CN104072798B - A kind of preparation method of the nanometer particle-modified sponge dressing with antibacterial functions - Google Patents
A kind of preparation method of the nanometer particle-modified sponge dressing with antibacterial functions Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of the nanometer particle-modified sponge dressing with antibacterial functions, and step is as follows：(1) pre-processed for sponge raw material；(2) soak is prepared：Soak is soluble metal salt solution or/and nano-metal-oxide particle dispersion：Soluble metal salt solution is homogeneous aqueous solution of the composition for soluble metal salt or metal complex, described nano-metal-oxide dispersion liquid composition is the uniform suspension that nano-metal-oxide uniform particle is scattered in gained in solvent, (3) sponge substrate that processing is completed in step (1) is fully immersed in the soak of step (2) preparation, opens ultrasonic wave and be ultrasonically treated；(4) after ultrasound stops, sponge base-material is removed into soak, it is post-processed, you can obtains the sponge dressing with anti-microbial property.Sponge dressing with antibacterial functions prepared by the present invention, nano metal or metal oxide particle are incorporated into sponge substrate surface, sponge is shown anti-microbial property.
Description
Technical field
The present invention relates to the preparation method of medical antibacterial dressing, specifically a kind of nano-particle with antibacterial functions
The preparation method of modified sponge dressing.
Background technology
The correct processing of surgical wound is one of key of surgical intervention success or failure, and the good healing of the surface of a wound is machine after wound
The important prerequisite and mark of body function rehabilitation, and with the horizontal lifting of popular life, medical treatment people and doctor are for site of injury
The requirement of reason and the validity of agglutination, applicability, ease for operation or even comfortableness is also constantly lifted, therefore is cured on the surface of a wound
The research of conjunction is more and more widely paid close attention to, and the development wherein for Wound dressing also turns into the focus of research therewith.With
And wound healing research is goed deep into, researcher is gradually recognized in wound, and the use of dressing can not only be covered
The impaired skin of the lid surface of a wound, replacement and soft tissue play temporary barrier action so as to avoid or control wound infection, simultaneously
One micro- wet environment for being advantageous to wound healing can be also provided, largely promote the healing of wound tissue.But simultaneously
Researcher is it is also recognized that the shortcomings that use of traditional Wound dressing such as gauze etc. is difficult to avoid that in the presence of many：Easy breed bacteria；Wound
Face diffusate easily forms crust obstruction epithelialization with drying dermal tissue；New granulation tissue is easy to dressing adhesion, draws during replacing
Play pain and bring secondary insult；Frequently replacing and medication is needed to keep effect etc..Due to these deficiencies be present, market is needed badly
New Wound dressing is to meet the requirement of patient and doctor., can in the various new pattern compress developed at present
The sponge kind dressing for coordinating negative-pressure sealed drainage technology to use is widely used and approved because of its excellent performance.By height
The various sponge kind dressing that molecular material is processed into have good toughness and elasticity, and processing characteristics is good, while its biofacies
Capacitive is excellent, and no sensitization and toxic side effect, particularly layered porous structure are advantageous to the discharge of wound secretion and diffusate,
And ensure the moistening of the surface of a wound so as to promoting the healing of wound tissue simultaneously.Simultaneously its it is stable and can the reason that adjust according to demand
Change structure, the introducing of all kinds of modified functions can be applied to as base material.
Its particle scale of nano material is in cluster and macro object handover region, and there occurs very compared with conventional powder
Big change, have a series of traditional materials not available for novel and special Wuli-Shili-Renli system approach, Catalyst,
Physics especially medical science and bioengineering etc. have a wide range of applications.The use of various other materials is template, Xiang Qi
Middle introducing nano material, so that material embodies the design performance of novelty, it is that the one kind being widely adopted at present prepares function
The method of material.
