CN105386113A - Preparing method of titanium-based material surface composite antibacterial coating - Google Patents
Preparing method of titanium-based material surface composite antibacterial coating Download PDFInfo
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Abstract
A preparing method of a titanium-based material surface composite antibacterial coating mainly comprises the steps that the titanium-based material surface pretreatment is carried out, the surface of a titanium-based material is smooth and bright, an oxide surface layer is removed, the electrochemical oxidation is carried out on the titanium-based material surface and soluble fluoride, titania nanotube arrays (TNTs) are formed on the titanium-based material surface, nano-silver is loaded in a titania nanotube array structure through the chemical reduction method, finally, the upper faces of titania nanotubes are loaded with a polylactic acid-poly lactic-co-glycolic acid (PLGA) coating containing biological membrane depolymerization micromolecule substance bi (3-amidogen propyl group) amine, and a TNTs-Ag-PLGA/bi(3- amidogen propyl group) amine three-dimensional composite antibacterial coating is formed. According to the antibacterial coating, the slow release time of nano-silver is obviously prolonged, the effectiveness of nano-silver is improved, and the more efficient and durable antibacterial effect is achieved.
Description
Technical field
The present invention originally relates to one and prepares compound fungistatic coating method at material surface, particularly relates to one and prepares titanium nanotube on titanium base material surface and loading nano silvery and the compound fungistatic coating method containing two (3-aminopropyl) amine polymer of microorganism depolymerization small molecules.Belong to Antimicrobial and microbial film control techniques field.
Background technology
Microbial film refers to that bacterioplankton is attached to biology or inanimate surfaces, and is combined by the extracellular polymeric (EPS) of himself secretion, the structural microflora of formation.Microbial film is extensively present in environment, as the human tissue organ under sterilisation system, water supply pipe, industrial pipeline, ventilation installation, medicine equipment and pathological state.The formation of harmful organism film can cause a lot of problem.At medical field, some pathogenic bacterium are inside and outside human body and to form microbial film be cause chronic infectious diseases recurrent exerbation and unmanageable one of the main reasons on medical material surface, and human body bacteriological infection 80% is all relevant with microbial film.At environmental area, biomembranous existence can cause the problem such as food and water pollution, mould material pollution, line clogging and corrosion.
Sterilant or antiseptic-germicide were adopted more, as clorox and microbiotic etc. for biomembranous control in the past.As antiseptic-germicide gentamicin has been assembled in the electrolytic polymer coating of degradable poly-amino ester, Hyaluronic Acid or polyacrylic acid formation by (2010) such as Schmidt.Antiseptic-germicide (Silver Nitrate or Cetrimide) has loaded in the ionogen coating of polyacrylic acid and polymine formation by Chuang etc. (2008).Because extracellular polymeric changes to Bacterial phenotype after the barrier protection effect of bacterium and formation microbial film thereof, life-time service microbiotic or sterilant may cause resistance to increase, and drug-resistant bacteria spreads, thus bring new environmental risk.
Nano-metal particle is the promising fungistat of one of development in recent years, wherein general with the application of nanometer silver.When nano-silver loaded is to material surface, the effect suppressing material surface biofilm formation can be reached by the slowly-releasing of silver ions.As nano-Ag particles to be fixed on the surface of production unit by number of patent application 200710016018.0 by the mode of chemical bonding, to establish the nanometer antibacterium coating with slow release characteristic, achieve control biomembranous in beer equipment.But, because the nanometer silver rate of release loading to material surface is relatively very fast, be often difficult to obtain permanent fungistatic effect.In order to improve the lasting effectiveness of nano silver antibacterial coating, this patent is for titanium base material, propose by preparing titanium nanotube and loading nano silvery on titanium base material surface, and then cover upper Poly(D,L-lactide-co-glycolide (PLGA) coating containing two (3-aminopropyl) amine, thus set up a kind of special three-dimensional structure fungistatic coating.Two (3-aminopropyl) amine is a kind of polyamines micromolecular material with ad hoc structure, amino in its structure can with the negative valency state in bacterial polysaccharides or band polar group neutral sugar generation chemical reaction, also may have an effect with extracellular dna, thus impel biofilm breakup.Poly(D,L-lactide-co-glycolide (PLGA) is a kind of polymkeric substance that can be degraded by microorganisms.The titanium base material surface three dimension compound fungistatic coating built in this way there is not yet report.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned deficiency of the prior art, provides a kind of titanium base material surface fungistatic coating preparation method.The method prepares array structure titania nanotube (Titaniananotubes by titanium base material surface preparation and electrochemical oxidation, TNTs), and by chemical reduction, nanometer silver is loaded in TNTs structure, Poly(D,L-lactide-co-glycolide (the poly (lactic-co-glycolicacid) of two (3-aminopropyl) amine of microorganism depolymerization small-molecule substance is finally contained at TNTs surface coverage one deck, PLGA) coating, achieve nanometer silver at titanium base material steady load and long-term sustained release, significantly improve its bacteriostasis property.
