CN104846354A - Antifouling and antibacterial treatment method for titanium and titanium alloy surface - Google Patents
Antifouling and antibacterial treatment method for titanium and titanium alloy surface Download PDFInfo
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Abstract
The invention belongs to the technical field of biological fouling protection, and relates to an antifouling and antibacterial treatment method for a titanium and titanium alloy surface, which comprises the following steps: firstly, performing plasma activation on the titanium or titanium alloy surface, placing above a silane coupling agent and cyclohexane mixed solution, and vacuumizing a dryer for vapor deposition; then, placing titanium metal of which the surface is modified with silane coupling agent in a mixed solution containing dopamine and a hydrochloric acid solution of tris (hydroxymethyl) amino methane hydrochloride, and placing in a flask; adding methylbenzene and triethylamine, introducing nitrogen and dropwise adding bromo-isobutyryl bromide for reaction, then taking out, washing, blow-drying, and placing in another flask; sequentially adding 2,2'-Bipyridine, water, methanol and methy-propylene-acyloxy modified lycine, and then introducing nitrogen continuously; then adding cuprous bromide for performing polymerization, placing in a silver nitrate aqueous solution for reaction, and then washing thoroughly, thus realizing the antifouling and antibacterial treatment for the titanium metal surface. The process is simple, the operation is convenient, the suitable environment condition is wide, the broad-spectrum property is good, and the method has good antifouling and antibacterial performance.
Description
Technical field:
The invention belongs to biodeterioration guard technology field, relate to a kind of antifouling and antibiosis treatment process of titanium or titanium alloy surface, particularly a kind of in titanium or titanium alloy surface chemical modification betaines molecule and silver-colored antifouling and antibiosis treatment process.
Background technology:
Titanium or titanium alloy relies on the biocompatibility of high specific strength, high anti-corrosion and excellence to be widely used in the fields such as boats and ships, oceanographic engineering and biomedicine, comprises oil and gas platform, seawater desalination system, heat exchanging apparatus, medicine equipment and orthopedic material etc.In common used material, the antifouling property of titanium is poor, is easily produced stained by biological attachment, as the sea marine organism pollution on Marine Materials surface, the bacterial adhesion of implantation material surface is stained, the blood coagulation of intravascular stent, the dirt deposition etc. of heat exchanging apparatus pipeline, affects its normal usage energy.Therefore, the antifouling and antibiosis problem of special concern titanium or titanium alloy is needed.
Application antifouling paint is the important means of marine anti-pollution, adopts the anti-pollution measure of stain control agent poisoning can work the mischief to ocean environment, is prohibited or limits use.Environmentally friendly anti-fouling material more and more causes concern, as CN1170020A, (application number is 96110261.6, a kind of low surface energy antifouling coating for seas), (application number is 201010142998.0 to CN101818024A, a kind of emulsion-type organic silicon antifouling paint and preparation method thereof and application) etc. pollution release type organic silicon antifouling material disclosed in patent, (application number is 200610015092.6 to CN101117529A, prevent the low surface energy anti-fouling paint that marine sessile organism is stained) disclosed in comprise the low surface energy anti-fouling paint etc. of tetrafluoroethylene and liquid Capsaicin.But environmentally friendly antifouling paint is comparatively difficult in chemically inert surface of metal titanium application, biocompatibility is also difficult to the requirement reaching embedded material.