The metal or metal oxide particle of nanoscale, it is applied to various research fields and shows each solely
Special performance.Wherein it is widely studied and approves, is exactly the anti-microbial property of a variety of nano metals or metal oxide particle.When
These nano-particles are doped to material internal by various physics and chemistry processing modes or are incorporated into material surface, can not changed
On the basis of base material performance itself, obvious anti-microbial property advantageously extremely is introduced for material, so as to obtain new antibacterial work(
Can property material.
But method such as hydro-thermal method of nanometer particle-modified functional material etc. used at present, its preparation method is to producing bar
The requirement of part is extremely strict, and complex technical process is difficult to control, therefore the preparation of high-volume unified standard material difficult to realize, no
The needs of practical application can be met.
The content of the invention
It is an object of the invention to provide a kind of requirement of working condition is simple, raw material sources are extensive, and cost is low and technique
The preparation method of the simple nanometer particle-modified sponge dressing with antibacterial functions, the present invention is by sonochemical method in sponge
The surface in situ generation of dressing or directly in conjunction with the upper metal or metal oxide nanoparticles with antibacterial ability, so as to
Realize for the antibacterial modified of sponge dressing.
Technical scheme provided by the invention is：A kind of preparation side of the nanometer particle-modified sponge dressing with antibacterial functions
Method, step are as follows：
(1) pre-processed for sponge raw material：Pretreatment include curing, cleaning, dry, wind leaching processing, cut,
Co60 x ray irradiation xs；
(2) soak is prepared：Soak is soluble metal salt solution or/and nano-metal-oxide particle dispersion：
Soluble metal salt solution is that composition is molten for the metal salt of solubility or the homogeneous aqueous solution of metal complex, including silver nitrate
Liquid, silver ammino solution, copper ammon solution, copper chloride solution, copper nitrate solution, copper-bath, solution of zinc sulfate, liquor zinci chloridi,
Zinc nitrate solution, nitric acid cadmium solution, iron nitrate solution, acetic acid copper solution, zinc acetate solution, magnesium chloride solution, magnesium nitrate solution,
And the uniform salting liquid or complex solution of other known associated metals；Described nano-metal-oxide dispersion liquid composition
The uniform suspension of gained in solvent is scattered in for nano-metal-oxide uniform particle, nano-metal-oxide particle includes oxygen
Change one or both of zinc, cupric oxide, magnesia, Nano Silver, titanium dioxide, vanadic anhydride and two or more mixing；
(3) sponge substrate that processing is completed in step (1) is fully immersed in the soak of step (2) preparation, opened
Ultrasonic wave is ultrasonically treated；
(4) after ultrasound stops, sponge base-material is removed into soak, it is post-processed, you can acquisition has antibiotic property
The sponge dressing of energy.
The concentration of soluble metal salt solution described in described step (2) is 0.01mol/L-10mol/L, nanogold
The concentration for belonging to oxidate dispersion solution is 0.01g/L-100g/L.
Preferably, the concentration of the soluble metal salt solution described in step (2) is 0.02mol/L-1mol/L, nanogold
The concentration for belonging to oxidate dispersion solution is 0.5g/L-10g/L.
Preferably, the soak selection heterogeneity described in described step (2) is combined use, including copper nitrate,
The mixing point of the mixed solution of silver nitrate, the mixed solution of copper acetate and zinc acetate, Nano Silver or silver nitrate and nano-titanium oxide
The mixed dispersion liquid of dispersion liquid, nano cupric oxide and nano zine oxide.
Preferably, described sponge material from hydrophily and all more excellent Pioloform, polyvinyl acetal sponge of permeability or
The multilayer that including negative pressure conducting shell be hydrophobic porous sponge layer and drainage protective layer is hydrophilic porous sponge layer
Sponge material.
Ultrasonic intensity used in described step (3) is 50-5000W/cm-2, frequency 10-40kHz, ultrasound work
It is 5-300min with the time.
Preferably, the ultrasonic intensity used in step (3) is 750-4000W/cm-2, frequency 20-27kHz, effect
Time is 5-30min ul-trasonic irradiation pattern.
