CN115636666B - Temperature change antibacterial composition, preparation method and application - Google Patents
Temperature change antibacterial composition, preparation method and application Download PDFInfo
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Abstract
The invention discloses a temperature change antibacterial composition, a preparation method and application thereof. The composition of the present invention can provide an antibacterial effect or enhance the antibacterial effect when the temperature is changed, and thus can be used for antibacterial under frequent temperature changes at all times, and the form of the temperature-change antibacterial composition includes but is not limited to an antibacterial coating, a gel or a liquid form. In an exemplary embodiment, the composition of the invention can link the fluctuation characteristics of physiological temperature and environmental temperature with antibacterial performance, combines daily practice, catalyzes the antibacterial effect of pyroelectric particles by utilizing temperature difference change, establishes a self-antibacterial technology, and develops an antibacterial component of a self-antibacterial particle material or a coating material which has a long-acting antibacterial function and can still stably and continuously meet the daily temperature difference amplitude change.
Description
Technical Field
The invention relates to the field of temperature change antibiosis, in particular to a temperature change antibacterial composition, a preparation method and application thereof.
Background
In recent years, physical antibacterial methods have attracted attention in the field of antibacterial technology research because of their advantages such as ease of use, avoidance of bacterial resistance caused by use of drugs, and the like. Common physical antibacterial methods include electric, magnetic, optical, ultrasonic and thermal stimulation methods, and especially electric stimulation antibacterial methods have attracted great interest.
At present, inorganic antibacterial materials are mainly ions, oxides or photocatalytic materials of transition metals such as silver, copper, zinc and the like, and inorganic materials are taken as carriers (ZrO) 2 、TiO 2 ) Most of composite antibacterial products are nano materials with large specific surface area so as to achieve excellent antibacterial effect. Compared with antibiotics and cationic polymers, the antibacterial agent has stable antibacterial effect and better antibacterial effect, and mainly comprises metal and oxides thereofMaterials, photocatalytic antibacterial materials and composite inorganic antibacterial materials.
The inorganic antibacterial material is mainly antibacterial in two ways. The first is that the metal element contacts with the bacteria, acts on the cell membrane and the cell wall of the bacteria, destroys the cell wall and the cell membrane structure, and promotes the dissolution of internal substances, thereby achieving the antibacterial effect. The second is that an antibacterial material containing a metal element is dissolved in a solution. Some of the smaller metal elements can permeate into cells through cell membranes, be used for substances in the cells, react, and then be inactivated to achieve an antibacterial effect.
Chinese patent publication No. CN113827771A discloses a preparation technology of nano composite antibacterial particles, which is a compound formed by chelating polyphenol and metallic silver ions on the surface of medical metal, and improves the bonding strength of nano particles on the surface of medical metal by high temperature treatment, but still realizes antibacterial action by metal ion antibacterial drugs.
Chinese patent publication CN110694493A discloses a preparation method of porous nano antibacterial particles and composite nanofiltration membrane, and a preparation technology of composite nanofiltration membrane, which is to coat porous copper with TiO 2 The nano antibacterial particles are added into the base solution, and the porous nano antibacterial particles are uniformly embedded into the base solution through ultrasonic dispersion or strong stirring to prepare a monomer solution, but the pyroelectric effect of the ferroelectric material is not involved to carry out antibacterial design.
Chinese patent publication CN107653498A discloses a method for preparing a doped antibacterial granular fiber by electrostatic spinning, which comprises adding chitosan quaternary ammonium salt and acetic acid aqueous solution into a mixing vessel to obtain a solution I; adding hydroxyapatite and nano ZnO into the solution I to obtain a solution II; and adding calcium alginate into the solution II to obtain a spinning solution, and then obtaining the doped antibacterial granular fiber by an electrostatic spinning technology.
Although a scheme of sterilizing by using a nano-scale material to generate active oxygen under, for example, light conditions is also disclosed, a specific light condition is required, and the use is limited in a case where there is no light or inconvenience in light. With the development of science and technology, the demand of people for antibiosis is increasing day by day, and more diversified antibiosis schemes are needed.
The information in this background is only for the purpose of illustrating the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is known to a person skilled in the art.
