiotic property adding copper anti-bacteria stainless steel, add silver anti-bacteria stainless steel even across also not interfering with its antibiotic property after surface grinding, and add copper anti-bacteria stainless steel antibiotic property after surface grinding and just have decline.Therefore, with adding the various devices that silver anti-bacteria stainless steel is made, after welding, its antibiotic property and corrosion resistance are also ensured that.It can be widely used for all various aspects requiring antibiotic property effect such as kitchen utensils, washing machine, home appliances, medical apparatus.
But, both anti-bacteria stainless steels are all to add silver or copper when steel-making in molten steel and obtain, and for only having only to for surface has the metal of medical medical apparatus and instruments of anti-microbial property, cost is the highest.For this reason, it is necessary to develop a kind of the antimicrobial coating in metal surface with anti-microbial property, and the titania coating of argentiferous of the present invention just has easy construction, with low cost, effective feature.
Titanium oxide is a kind of n-type semiconductor, and after it is excited higher than the light of energy gap by energy, the electronics in titanium oxide produces energy level transition, forms redox photocatalytic effect on the surface of titanium oxide, can be decomposed by Organic substance.Titanium oxide is a kind of good stability, good biocompatibility, nontoxic, pollution-free and can the material of the most long-acting use.In patent 201210568067.6, disclosing one " method that oral cavity CoCr alloy material surface prepares silver-containing antibacterial coating ", the raw material that it uses is titanate esters and silver salt.In patent 201010153504.9, disclose one " a kind of Ag doping titanium deoxid film and preparation method thereof ".Both approaches is all not added with silicon compound, and the specific surface area of the coating obtained is the most little.
Summary of the invention
It is an object of the invention to provide the antimicrobial coating of a kind of medical medical apparatus and instruments metal.
Further object is that the preparation method of the antimicrobial coating that a kind of medical medical apparatus and instruments metal is provided.
For realizing the above-mentioned purpose of the present invention, the present invention adopts the following technical scheme that.
After medical medical apparatus and instruments metallic surface, the titanium oxide antimicrobial coating of coating argentiferous, first it is dried and calcines again.Described method includes following two step.
(1), after titanate esters being dissolved with solvent, whipping process is sequentially added into acid, water, silicon-containing compound, dispersant, silver salt and synergist, stirs evenly prepared titanium oxide coating.
(2) the most uniformly being proposed by the medical medical apparatus and instruments metal being immersed in step (1) gained titanium oxide coating, dry, dry up or 30-80 DEG C of drying, this process can be repeatedly to obtain the coating (thickness is usually less than 10 microns) of different coating thickness;Then, the above-mentioned metal after film is placed in Muffle furnace, calcines 1-60 hour in 100-300 DEG C;Naturally cool to room temperature after taking-up, obtain the antimicrobial coating of medical medical apparatus and instruments metal.
According to the method described in step (1), described metatitanic acid fat is one or more in butyl titanate, titanium propanolate, tetraethyl titanate, and mass fraction shared in coating is 0.1-10%.
According to the method described in step (1), described solvent is one or more in methanol, ethanol, propanol, butanol, acetone, and mass fraction shared in coating is 65-99%.
According to the method described in step (1), described acid is one or more in hydrochloric acid, Fluohydric acid., nitric acid, formic acid, acetic acid, citric acid, tartaric acid, and mass fraction shared in coating is 0.1-10%.
According to the method described in step (1), described silicon-containing compound is one or more in silester, methyl trichlorosilane, MTES, MTMS, propyl trimethoxy silicane and VTES, and mass fraction shared in coating is 0.1-10%;The addition of silicon-containing compound can strengthen the film adhesiveness to parent metal material, and provides bigger serface, thus improves antibacterial speed.
According to the method described in step (1), described dispersant is at least one in triazole, BTA, methyl benzotriazazole, and mass fraction shared in coating is 0.001-1%.It may ensure that coating does not turns black after being irradiated by light during storage or use, do not produce precipitation.
According to the method described in step (1), described silver salt is silver nitrate, and mass fraction shared in coating is 0.001-1%.
According to the method described in step (1), described synergist is at least one in zirconium nitrate, zirconium oxychloride, nickel nitrate, zinc nitrate, zinc chloride, chloroplatinic acid, mass fraction shared in coating is 0.01-5%, they can improve the antibacterial effect of film, especially enhances coating antibacterial effect in the dark.
The present invention uses the titanium oxide-coating film of argentiferous as anti-biotic material, and add silicon-containing compound and synergist, have preparation method be simple and convenient to operate, the feature of low cost, good anti-bacterial effect, be possible to prevent class coating material in use to come off, and made coating can preserve for a long time.
Detailed description of the invention