Sponge post processing used in described step (4) includes rinse cleaning repeatedly, heat blowing drying, low temperature cold
Jelly, Co60 x ray irradiation xs, vacuum sealed package.
Advantages of the present invention：The sponge dressing with antibacterial functions prepared according to this mode, is determined by ESEM
The microstructure composition of product, the anti-microbial property of product is determined by inhibition zone method.Measurement result shows, nano metal or metal
Oxide particle is incorporated into sponge substrate surface, and realizes the modification to sponge, sponge is shown anti-microbial property.
Brief description of the drawings
Fig. 1 be by SEM obtain sponge substrate surface effectively combine upper generated in-situ silver oxide/
Cupric oxide composite nanoparticle experimental result picture.
Fig. 2 is to show obvious anti-microbial property picture using modified sponge dressing.
Embodiment
The preparation method of the nanometer particle-modified sponge dressing with antibacterial functions of the present invention, step are as follows：
(1) pre-processed for sponge raw material, the sponge base-material for meeting design specification is made：Pretreatment includes ripe
Change, clean, drying, wind leaching is handled, is cut, Co60 x ray irradiation xs；
(2) soak is prepared：Soak is soluble metal salt solution or/and nano-metal-oxide particle dispersion：
Soluble metal salt solution is that composition is molten for the metal salt of solubility or the homogeneous aqueous solution of metal complex, including silver nitrate
Liquid, silver ammino solution, copper ammon solution, copper chloride solution, copper nitrate solution, copper-bath, solution of zinc sulfate, liquor zinci chloridi,
Zinc nitrate solution, nitric acid cadmium solution, iron nitrate solution, acetic acid copper solution, zinc acetate solution, magnesium chloride solution, magnesium nitrate solution,
And the uniform salting liquid or complex solution of other known associated metals；Described nano-metal-oxide dispersion liquid composition
The uniform suspension of gained in solvent is scattered in for nano-metal-oxide uniform particle, nano-metal-oxide particle includes oxygen
Change one or both of zinc, cupric oxide, magnesia, Nano Silver, titanium dioxide, vanadic anhydride and two or more mixing；
(3) sponge substrate that processing is completed in step (1) is fully immersed in the soak of step (2) preparation, opened
Ultrasonic wave is ultrasonically treated；
(4) after ultrasound stops, sponge base-material is removed into soak, it is post-processed, you can acquisition has antibiotic property
The sponge dressing of energy.
The concentration of soluble metal salt solution described in described step (2) is 0.01mol/L-10mol/L, nanogold
The concentration for belonging to oxidate dispersion solution is 0.01g/L-100g/L.
Preferably, the concentration of the soluble metal salt solution described in step (2) is 0.02mol/L-1mol/L, nanogold
The concentration for belonging to oxidate dispersion solution is 0.5g/L-10g/L.
The preferred different metal composition of soak described in step (2) is combined use, and preferable formula combination includes nitre
The mixed solution of sour copper and silver nitrate, mixed solution, Nano Silver or the silver nitrate of copper acetate and zinc acetate and nano-titanium oxide
Mixed dispersion liquid of mixed dispersion liquid, nano cupric oxide and nano zine oxide etc., these combination matchings can effectively play collaboration
Effect, more significantly strengthen anti-microbial property.
Sponge material used is Pioloform, polyvinyl acetal sponge, polyurethane sponge, polyethers sponge, chitosan sponge, marine alga
Hydrochlorate sponge, gelfoam, Silica hydrogel sponge etc., and other known various medical sponge materials.The present invention can both make
With one kind of above sponge material, two kinds and two or more can also be used in mixed way.
Preferably, described sponge material from hydrophily and all more excellent Pioloform, polyvinyl acetal sponge of permeability or
The multilayer that including negative pressure conducting shell be hydrophobic porous sponge layer and drainage protective layer is hydrophilic porous sponge layer
Sponge material.Its reason is good hydrophily and transparent performance more effectively improves active area with solution in step (2)
And action effect.