Finishing is the function modified important means of surface of metal titanium, and conventional surface modification method has two large classes: physical modification method and chemical modification method.Wherein physical modification method generally adopts plasma spraying, anodic oxidation and differential arc oxidation etc., as CN103834979A, (application number is 201410093637.X, the preparation method of calcium phosphorus silver nanotube array is carried on a kind of medical titanium surface) the disclosed anodizing technology introducing calcium microcosmic salt and antiseptic-germicide, (application number is 201410253398.X to CN104001207A, a kind of medical titanium surface composite coating and preparation method thereof) antibacterial processing method of disclosed titanium surface manganese adulterated TiOx, (application number is 201210081053.1 to CN102580149A, a kind of antimicrobial coating and preparation method thereof) antibacterial processing method of disclosed silver ion implantation titania coating, (application number is 201310033809.X to CN103046101B, a kind of preparation method with the two-stage hole micro-arc biological coating of bacteriostatic action) the surperficial antibacterial processing method etc. be oxidized for three times of disclosed titanium, easily there is bonding force difference in these physical modification methods, surface roughen and the problem such as uneven.Chemical modification does not need complicated equipment usually, technique is relatively simple, cost is lower, it is the function modified ideal method of surface of metal titanium, the antibacterial antitumor treatment process of titanium finishing chitosan as disclosed in CN103463675A (application number is 201310374522.4, a kind of antibacterial antitumor orthopaedic implantation material and preparation method thereof), methotrexate, heparin sodium and Dopamine HCL.But the antifouling and antibiosis such as chitosan and polyoxyethylene glycol molecule antifouling and antibiosis effect when pH value change or temperature variation can be had a strong impact on, and is greatly affected in the use of human body implantation or ocean environment.Betaines zwitterionics (as sulfonic group trimethyl-glycine) have nontoxic, pungency is little, feature to ph stability, modifies the non-specific adsorption that can prevent protein at material surface; Silver is a kind of modal inorganic antiseptic, has efficient, safety, broad-spectrum antimicrobial feature.Therefore, seek a kind of antifouling and antibiosis treatment process of titanium or titanium alloy surface, betaines zwitterionics and silver are combined and can improve the antifouling and antibiosis performance of titanium metal material.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, design provides a kind of antifouling and antibiosis treatment process of titanium or titanium alloy surface, modifies realize antifouling and antibiosis by carrying out betaines molecule and silver chemical in surface of metal titanium.
To achieve these goals, the antifouling and antibiosis treatment process on titanium or titanium alloy surface of the present invention specifically comprises the following steps:
(1), by titanium or titanium alloy surface use acetone and deionized water ultrasonic cleaning, drying successively, then carry out plasma-activated obtaining and activate titanium metal;
(2), by activation titanium metal be positioned over above silane coupling agent-hexanaphthene mixing solutions, in moisture eliminator, vacuumize vapour deposition 2 ~ 48 hours, obtain the titanium metal that finishing has silane coupling agent; Wherein the volume ratio of silane coupling agent and hexanaphthene is 1:1 ~ 10;
(3), Dopamine HCL is dissolved in three (methylol) aminomethane hydrochloride-hydrochloric acid soln, lucifuge stirs and obtains mixing solutions in 0 ~ 24 hour, finishing had the titanium metal of silane coupling agent to be placed in mixing solutions again to stir 1 ~ 48 hour, taking-up flushing dries up, obtain the titanium metal that finishing has Dopamine HCL, wherein the concentration of three (methylol) aminomethane hydrochloride-hydrochloric acid soln is 1 ~ 20mM, and pH value is 7 ~ 9, and the concentration of Dopamine HCL is 0.5 ~ 10g/L;
(4), the titanium metal of Dopamine HCL finishing is had to be placed in flask, add the triethylamine of the toluene of 30 weight parts, 1 weight part, logical nitrogen in ice-water bath also drips the bromo isobutyl acylbromide of 0.9 weight part, and room temperature reaction takes out flushing after 3 ~ 24 hours and dries up; Then another flask is placed in, logical nitrogen is continued after adding the methacryloxy modified betaine of 2 ' 2 dipyridyls of 0.21 weight part, the water of 5 weight parts, the methyl alcohol of 10 weight parts and 1 ~ 10 weight part successively, the cuprous bromide adding 0.08 weight part is again polymerized, and obtains the titanium metal that finishing has trimethyl-glycine molecule;
(5), the titanium metal of trimethyl-glycine molecule finishing is had to put into the silver nitrate aqueous solution of 5g/L, lucifuge stirring reaction 1 ~ 48 hour, taking-up deionized water rinsing is clean, prepare the titanium metal that finishing has trimethyl-glycine molecule and silver, realize the antifouling and antibiosis process on titanium or titanium alloy surface.