Disclosure of Invention
In order to solve at least part of technical problems in the prior art, the invention provides a composition for realizing antibacterial effect or enhancing antibacterial effect through temperature change, and a preparation method and application thereof. Specifically, the present invention includes the following.
In a first aspect of the present invention, there is provided a temperature-sensitive antibacterial composition comprising, as an antibacterial active ingredient, an inorganic material capable of providing an antibacterial or bacteriostatic effect or enhancing, improving an antibacterial or bacteriostatic effect upon a change in temperature.
In certain embodiments, the temperature-sensitive antimicrobial composition of the present invention, wherein the inorganic material is in the form of particles, powder, or short fibers.
In certain embodiments, the temperature-sensitive antimicrobial composition according to the present invention, wherein the inorganic material comprises a ferroelectric phase material prepared using raw materials comprising barium carbonate, strontium carbonate, and titanium dioxide.
In certain embodiments, the temperature-dependent antimicrobial composition according to the present disclosure, wherein the inorganic material is corona-polarized treated barium strontium titanate.
In a second aspect of the present invention, there is provided a method for preparing a temperature-sensitive antibacterial composition, wherein the temperature-sensitive antibacterial composition comprises an inorganic material as an antibacterial active ingredient, the inorganic material being capable of providing an antibacterial or bacteriostatic effect or enhancing, improving the antibacterial or bacteriostatic effect when temperature is changed, the method comprising a process for preparing the inorganic material by:
(1) Weighing ferroelectric ceramic raw materials, uniformly mixing and levigating to obtain a mixture;
(2) Calcining the mixture at high temperature, carrying out solid-phase reaction to generate an antibacterial particle precursor, and grinding to obtain pyroelectric antibacterial powder;
(3) And (2) carrying out corona polarization treatment on the pyroelectric antibacterial powder to obtain the inorganic material, wherein the parameters of the corona polarization treatment comprise: the polarization voltage is 1-30kV, the polarization distance is 1-50mm, and the polarization time is 1-60min.
In certain embodiments, the high temperature calcination includes pre-sintering the mixture at 1250-1350 ℃ for 1-3 hours, cooling and granulating, raising the temperature to 1350-1450 ℃ by a staged temperature raising process for 3-5 hours, and then cooling to room temperature by a staged temperature lowering process.
In certain embodiments, the method for preparing a temperature-varying antibacterial composition according to the present invention, wherein the stepwise temperature-increasing process comprises increasing the temperature at 0.5-1.5 ℃/min to 500-700 ℃, maintaining the temperature for 2-4 hours, and then increasing the temperature at 2-4 ℃/min to 1350-1450 ℃, and the stepwise temperature-decreasing process comprises decreasing the temperature at 2-4 ℃/min from 1350-1450 ℃ to 500-700 ℃, and then naturally cooling to room temperature.
In a third aspect of the invention, there is provided a method of combating or enhancing the combating of bacteria, wherein there is used the step of applying a composition according to the first aspect of the invention.
In certain embodiments, the method of antimicrobial or enhancing antimicrobial activity according to the present invention, wherein the temperature of the composition is varied within a temperature interval, preferably the temperature interval comprises the curie temperature of the inorganic material.
In a fourth aspect of the present invention there is provided the use of an inorganic material in the manufacture of an antimicrobial composition, wherein the inorganic material is selected from barium titanate and/or barium strontium titanate.
The composition of the invention can provide antibacterial effect or enhance and improve antibacterial effect when temperature changes, and can be suitable for various environments with temperature changes. For example, the oral cavity of a human body is constantly in a state of frequent temperature changes due to the characteristics of daily activities and physiological functions (such as diet, speech, respiration, etc.). Therefore, in an exemplary embodiment, the composition of the invention can link the fluctuation characteristics of physiological temperature and environmental temperature with antibacterial performance, combine daily practice, catalyze the antibacterial effect of the pyroelectric particles by using temperature difference change, establish a self-antibacterial technology, and develop a self-antibacterial particle material which has long-acting antibacterial function and can meet the requirement of stable and continuous operation under the change of daily temperature difference amplitude.
Drawings
Fig. 1 is an XRD pattern of an exemplary inorganic material.
FIG. 2 is an electron micrograph of a particle obtained in example 2 of the present application.
Fig. 3 illustrates the antimicrobial effect of inorganic materials against gram-negative bacteria.