A kind of titanium base material surface recombination fungistatic coating preparation method, its concrete steps comprise:
(1) titanium base material surface preparation: by the polishing of titanium base material sand for surface paper to light and without obvious cut, and then the oxide compound on top layer is removed by Chemical Pretreatment, its concrete steps comprise: the titanium base material after polished finish be impregnated in ultrasonic 15-30min in 10-40%NaOH solution, then ultrapure water cleaning down titanium base material is used, dry up, then titanium base material is placed in 5-10% oxalic acid solution and boils 1-2h, take out titanium base material ultrapure water and clean, for subsequent use.
(2) titanium nano-tube array (TNTs) is prepared on titanium base material surface: titanium material sample good for pre-treatment is placed in electrochemical anodic oxidation device, take titanium sheet as anode, graphite or platinized platinum are negative electrode, with NaF, KF or NH containing the 0.5-2%HF aqueous solution or 0.5-5%
4f is anolyte; Oxidation voltage is respectively 20-60V, oxidization time 20-60min; Sample anodic oxidation obtained is placed in retort furnace and makes TNTs at 400-500 DEG C of thermal treatment 2-3h.
(3) TNTs is loaded into nanometer silver (TNTs/Ag): the titanium material sample processed through step (2) is placed in 10-50g/LAgNO
3in solution, magnetic agitation 10-30min, makes silver ions be well-dispersed in titanium nanotube surface; Drip equimolar NaBH
4solution, and by solution NH
4oH is adjusted to pH=10, magnetic agitation 20-60min, nanometer silver can load in titanium nano tube structure, and by load, the titanium material sample ultrapure water of nanometer silver cleans, dry.
(4) load is containing the PLGA coating of two (3-aminopropyl) amine: the titanium material sample (TNTs-Ag) of the load that above-mentioned steps (3) is obtained nanometer silver impregnated in the PLGA solution (1-2% (w/v) is in methylene dichloride) containing two (3-aminopropyl) amine of 0.5-1.5mg/mL, 5-15 takes out after second, 50-70 DEG C of dry 10-20min, and then impregnated in the above-mentioned PLGA solution containing two (3-aminopropyl) amine, repetition like this 1-10 time, just complete two (3-aminopropyl) the amine compound fungistatic coating of titanium material sample surface preparation TNTs-Ag-PLGA/.
Useful benefit
The titanium base material that the present invention proposes prepares the method for two (3-aminopropyl) the amine compound fungistatic coating of TNTs-Ag-PLGA/, simple, reproducible, economical and efficient.The nanometer silver that coating adopts is a kind of wide-spectrum bactericide, effectively can suppress various bacteria.(3-aminopropyl) amine is a kind of small-molecule substance that can promote microorganism depolymerization, can the polysaccharide of useful effect in microbial film, promotes that biological aggressiveness dissociates.The combined utilization of (3-aminopropyl) amine and nanometer silver improves the validity of nanometer silver.The PLGA coating of TNT surface coverage, it is a kind of biodegradable coating, it covers the titanium nanotube mouth of pipe, but when having a certain amount of microbe deposition on its surface and being degraded, sealing is opened, nanometer silver slowly-releasing out, thus constructs a kind of based on the three-dimensional compound fungistatic coating under microorganism stimuli responsive pattern.This fungistatic coating can reach the bacteriostasis rate of 40-70% in 30 days.