Ultrasonic intensity used in described step (3) is 50-5000W/cm-2, frequency 10-40kHz, ultrasound work
It is 5-300min with the time.
Preferably, the ultrasonic intensity used in step (3) is 750-4000W/cm-2, frequency 20-27kHz, effect
Time is 5-30min ul-trasonic irradiation pattern.The particle diameter of nano-particle and scattered feelings can be preferably controlled under this condition
Condition, and effectively avoid drawback caused by thermal effect of ultrasound.
Sponge post processing used in described step (4) includes rinse cleaning repeatedly, heat blowing drying, low temperature cold
Jelly, Co60 x ray irradiation xs, vacuum sealed package.
Embodiment 1：
The polyurethane sponge of selection is cut, cleaned, wind leaching processing；Configure AgNO3Concentration is 0.2mol/L, Cu
(NO3)2Concentration is 0.2mol/L mixed solution；Polyurethane sponge is fully immersed in mixed solution, system is carried out
30min is ultrasonically treated (20kHz, 750W/cm2), then polyurethane sponge is taken out, carries out cleaning treatment.To the product of gained
It is scanned electron microscopic observation and Bactericidal test.Test result indicates that effectively combined on sponge substrate surface upper generated in-situ
Silver oxide/cupric oxide composite nanoparticle (as shown in Figure 1), and sponge dressing modification is shown obvious antibiotic property
Energy (as shown in Figure 2), its antibacterial circle diameter have reached 4.0cm.
Embodiment 2：
The Pioloform, polyvinyl acetal sponge of selection is cut, cleaning treatment；Configure Zn (NO3)2Concentration be 0.5mol/L,
Cu(NO3)2Concentration is 0.05mol/L mixed solution；Pioloform, polyvinyl acetal sponge is fully immersed in mixed solution, to body
System carries out 60min supersound process (27kHz, 750W/cm2), then Pioloform, polyvinyl acetal sponge is taken out, carries out cleaning treatment.
Electron microscopic observation and Bactericidal test are scanned to the product of gained.Test result indicates that effectively combined on sponge substrate surface
Upper generated in-situ cupric oxide/zinc oxide compound nano particle, and sponge dressing modification is shown obvious antibacterial
Performance, its antibacterial circle diameter have reached 3.2cm.
Embodiment 3：
The Pioloform, polyvinyl acetal sponge of selection is cut, cleaning treatment；Configure AgNO3Concentration be 0.2mol/L,
MgCl2Concentration is 4mol/L mixed solution；Pioloform, polyvinyl acetal sponge is fully immersed in mixed solution, system is carried out
120min is ultrasonically treated (27kHz, 100W/cm2), then Pioloform, polyvinyl acetal sponge is taken out, carries out cleaning treatment.To gained
Product be scanned electron microscopic observation and Bactericidal test.Test result indicates that effectively combine upper original position on sponge substrate surface
The silver oxide of generation/magnesia composite nanoparticle, and sponge dressing modification is shown obvious anti-microbial property,
Its antibacterial circle diameter has reached 2.3cm.
Embodiment 4：
The chitosan gelatin sponge of selection is cut, cleaning treatment；Configure TiO2Concentration is 4g/L, AgNO3Concentration is
0.4mol/L mixing suspension；Polyurethane sponge is fully immersed in mixed liquor, 120min supersound process is carried out to system
(15kHz, 100W/cm2), then sponge is taken out, carries out cleaning treatment.The product of gained is scanned electron microscopic observation and
Bactericidal test.Test result indicates that effectively combined silver oxide/titanium oxide composite nanoparticle upper on sponge substrate surface, and
And sponge dressing modification is shown obvious anti-microbial property, its antibacterial circle diameter has reached 3.7cm.