Silane coupling agent involved in the present invention comprises aminopropyl triethoxysilane, aminopropyl trimethoxysilane etc. containing amino silane coupling agent.
Methacryloxy modified betaine involved in the present invention comprises the sulphonic acid betaine of methacryloxy modification, the carboxylic acid trimethyl-glycine of methacryloxy modification.
The present invention compared with prior art, the antifouling and antibiosis treatment process of betaines molecule and silver chemical modification is carried out in surface of metal titanium, its technique is simple, easy to operate, Ti-SBMA and the Ti-SBMA-Ag surface uniform of preparation, do not change the original pattern of titanium metal, suitable environment condition is wide, broad spectrum is good, there is good antifouling and antibiosis performance, more than 95% is reached to the inhibiting rate of pinniform boat-shaped algae attachment, to intestinal bacteria and blue or green vibrios far away, there is obvious restraining effect, Ti-SBMA-Ag is to intestinal bacteria, blue or green vibrios far away has significant restraining effect, can be applicable to marine anti-pollution and embedded material antimicrobial treatment.
Accompanying drawing illustrates:
Fig. 1 is that diatom adhiesion test result schematic diagram is carried out on Ti-Dopa, Ti-SBMA surface of the embodiment of the present invention 1 to preparation.
Fig. 2 is that the Ti-SBMA-Ag of the embodiment of the present invention 3 preparation is to intestinal bacteria biocidal property test-results schematic diagram, wherein (a) is for untreated Titanium base is to colibacillary suppression result, and (b) is for Ti-SBMA-Ag is to colibacillary suppression result.
Fig. 3 is that the Ti-SBMA-Ag of the embodiment of the present invention 3 preparation is to blue or green vibrios biocidal property test-results schematic diagram far away, wherein (a) is for untreated Titanium base is to the suppression result of blue or green vibrios far away, and (b) is for Ti-SBMA-Ag is to the suppression result of blue or green vibrios far away.
Embodiment:
Below by embodiment, also the present invention will be further described by reference to the accompanying drawings.
Embodiment 1:
The detailed process of the present embodiment to the antifouling and antibiosis process on titanium or titanium alloy surface is:
(1), by titanium or titanium alloy surface use acetone and deionized water ultrasonic cleaning, drying successively, carry out plasma-activated obtaining and activate titanium metal;
(2), activation titanium metal is placed in above aminopropyl triethoxysilane-hexanaphthene mixing solutions, vapour deposition is vacuumized 12 hours in moisture eliminator, obtain Ti-Apts, in wherein aminopropyl triethoxysilane-hexanaphthene mixing solutions, the volume ratio of aminopropyl triethoxysilane and hexanaphthene is 1:3;
(3) be dissolved in by Dopamine HCL in three (methylol) aminomethane hydrochloride-hydrochloric acid soln, lucifuge stirs and obtains mixing solutions in 12 hours, then Ti-Apts is placed in mixing solutions stirring 24 hours, takes out flushing and dries up, obtain Ti-Dopa; Wherein the concentration of three (methylol) aminomethane hydrochloride-hydrochloric acid soln is 10mM, and pH value is 8.5, and the concentration of Dopamine HCL is 0.5g/L;
(4) Ti-Dopa is placed in flask, in ice-water bath, lead to nitrogen after adding 30 parts of toluene and 1 part of triethylamine and drip 0.9 part of bromo isobutyl acylbromide, room temperature reaction 12 hours, reacted Ti-Dopa taking-up flushing being dried up is placed in another flask, add the carboxylic acid trimethyl-glycine of 0.21 part of 2 ' 2 dipyridyl, 5 parts of water, 10 parts of methyl alcohol and the modification of 5 parts of base acryloxies successively, continue logical nitrogen, then add 0.08 part of cuprous bromide and be polymerized, obtain Ti-SBMA.