Accompanying drawing explanation
Titanium nano-tube array (TNTs) form of Fig. 1 titanium base material surface preparation
The three-dimensional compound coating configuration of surface of two (3-aminopropyl) amine of TNTs-Ag-PLGA/ of Fig. 2 titanium base material surface preparation
Fig. 3 be different titanium sheet stratum basale slowly-releasing after 16 days to biofilm formation inhibition
Embodiment
Embodiment 1
(1) titanium plate surface pre-treatment: by titanium plate surface sand papering to light and without obvious cut, titanium sheet material after polished finish is dipped in 30%NaOH solution, ultrasonic 30min, then ultrapure water titanium sheet is used, after rinsing well, dry up, then titanium sheet is positioned in 10% oxalic acid solution and boils 1h, take out titanium sheet ultrapure water and clean.
(2) titanium plate surface prepares TNTs: titanium sheet good for step (1) pre-treatment is placed in electrochemical anodic oxidation device, take titanium sheet as anode, graphite is negative electrode, electrolytic solution is the aqueous solution containing 1%HF, distance between anodic-cathodic is respectively 6cm, under constant potential 40V, be oxidized 20min, then take out titanium sheet and be placed in retort furnace, make the TNTs of Detitanium-ore-type at 500 DEG C of thermal treatment 1h.
(3) TNTs is loaded into nanometer silver (TNTs-Ag): the titanium sheet processed through step (2) is placed in 10g/LAgNO
3in solution, magnetic agitation 30min, makes silver ions be well-dispersed in nanotube surface; Drip equimolar NaBH
4solution, by solution NH
4oH is adjusted to pH=10, magnetic agitation 30min, is cleaned by sample ultrapure water, dry, obtains TNTs-Ag.
(4) load is containing the PLGA coating of two (3-aminopropyl) amine: PLGA is dissolved in methylene dichloride, preparation 1%PLGA dichloromethane solution, take a certain amount of two (3-aminopropyl) amine, joined in 1%PLGA dichloromethane solution, join to obtain the PLGA solution (1% (w/v) is in methylene dichloride) containing two (3-aminopropyl) amine of 1.0mg/mL, the titanium sheet processed through step (3) is immersed in the PLGA solution containing two (3-aminopropyl) amine, 10 seconds afterwards take out and at 70 DEG C of dry 20min, repetition like this 5 times, just complete titanium plate surface and prepare two (3-aminopropyl) the amine fungistatic coating of TNTs-Ag-PLGA/.
(5) coating characterization and inhibitory effect: the titanium nano tube structure that titanium sample obtains after electrochemical oxidation characterizes as shown in Figure 1 by scanning electron microscope, and titanium nano tube structure is in good order.On its area load nanometer silver and two (3-aminopropyl) amine PLGA coating after, scanning electron microscope (SEM) photograph is as indicated with 2.Define two (3-aminopropyl) film of the very thin PLGA/ of one deck on TNTs surface as can clearly be seen from Figure, this layer film completely by TNTs surface coverage, the shutoff nanotube mouth of pipe.This had the titanium sample of fungistatic coating and be placed in the mixed bacterial prepared by active sludge without the control sample of fungistatic coating, 24h is cultivated at temperature is 30 DEG C, find that, compared with contrast titanium sheet, the titanium sheet of load fungistatic coating to maintain the antibacterial efficiency of 41-55% in 16 days.Fig. 3 is that two (3-aminopropyl) amine fungistatic coating of TNTs-Ag-PLGA/ of preparation compares at the 16th day fungistatic effect with other fungistatic coatings.
Embodiment 2
(1) titanium plate surface pre-treatment: get the sand papering of pure titanium sample surfaces to light and without obvious cut, titanium sheet material after polished finish is dipped in 40%NaOH solution, ultrasonic 20min, then ultrapure water titanium sheet is used, after rinsing well, dry up, then titanium sheet is positioned in 10% oxalic acid solution and boils 1h, take out titanium sheet ultrapure water and clean.
(2) titanium base material surface preparation TNTs: the titanium sheet that pre-treatment is good is placed in electrochemical anodic oxidation device, take titanium sheet as anode, and graphite is negative electrode, and electrolytic solution is containing 2%NaF, 85% ethylene glycol and 13% water; Distance between anodic-cathodic is respectively 10cm, under constant potential 40V, be oxidized 20min, then takes out titanium sheet and is placed in retort furnace, make the TNTs of Detitanium-ore-type at 500 DEG C of thermal treatment 2h.