Below in conjunction with specific embodiment, such scheme is described further.It should be understood that these embodiments are for illustrating that the present invention is not limited to limit the example of the present invention.The implementation condition used in embodiment further can be adjusted according to practical situation, and not marked implementation condition is usually the condition in routine test.
Embodiment 1.
Preparation titanium oxide coating: under stirring, it is sequentially added into ethanol, butanol, butyl titanate, nitric acid, silester, triazole, silver nitrate and zinc nitrate, addition is 70%, 21.435%, 5%, 1.5%, 2%, 0.01%, 0.05%, 0.005% respectively, and stirring 5h prepares titanium oxide coating.
By medical medical apparatus and instruments immersion metal after titanium oxide coating 5 minutes, then the most uniformly proposing this metal with the speed of 1-5cm/min, 80 DEG C are dried 1 hour.Then, this metal is placed in Muffle furnace, calcines 4 hours in 150 DEG C.Naturally cool to room temperature after taking-up, obtain medical medical apparatus and instruments metal antibacterial coating.This coating surface is smooth, is still underlying metal material color, does not turns black, good anti-bacterial effect, to staphylococcus aureus, colibacillary antibiotic rate more than 99.98%.
The examining report of titanium oxide antimicrobial coating.
Detection 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.
Analyze testing result.
Titanium oxide antimicrobial coating is applied to the examining report of medical suture needle.
Detection unit: State Food and Drug Administration Hangzhou medical apparatus and instruments quality surveillance inspection center.
Survey report is numbered: G20140230.
Sample ID: medical medical apparatus and instruments metal coating sewing needle.
Specification: △ 1/2 7 × 17.
Sample size: 17.
By inspection unit/production unit: Wo Xin source, Shenyang commerce and trade company limited.
Test basis: YY0043-2005.
Inspection project: 4.1.1 force of piercing, 4.1.2 cutting force, 4.2.1 hardness, 4.2.2 elasticity, 4.2.3 toughness, 4.3.3 surface roughness.
Testing result is as follows.
Test result: the examined project of test sample meets the requirement of YY0043-2005 " medical suture needle " standard.
Titanium oxide antimicrobial coating is applied to the examining report of knife blade.
Detection unit: State Food and Drug Administration Hangzhou medical apparatus and instruments quality surveillance inspection center.
Survey report is numbered: G20140229.
Sample ID: medical medical apparatus and instruments metal coating knife blade.
Specification: 11#.
Sample size: 18.
By inspection unit/production unit: Wo Xin source, Shenyang commerce and trade company limited.
Test basis: YY0174-2005 " knife blade " standard.
Inspection project: 4.2.1 outward appearance (roughness), 4.3 sharpness, 4.4.1 blade stiffness, 4.4.2 blade are elastic.
Testing result is as follows.
Test result: the examined project of test sample meets the requirement of YY0174-2005 " knife blade " standard.
Embodiment 2.
Preparation titanium oxide coating: under stirring, it is sequentially added into ethanol, isopropanol, butanol, metatitanic acid isopropyl alcohol ester, hydrochloric acid, methyl trichlorosilane, BTA, silver nitrate and zirconium nitrate, addition is 60%, 21%, 12.96%, 4%, 0.5%, 1.5%, 0.005%, 0.005%, 0.03% respectively, and stirring 7h prepares titanium oxide coating.
By medical medical apparatus and instruments immersion metal after titanium oxide coating 10 minutes, then the most uniformly proposing this metal with the speed of 1-5cm/min, blower fan blows 1.5 hours.After drying, this metal is placed in Muffle furnace, calcines 8 hours in 120 DEG C.Naturally cool to room temperature after taking-up, obtain medical medical apparatus and instruments metal antibacterial coating.This coating surface is smooth, is still underlying metal material color, does not turns black, good anti-bacterial effect.
Embodiment 3.
Preparation titanium oxide coating: under stirring, it is sequentially added into methanol, butanol, butyl titanate, hydrochloric acid, silester, methyl benzotriazazole, silver nitrate and zirconium oxychloride, addition is 80%, 13.454%, 3%, 1.5%, 2%, 0.003%, 0.003%, 0.04% respectively, and stirring 5h prepares titanium oxide coating.
By medical medical apparatus and instruments immersion metal after titanium oxide coating 10 minutes, then the most uniformly proposing this metal with the speed of 1-5cm/min, 50 DEG C are dried 3 hours.After drying, this metal is placed in Muffle furnace, calcines 1 hour in 230 DEG C.Naturally cool to room temperature after taking-up, obtain medical medical apparatus and instruments metal antibacterial coating.This coating surface is smooth, is still underlying metal material color, does not turns black, good anti-bacterial effect.
Embodiment 4.
Preparation titanium oxide coating: under stirring, it is sequentially added into ethanol, butyl titanate, nitric acid, citric acid, VTES, BTA, silver nitrate, nickel nitrate and chloroplatinic acid, addition is 92.9395%, 2.5%, 1.5%, 0.05%, 3%, 0.003%, 0.0035%, 0.003%, 0.001% respectively, and stirring 5h prepares titanium oxide coating.
By medical medical apparatus and instruments immersion metal after titanium oxide coating 10 minutes, then the most uniformly proposing this metal with the speed of 1-5cm/min, 50 DEG C are dried 3 hours.After drying, this metal is placed in Muffle furnace, calcines 1 hour in 240 DEG C.Naturally cool to room temperature after taking-up, obtain medical medical apparatus and instruments metal antibacterial coating.This coating surface is smooth, is still underlying metal material color, does not turns black, good anti-bacterial effect.