Embodiment 5：
The Pioloform, polyvinyl acetal sponge of selection is cut, cleaned, wind leaching processing；It is 8g/L, CuO to configure ZnO concentration
Concentration is 8g/L mixing suspension；Pioloform, polyvinyl acetal sponge is fully immersed in mixed liquor, 180min is carried out to system
It is ultrasonically treated (20kHz, 100W/cm2), then Pioloform, polyvinyl acetal sponge is taken out, carries out cleaning treatment.To the product of gained
It is scanned electron microscopic observation and Bactericidal test.Test result indicates that effectively combined on sponge substrate surface upper well dispersed
Zinc oxide nano-particle and copper oxide nano particle, and sponge dressing modification is shown obvious anti-microbial property, its
Antibacterial circle diameter has reached 2.7cm.
Embodiment 6：
The Pioloform, polyvinyl acetal sponge of selection is cut, cleaned, wind leaching processing；Configure Cu (Ac)2Concentration is 2mol/
L solution；Pioloform, polyvinyl acetal sponge is fully immersed in mixed solution, system is carried out 30min supersound process (20kHz,
1000W/cm2), then Pioloform, polyvinyl acetal sponge is taken out, carries out cleaning treatment.Electronic Speculum sight is scanned to the product of gained
Examine and Bactericidal test.Test result indicates that effectively combine upper generated in-situ cupric oxide nano grain on sponge substrate surface
Son, and sponge dressing modification is shown obvious anti-microbial property, its antibacterial circle diameter has reached 3.3cm.
Embodiment 7：
The polyurethane sponge of selection is cut, cleaned, wind leaching processing；Configure Cu (Ac)2Concentration is 0.5mol/L, Zn
(Ac)2Concentration is 0.25mol/L mixed solution；Polyurethane sponge is fully immersed in mixed solution, system is carried out
60min is ultrasonically treated (27kHz, 4000W/cm2), then polyurethane sponge is taken out, carries out cleaning treatment.To the product of gained
It is scanned electron microscopic observation and Bactericidal test.Test result indicates that effectively combined on sponge substrate surface upper generated in-situ
Zinc oxide/cupric oxide composite nanoparticle, and sponge dressing modification is shown obvious anti-microbial property, its inhibition zone
Diameter has reached 4.2cm.
Claims (3)
1. a kind of preparation method of the nanometer particle-modified sponge dressing with antibacterial functions, step are as follows：
(1) sponge material selects the Pioloform, polyvinyl acetal sponge with hydrophily and permeability or is hydrophobic including negative pressure conducting shell
Property perforated foams layer and drainage protective layer be hydrophilic porous sponge layer multilayer sponge material, for sponge former material
Material is pre-processed：Pretreatment includes cleaning, dry, wind leaching processing, cutting, Co60 x ray irradiation xs；
(2) soak is prepared：Soak is soluble metal salt solution or/and nano-metal-oxide particle dispersion：It is solvable
Property metal salt solution be composition for soluble metal salt or metal complex homogeneous aqueous solution, including silver nitrate solution, silver
Ammonia solution, copper ammon solution, copper chloride solution, copper nitrate solution, copper-bath, solution of zinc sulfate, liquor zinci chloridi, zinc nitrate
Solution, nitric acid cadmium solution, iron nitrate solution, acetic acid copper solution, zinc acetate solution, magnesium chloride solution, magnesium nitrate solution, soak
Selection heterogeneity is combined use；Described nano-metal-oxide dispersion liquid composition is that nano-metal-oxide particle is equal
The even uniform suspension for being scattered in gained in solvent, nano-metal-oxide particle include zinc oxide, cupric oxide, magnesia, two
One or both of titanium oxide, vanadic anhydride are mixed above；The concentration of described soluble metal salt solution is
0.02mol/L-1mol/L, the concentration of nano-metal-oxide dispersion liquid is 0.5g/L-10g/L；
(3) sponge substrate that processing is completed in step (1) is fully immersed in the soak of step (2) preparation, opens ultrasound
Ripple is ultrasonically treated；Used ultrasonic intensity is 750-4000W/cm2, frequency 20-27kHz, action time 5-
30min ul-trasonic irradiation pattern；
(4) after ultrasound stops, sponge base-material is removed into soak, it is post-processed, you can is obtained with anti-microbial property
Sponge dressing.