Fig. 4 illustrates the antimicrobial effect of an inorganic material against gram-positive bacteria.
FIG. 5 shows the antibacterial effect of the inorganic material of the present invention when a temperature-varying treatment is performed on a coated flat plate.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that the upper and lower limits of the range, and each intervening value therebetween, is specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control. Unless otherwise indicated, "%" is percent by weight.
In a first aspect of the present invention, there is provided a temperature-change antibacterial composition, sometimes also referred to herein simply as "the composition of the present invention", which achieves antibacterial or bacteriostatic action or enhances, improves the antibacterial or bacteriostatic effect by temperature change within a certain temperature change range, the composition of the present invention comprising an inorganic material as an antibacterial active ingredient.
The form of the temperature-change antibacterial composition of the present invention is not limited and may be any form, and examples thereof include antibacterial coatings, gels or liquid forms. In an exemplary embodiment, the temperature-sensitive antimicrobial composition of the present invention is an antimicrobial coating for environmental, sanitary, household materials. Preferably, it is an antimicrobial coating applied to the surface of an object. In an exemplary embodiment, the temperature-change antibacterial composition of the present invention is a plastic gel composition.
In the present invention, the temperature-variable range is not particularly limited in general, but in order to have higher temperature-variable antibacterial activity, it is preferable that the temperature-variable range crosses the curie temperature of the inorganic material or that the boundary of the temperature-variable range is the curie temperature. For example, when the curie temperature of the inorganic material is 30 ℃, the temperature variation range may be, for example, 20 to 50 ℃, 25 to 45 ℃,30 to 45 ℃, or the like.
In the present invention, the inorganic material is an inorganic material capable of generating a free charge when the temperature is changed. Preferably a ferroelectric phase material, such as a barium strontium titanate material, prepared using a feedstock comprising barium carbonate, strontium carbonate and titanium dioxide. For example, the composition is (Ba) x Sr 1-x )TiO 3 Wherein x is a number between more than 0 and less than 1, preferably x is 0.5-0.95, such as 0.6, 0.7, 0.8, etc. In the present invention, the inorganic material may also be doped barium strontium titanate.
In certain embodiments, the inorganic material of the present invention is (Ba) x Sr 1-x )TiO 3 Wherein, the temperature changing range is selected according to the x value. As a general rule, every time x is increased or decreased by 0.1, the temperature is increased or decreased by about 3.3 ℃ on the basis of the standard variable temperature range, that is, the upper limit or the lower limit of the standard variable temperature range is increased or decreased by 3.3 ℃. Standard variable temperature rangeSo as to be a standard temperature range corresponding to different values of x, which is determined by experiments, within which the curie temperature at the inorganic material lies. For example, when x is 0.7, if the corresponding standard temperature swing range is 20-45 ℃, then when x =0.5 is used, the preferred reference temperature swing range for antimicrobial selection is 23-48 ℃.
In certain embodiments, given the temperature range for a particular application, the value of x is selected based on the temperature range. For example, in the case of antibacterial at a daily environment, for example, at 20 to 45 ℃, x is preferably 0.65 to 0.75, and more preferably 0.7, to have a higher temperature-swing antibacterial activity.
The form of the inorganic material of the present invention is not particularly limited, and may be a particle or a short fiber. In the case of particles, the particle diameter is not particularly limited, and may be 10nm to 10 μm, for example, 100nm to 8 μm, 500nm to 5 μm, 800nm to 3 μm, 1 to 3 μm. In the case of staple fibers, the aspect ratio of the fibers is (1-30): 1, preferably (1.5-20): 1, more preferably (3-10): 1, e.g., (3-5): 1, and the like. In exemplary embodiments, the staple fibers have a length of 1 to 10 μm, such as 2 to 8 μm, 3 to 5 μm, and the like. In further exemplary embodiments, the staple fibers have a diameter of 10 to 600nm, 20 to 500nm, 50 to 300nm, 100 to 400nm, 200 to 400nm, and the like. Particle size in this context refers to the longest straight line distance through the interior of the particle. The larger the aspect ratio, the more the antibacterial property tends to be improved under the same conditions. In certain embodiments, the present invention uses inorganic ferroelectric ceramic particles having a particle size of 1 to 3 μm. The inorganic material has uniform structure and stable electrical property, thereby better playing the role of antibiosis. In certain embodiments, the present invention uses ferroelectric ceramic short fibers having an aspect ratio of 1 to 6 to achieve enhanced antimicrobial activity, perhaps because the short fibers are more conducive to the conduction of electrical current generated by the inorganic material.