The present embodiment for contrast, carries out diatom adhiesion test to Ti-Dopa, Ti-SBMA surface of preparation with untreated surface of metal titanium, and first being diluted by pinniform boat-shaped algae sterilizing seawater is 1 × 10
5the concentration of individual/ml, then test sample is placed in diatom suspension, take out after 3 hours, read 30 visuals field at random under the microscope, calculate the average attachment quantity of diatom, as shown in Figure 1, diatom is 30/mm at the adhesion amount of untreated surface of metal titanium to result
2, be 9.2/mm in Ti-Dopa surface attachment amount
2, Ti-SBMA surface attachment amount is 0.4/mm
2, after surface treatment, surface of metal titanium has excellent antifouling property.
Embodiment 2:
The detailed process of the present embodiment to the antifouling and antibiosis process on titanium or titanium alloy surface is:
(1) titanium or titanium alloy surface are used successively acetone and deionized water ultrasonic cleaning, drying, carry out plasma-activated obtaining and activate titanium metal;
(2) activation titanium metal is placed in above aminopropyl trimethoxysilane-hexanaphthene mixing solutions, in moisture eliminator, vacuumizes vapour deposition 2 hours, obtain Ti-Apts; In wherein aminopropyl trimethoxysilane-hexanaphthene mixing solutions, aminopropyl trimethoxysilane and hexanaphthene volume ratio are 1:1;
(3), by Dopamine HCL be dissolved in three (methylol) aminomethane hydrochloride-hydrochloric acid soln, lucifuge stirs 24 hours, then Ti-Apts is placed in this solution, stirs 48 hours, takes out flushing and dries up, obtain Ti-Dopa; Wherein the concentration of three (methylol) aminomethane hydrochloride-hydrochloric acid soln is 1mM, and pH value is 7, and the concentration of Dopamine HCL is 5g/L;
(4) Ti-Dopa is placed in flask, add 30 parts of toluene, 1 part of triethylamine, logical nitrogen in ice-water bath also drips 0.9 part of bromo isobutyl acylbromide, room temperature reaction 3 hours, reacted Ti-Dopa is taken out flushing to dry up and be placed in another flask, add the sulphonic acid betaine of 0.21 part of 2 ' 2 dipyridyl, 5 parts of water, 10 parts of methyl alcohol and 1 part of methacryloxy modification successively, logical nitrogen, add 0.08 part of cuprous bromide to be again polymerized, obtain Ti-SBMA;
(5), by Ti-SBMA put into the silver nitrate aqueous solution of 5g/L, lucifuge stirring reaction 1 hour, taking-up deionized water rinsing, obtains Ti-SBMA-Ag.
Embodiment 3:
The detailed process of the present embodiment to the antifouling and antibiosis process on titanium or titanium alloy surface is:
(1), titanium or titanium alloy surface are carried out plasma-activated obtaining with acetone and deionized water ultrasonic cleaning, drying successively and activate titanium metal;
(2) activation titanium metal is placed in above aminopropyl trimethoxysilane-hexanaphthene mixing solutions, in moisture eliminator, vacuumizes vapour deposition 48 hours, obtain Ti-Apts; In wherein aminopropyl trimethoxysilane-hexanaphthene mixing solutions, aminopropyl trimethoxysilane and hexanaphthene volume ratio are 1:10;
(3) Dopamine HCL is dissolved in three (methylol) aminomethane hydrochloride-hydrochloric acid soln, Ti-Apts is placed in this solution, stir 1 hour, take out flushing and dry up, obtain Ti-Dopa; Wherein the concentration of three (methylol) aminomethane hydrochloride-hydrochloric acid soln is 20mM, and pH value is 9, and the concentration of Dopamine HCL is 10g/L;
(4) Ti-Dopa is placed in flask, in ice-water bath, lead to nitrogen after adding 30 parts of toluene and 1 part of triethylamine and drip 0.9 part of bromo isobutyl acylbromide, room temperature reaction 24 hours, reacted Ti-Dopa taking-up flushing being dried up is placed in another flask, add the sulphonic acid betaine of 0.21 part of 2 ' 2 dipyridyl, 5 parts of water, 10 parts of methyl alcohol and 10 parts of methacryloxy modifications successively, logical nitrogen, then add 0.08 part of cuprous bromide and be polymerized, obtain Ti-SBMA;
(5) Ti-SBMA is put into the silver nitrate aqueous solution of 5g/L, lucifuge stirring reaction 48 hours, taking-up deionized water rinsing, obtains Ti-SBMA-Ag.