(3) TNTs is loaded into nanometer silver (TNTs-Ag): the titanium sheet processed through step (2) is placed in 10g/LAgNO
3in solution, magnetic agitation 30min, makes silver ions be well-dispersed in nanotube surface; Drip equimolar NaBH
4solution, by solution NH
4oH is adjusted to pH=10, magnetic agitation 30min, is cleaned by sample ultrapure water, dry, obtains TNTs-Ag.
(4) load is containing the PLGA coating of two (3-aminopropyl) amine: PLGA is dissolved in methylene dichloride, preparation 1%PLGA dichloromethane solution, take a certain amount of two (3-aminopropyl) amine, joined in 1%PLGA dichloromethane solution, join contain in the PLGA solution (1% (w/v) is in methylene dichloride) of two (3-aminopropyl) amine of 0.5mg/mL, the titanium sheet processed through step (3) is immersed in the PLGA solution containing two (3-aminopropyl) amine, 5 seconds afterwards take out and at 70 DEG C of dry 20min, repetition like this 5 times, just complete titanium plate surface and prepare two (3-aminopropyl) the amine fungistatic coating of TNTs-Ag-PLGA/.
Embodiment 3
The step 1 of the present embodiment, 3,4 identical with embodiment 2, difference is that the present embodiment step 2 adopts NH when titanium base material surface preparation TNTs
4f is oxygenant, and concrete steps comprise: the titanium sheet that pre-treatment is good is placed in electrochemical anodic oxidation device, take titanium sheet as anode, and graphite is negative electrode, and electrolytic solution is containing 5%NH
4f, 85% ethylene glycol and 10% water; Distance between anodic-cathodic is respectively 6cm, under constant potential 40V, be oxidized 20min; Then taking out titanium sheet is placed in retort furnace, makes the TNTs of Detitanium-ore-type at 500 DEG C of thermal treatment 2h.
Embodiment 4
The step 1 of the present embodiment, 3,4 identical with embodiment 2, difference is that the step 2 of the present embodiment adopts KF to be oxygenant when titanium base material surface preparation TNTs, concrete steps comprise: the titanium sheet that pre-treatment is good is placed in electrochemical anodic oxidation device, take titanium sheet as anode, graphite is negative electrode, and electrolytic solution is containing 5%KF, 85% ethylene glycol and 10% water; Distance between anodic-cathodic is respectively 6cm, under constant potential 40V, be oxidized 20min, then takes out titanium sheet and is placed in retort furnace, make the TNTs of Detitanium-ore-type at 500 DEG C of thermal treatment 2h.
Embodiment 5
The step 1 of the present embodiment, 2,4 identical with embodiment 2, be with the difference of embodiment 2, the present embodiment step 3 is that the concrete steps of TNTs loading nanometer silver (TNTs-Ag) comprising: the titanium sheet processed through step (2) is placed in 40g/LAgNO
3in solution, magnetic agitation 30min, makes silver ions be well-dispersed in nanotube surface; Drip equimolar NaBH
4solution, by solution NH
4oH is adjusted to pH=10, magnetic agitation 30min, is cleaned by sample ultrapure water, dry, obtains TNTs-Ag.
Embodiment 6
The step 1 of the present embodiment, 2, 3 is identical with embodiment 2, be with the difference of embodiment 2, the present embodiment step 4 is that PLGA coating that load contains two (3-aminopropyl) amine has and comprises: PLGA is dissolved in methylene dichloride, preparation 2%PLGA dichloromethane solution, take a certain amount of two (3-aminopropyl) amine, joined in 2%PLGA dichloromethane solution, join contain in the PLGA solution (2% (w/v) is in methylene dichloride) of two (3-aminopropyl) amine of 1.0mg/mL, the titanium sheet processed through step (3) is immersed in the PLGA solution containing two (3-aminopropyl) amine, 5 seconds afterwards take out and at 70 DEG C of dry 20min, repetition like this 2 times, just complete titanium plate surface and prepare two (3-aminopropyl) the amine fungistatic coating of TNTs-Ag-PLGA/.