Claims (2)

1. the preparation method of a medical medical apparatus and instruments metal antibacterial coating, it is characterised in that: preparation method includes following two step,
(1), after titanate esters being dissolved with solvent, whipping process is sequentially added into acid, water, silicon-containing compound, dispersant, silver salt and synergist, stirs evenly prepared titanium oxide coating;
(2) the most uniformly being proposed by the medical medical apparatus and instruments metal being immersed in step (1) gained titanium oxide coating, dry, dry up or 30-80 DEG C of drying, this process can be repeatedly to obtain the coating of different coating thickness, and its thickness is less than 10 microns;Then, the above-mentioned metal after film is placed in Muffle furnace, calcines 1-60 hour in 100-300 degree;Naturally cool to room temperature after taking-up, obtain the antimicrobial coating of medical medical apparatus and instruments metal;
Described titanate esters is one or more in butyl titanate, titanium propanolate, tetraethyl titanate;
Described solvent is one or more in methanol, ethanol, propanol, butanol, acetone;
Described acid is one or more in hydrochloric acid, Fluohydric acid., nitric acid, formic acid, acetic acid, citric acid, tartaric acid;
Described silicon-containing compound is one or more in silester, methyl trichlorosilane, MTES, MTMS, propyl trimethoxy silicane and VTES;
Described dispersant is at least one in triazole, BTA, methyl benzotriazazole;
Described silver salt is silver nitrate;
Described synergist is at least one in zirconium nitrate, zirconium oxychloride, nickel nitrate, zinc nitrate, zinc chloride, chloroplatinic acid.
The preparation method of medical medical apparatus and instruments metal antibacterial coating the most as claimed in claim 1, it is characterised in that: described titanate esters mass fraction shared by coating is 0.1-10%;Described solvent mass fraction shared by coating is 65-99%;Described acid mass fraction shared by coating is 0.1-10%;Described silicon-containing compound mass fraction shared by coating is 0.1-10%;Described dispersant mass fraction shared by coating is 0.001-1%;Described silver salt mass fraction shared by coating is 0.001-1%;Described synergist mass fraction shared by coating is 0.01-5%.
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Effective date of registration: 20210412

Address after: 110000 5-1-1, no.9b 5, beiyixi Road, Tiexi District, Shenyang City, Liaoning Province

Patentee after: Liu Jun

Address before: 110021 No.5, 10th floor, building 1, No.57 Xinggong North Street, Tiexi District, Shenyang City, Liaoning Province

Patentee before: SHENYANG WOXINYUAN TRADING Co.,Ltd.