The present embodiment gets cultured bacterium 50 microlitre in Bechtop, drip the solid culture primary surface in cooling, with spreading rod by even for the coating of bacterium liquid, then be placed with Ti-SBMA-Ag sample prepared by the gripping of sterilizing tweezers and entreat in the medium, be positioned in shaking culture case and cultivate 24h, culture condition is 37 degrees Celsius, 100rpm, observe antibacterial circle diameter size, the larger explanation fungistatic effect of diameter is better, experimental result shows, Ti-SBMA-Ag has significant restraining effect to intestinal bacteria (Fig. 2), blue or green vibrios far away (Fig. 3).
Claims (3)
1. the antifouling and antibiosis treatment process on titanium or titanium alloy surface, is characterized in that specifically comprising the following steps:
(1), by titanium or titanium alloy surface use acetone and deionized water ultrasonic cleaning, drying successively, then carry out plasma-activated obtaining and activate titanium metal;
(2), by activation titanium metal be positioned over above silane coupling agent-hexanaphthene mixing solutions, in moisture eliminator, vacuumize vapour deposition 2 ~ 48 hours, obtain the titanium metal that finishing has silane coupling agent; Wherein the volume ratio of silane coupling agent and hexanaphthene is 1:1 ~ 10;
(3), Dopamine HCL is dissolved in three (methylol) aminomethane hydrochloride-hydrochloric acid soln, lucifuge stirs and obtains mixing solutions in 0 ~ 24 hour, finishing had the titanium metal of silane coupling agent to be placed in mixing solutions again to stir 1 ~ 48 hour, taking-up flushing dries up, obtain the titanium metal that finishing has Dopamine HCL, wherein the concentration of three (methylol) aminomethane hydrochloride-hydrochloric acid soln is 1 ~ 20mM, and pH value is 7 ~ 9, and the concentration of Dopamine HCL is 0.5 ~ 10g/L;
(4), the titanium metal of Dopamine HCL finishing is had to be placed in flask, add the triethylamine of the toluene of 30 weight parts, 1 weight part, logical nitrogen in ice-water bath also drips the bromo isobutyl acylbromide of 0.9 weight part, and room temperature reaction takes out flushing after 3 ~ 24 hours and dries up; Then another flask is placed in, logical nitrogen is continued after adding the methacryloxy modified betaine of 2 ' 2 dipyridyls of 0.21 weight part, the water of 5 weight parts, the methyl alcohol of 10 weight parts and 1 ~ 10 weight part successively, the cuprous bromide adding 0.08 weight part is again polymerized, and obtains the titanium metal that finishing has trimethyl-glycine molecule;
(5), the titanium metal of trimethyl-glycine molecule finishing is had to put into the silver nitrate aqueous solution of 5g/L, lucifuge stirring reaction 1 ~ 48 hour, taking-up deionized water rinsing is clean, prepare the titanium metal that finishing has trimethyl-glycine molecule and silver, realize the antifouling and antibiosis process of surface of metal titanium.
2. the antifouling and antibiosis treatment process on titanium or titanium alloy surface according to claim 1, is characterized in that described silane coupling agent comprises aminopropyl triethoxysilane and aminopropyl trimethoxysilane.