2. the preparation method of the nanometer particle-modified sponge dressing according to claim 1 with antibacterial functions, its feature
It is：Soak selection heterogeneity described in step (2) is combined use, including the mixed solution of copper nitrate, silver nitrate,
The mixed solution or silver nitrate of copper acetate and zinc acetate and the mixed dispersion liquid of nano-titanium oxide, nano cupric oxide with it is nano oxidized
The mixed dispersion liquid of zinc.
3. the preparation method of the nanometer particle-modified sponge dressing according to claim 1 or 2 with antibacterial functions, it is special
Sign is：Sponge post processing used in step (4) includes rinse cleaning, heat blowing drying, cryogenic freezing, Co60 repeatedly
X ray irradiation x, vacuum sealed package.
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| CN107115558A (en) * | 2017-04-27 | 2017-09-01 | 王天湶 | A kind of wound dressing of anti-pigment deposition and preparation method thereof |
| CN108192434A (en) * | 2017-12-26 | 2018-06-22 | 尚蒙科技无锡有限公司 | The preparation method of nano silver copper bimetal granule polyvinyl alcohol antimicrobial compound film |
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| CN109289085B (en) * | 2018-11-09 | 2021-02-02 | 广东体达康医疗科技有限公司 | Novel method for preparing hydrophilic polyurethane silver ion dressing |
| CN111001029B (en) * | 2019-12-31 | 2022-01-04 | 泰州市榕兴医疗用品股份有限公司 | Antibacterial foam dressing and preparation method thereof |
| CN111205427A (en) * | 2020-03-12 | 2020-05-29 | 恩龙实业(嘉兴)有限公司 | Antibacterial foamed plastic and preparation method thereof |
| BR102020011534A2 (en) * | 2020-06-09 | 2021-12-21 | British Ind E Comercio Ltda | Antiviral/antibacterial cleaning sponge manufacturing process and resulting product |
| CN111841634B (en) * | 2020-08-07 | 2023-06-27 | 苏州清德氢能源科技有限公司 | Sponge carrier catalyst for catalytic hydrolysis hydrogen production and preparation method and application thereof |
| CN112480470A (en) * | 2020-11-25 | 2021-03-12 | 南京双威生物医学科技有限公司 | Preparation method of medical polyurethane sponge for wound surface sealing negative pressure drainage |
| CN113476640B (en) * | 2021-06-11 | 2022-10-21 | 中南大学 | Preparation method of antibacterial hydrogel dressing containing heterogeneous ion doped metal sulfide |
| CN114854084B (en) * | 2022-03-31 | 2023-08-18 | 化学与精细化工广东省实验室揭阳分中心 | Sponge with nanoparticle coating and preparation method and application thereof |
| CN115806297A (en) * | 2022-12-01 | 2023-03-17 | 华侨大学 | Preparation method of antibacterial hydrophobic silica aerogel composite material |
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| CN1730803A (en) * | 2005-08-04 | 2006-02-08 | 东华大学 | Nano functional textile finishing method |
| CN102614544A (en) * | 2012-04-16 | 2012-08-01 | 夏毅敏 | Preparation method and application of nano silver antiseptic dressing |
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| CN103785852B (en) * | 2014-01-25 | 2016-08-17 | 华南理工大学 | A kind of nanometer silver-nano micro crystal cellulose complex and preparation method and application |
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| CN1730803A (en) * | 2005-08-04 | 2006-02-08 | 东华大学 | Nano functional textile finishing method |
| CN102614544A (en) * | 2012-04-16 | 2012-08-01 | 夏毅敏 | Preparation method and application of nano silver antiseptic dressing |
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