Embodiment 7
The step 1 of the present embodiment, 2, 3 is identical with embodiment 2, be with the difference of embodiment 2, the present embodiment step 4 is that PLGA coating that load contains two (3-aminopropyl) amine has and comprises: PLGA is dissolved in methylene dichloride, preparation 1%PLGA dichloromethane solution, take a certain amount of two (3-aminopropyl) amine, joined in 1%PLGA dichloromethane solution, join contain in the PLGA solution (1% (w/v) is in methylene dichloride) of two (3-aminopropyl) amine of 1.0mg/mL, the titanium sheet processed through step (3) is immersed in the PLGA solution containing two (3-aminopropyl) amine, 5 seconds afterwards take out and at 70 DEG C of dry 20min, repetition like this 6 times, just complete titanium plate surface and prepare two (3-aminopropyl) the amine fungistatic coating of TNTs-Ag-PLGA/.
Claims (3)
1. a titanium base material surface recombination fungistatic coating preparation method, is characterized in that comprising the following steps:
(1) titanium base material surface preparation: by the polishing of titanium material sample sand for surface paper to light and without obvious cut, and then the oxide compound on top layer is removed by Chemical Pretreatment, the concrete steps of Chemical Pretreatment comprise: the titanium material sample after polished finish be impregnated in ultrasonic 15-30min in 10-40%NaOH solution, then ultrapure water cleaning down titanium base material is used, dry up, then titanium titanium material sample be impregnated in 5-10% oxalic acid solution and boil 1-2h, take out titanium material sample ultrapure water to clean, for subsequent use;
(2) titanium nano-tube array (TNTs) is prepared on titanium base material surface: titanium material sample good for pre-treatment is placed in electrochemical anodic oxidation device, and with it for anode, with graphite or platinized platinum for negative electrode, with NaF, KF or NH containing the 0.5-2%HF aqueous solution or 0.5-5%
4f solution is anolyte; Oxidation voltage is 20-60V, and oxidization time is 20-60min; Titanium material sample anodic oxidation obtained is placed in retort furnace, and at 400-500 DEG C of thermal treatment 2-3h, titanium material sample surface forms titanium nano-tube array;
(3) TNTs is loaded into nanometer silver (TNTs-Ag): the titanium sheet processed through step (2) is placed in 10-50g/LAgNO
3in solution, magnetic agitation 10-30min, makes silver ions be well-dispersed in titanium nanotube surface; Drip equimolar NaBH
4solution, and by solution NH
4oH is adjusted to pH=10, magnetic agitation 20-60min, by nano-silver loaded in the titanium nanotube of titanium material sample surface array structure, is then cleaned by titanium material sample ultrapure water, dry;
(4) load is containing Poly(D,L-lactide-co-glycolide (PLGA) coating of two (3-aminopropyl) amine: the titanium material sample (TNTs-Ag) of the load that above-mentioned steps (3) is obtained nanometer silver impregnated in the PLGA solution (1-2% (w/v) is in methylene dichloride) containing two (3-aminopropyl) amine of 0.5-1.5mg/mL, 5-15 takes out titanium material sample at 50-70 DEG C of dry 10-30min after second, and then titanium material sample be impregnated in the above-mentioned PLGA solution containing two (3-aminopropyl) amine, repetition like this 1-10 time, just complete the three-dimensional compound fungistatic coating of two (3-aminopropyl) amine of titanium material sample surface preparation TNTs-Ag-PLGA/.
2. a kind of titanium base material surface recombination fungistatic coating preparation method according to claim 1, described titanium base material comprises pure titanium and its alloys.
3. a kind of titanium base material surface recombination fungistatic coating preparation method according to claim 1, the anode electrode liquid described in its step (2) is 0.5-5%NaF, KF or NH
4during F, need in electrolytic solution to add the ethylene glycol of 80-85% and the water of residue per-cent.
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| CN109267137A (en) * | 2018-10-12 | 2019-01-25 | 厦门大学 | A kind of preparation method of the surface graded nano silver of medical titanium |
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| CN115094496B (en) * | 2022-06-20 | 2024-01-26 | 西安理工大学 | Preparation method of titanium alloy surface bell type biological piezoelectric nanotube coating |
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