3. the antifouling and antibiosis treatment process on titanium or titanium alloy surface according to claim 1, is characterized in that described methacryloxy modified betaine comprises the sulphonic acid betaine of methacryloxy modification and the carboxylic acid trimethyl-glycine of methacryloxy modification.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105127666A (en) * | 2015-09-21 | 2015-12-09 | 上海交通大学 | Method for ultrafine modification of surface of TC4 titanium alloy |
| CN105218847A (en) * | 2015-09-14 | 2016-01-06 | 北京化工大学 | A kind of bill of material interface function method of modifying based on polyphenolic compound |
| CN105622870A (en) * | 2016-03-11 | 2016-06-01 | 中国船舶重工集团公司第七二五研究所 | Preparation method for sulfate reducing bacterium corrosion inhibiting film |
| CN112661929A (en) * | 2021-01-18 | 2021-04-16 | 丽水学院 | Polyurethane functionalized by click chemistry and preparation method thereof |
| CN113755828A (en) * | 2021-09-02 | 2021-12-07 | 福建医科大学附属口腔医院 | Method for antibacterial modification and improvement of bioactivity of titanium surface, coating and implant |
| US11407921B2 (en) | 2016-12-22 | 2022-08-09 | Henkel Ag & Co. Kgaa | Reaction products of catechol compounds and functionalized co-reactant compounds for metal pretreatment applications |
| CN115068679A (en) * | 2022-06-30 | 2022-09-20 | 浙江大学滨江研究院 | Anti-tissue adhesion titanium surface modification method for oral implantation, product and application thereof |
| US11891534B2 (en) | 2016-12-22 | 2024-02-06 | Henkel Ag & Co. Kgaa | Treatment of conversion-coated metal substrates with preformed reaction products of catechol compounds and functionalized co-reactant compounds |
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| CN105218847A (en) * | 2015-09-14 | 2016-01-06 | 北京化工大学 | A kind of bill of material interface function method of modifying based on polyphenolic compound |
| CN105218847B (en) * | 2015-09-14 | 2018-06-26 | 北京化工大学 | A kind of material surface and interface functional modification method based on polyphenol compound |
| CN105127666A (en) * | 2015-09-21 | 2015-12-09 | 上海交通大学 | Method for ultrafine modification of surface of TC4 titanium alloy |
| CN105622870A (en) * | 2016-03-11 | 2016-06-01 | 中国船舶重工集团公司第七二五研究所 | Preparation method for sulfate reducing bacterium corrosion inhibiting film |
| CN105622870B (en) * | 2016-03-11 | 2018-01-23 | 中国船舶重工集团公司第七二五研究所 | A kind of sulfate reducing bacteria corrosion suppresses the preparation method of film |
| US11891534B2 (en) | 2016-12-22 | 2024-02-06 | Henkel Ag & Co. Kgaa | Treatment of conversion-coated metal substrates with preformed reaction products of catechol compounds and functionalized co-reactant compounds |
| US11407921B2 (en) | 2016-12-22 | 2022-08-09 | Henkel Ag & Co. Kgaa | Reaction products of catechol compounds and functionalized co-reactant compounds for metal pretreatment applications |
| CN112661929A (en) * | 2021-01-18 | 2021-04-16 | 丽水学院 | Polyurethane functionalized by click chemistry and preparation method thereof |
| CN112661929B (en) * | 2021-01-18 | 2022-07-12 | 丽水学院 | Polyurethane functionalized by click chemistry and preparation method thereof |
| CN113755828A (en) * | 2021-09-02 | 2021-12-07 | 福建医科大学附属口腔医院 | Method for antibacterial modification and improvement of bioactivity of titanium surface, coating and implant |
| CN113755828B (en) * | 2021-09-02 | 2023-10-24 | 福建医科大学附属口腔医院 | Method for antibacterial modification of titanium surface and improvement of biological activity of titanium surface, coating and implant |
| CN115068679B (en) * | 2022-06-30 | 2023-06-06 | 浙江大学滨江研究院 | Titanium surface modification method for oral implantation for resisting tissue adhesion, product and application thereof |
| CN115068679A (en) * | 2022-06-30 | 2022-09-20 | 浙江大学滨江研究院 | Anti-tissue adhesion titanium surface modification method for oral implantation, product and application thereof |
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