In certain embodiments, the inorganic material of the present invention is a ferroelectric phase material prepared using a feedstock comprising barium carbonate, strontium carbonate, and titanium dioxide.
In the present invention, the form of the temperature-change antibacterial composition is not particularly limited as long as it contains or consists of the inorganic material of the present invention, and may be, for example, a solid state, a gel state or a liquid.
In a second aspect of the present invention, a method for preparing a temperature-sensitive antibacterial composition is provided. The production method of the present invention is not particularly limited, and may be any known method.
In certain embodiments, the preparation method of the present invention is a solid phase sintering reaction method, which at least comprises:
(1) Weighing ferroelectric ceramic raw materials, uniformly mixing and levigating to obtain a mixture;
(2) Calcining the mixture at high temperature, carrying out solid-phase reaction to generate an antibacterial particle precursor, and grinding to obtain pyroelectric antibacterial powder;
(3) And carrying out corona polarization treatment on the pyroelectric antibacterial powder to obtain the pyroelectric antibacterial particles, wherein the parameters of the corona polarization treatment comprise: the polarization voltage is 1-30kV, the polarization distance is 1-50mm, and the polarization time is 1-60min.
The step (1) of the invention is a material ball milling step, which comprises the steps of calculating the raw material proportion of different components according to the stoichiometric ratio, weighing raw material powder, putting the raw material powder into a ball milling tank, adding zirconia balls for milling, and adopting wet ball milling and absolute ethyl alcohol as a ball milling medium. Pouring the mixture into 2/3 of absolute ethyl alcohol in the volume of a ball milling tank, and carrying out ball milling on the mixture by a horizontal ball mill. And pouring the uniformly mixed original powder and absolute ethyl alcohol into a clean glass dish, and drying in a vacuum drying oven at the temperature of 80 ℃.
The step (2) of the invention is a step of sintering to generate the antibacterial particle precursor, which comprises the steps of pre-sintering the mixture at 1250-1350 ℃ for 1-3 hours, cooling and granulating, raising the temperature to 1350-1450 ℃ by a staged temperature raising program, keeping the temperature for 3-5 hours, and then cooling to room temperature by a staged temperature lowering program. The present invention has found that if the temperature of the stepwise temperature-rising temperature-programming is too high, e.g. above 1450 ℃, the resulting temperature antibacterial activity tends to become low, possibly because the particles of crystals obtained by the too high temperature tend to become large and the ferroelectric properties tend to become low. On the other hand, if the temperature is too low, e.g., below 1350 ℃, the antibacterial activity also tends to become low, possibly because the temperature is too low and the temperature at which atoms are diffused is not reached at the time of sintering, resulting in incomplete crystal growth.
In the present invention, the pre-sintering process comprises raising the temperature to 1250-1350 ℃ at 1-5 ℃/min, such as 2, 3 or 4 ℃/min, such as 1300 ℃ for 1, 2 or 3 hours. And then the mixture is put into a mortar for grinding after being cooled, and then is poured into a ball milling tank for secondary ball milling on a planetary ball mill, and the high-speed rotation of the planetary ball mill can lead the ball milling medium to grind and crush the pre-sintered powder, so that the powder is more uniform and fine. Next, the temperature is raised to 1350-1450 ℃ by a stepwise temperature raising program, for example, 1300 ℃ for 3-5 hours. An exemplary stepwise temperature ramp-up procedure includes ramping up to 600 ℃ at 1 ℃/min, holding the temperature at 600 ℃ for 3 h, then ramping up to 1350-1450 ℃ at 3 ℃/min, and holding the temperature for 4 h. Then, the temperature is reduced by a staged temperature reduction procedure, which comprises the step of reducing the temperature to 600 ℃ at the speed of 3 ℃/min, and then, the temperature is cooled to the room temperature along with the furnace.
Step (3) of the invention is a corona polarization treatment step, wherein the parameters of the corona polarization treatment comprise: the polarization voltage is 1-30kV, such as 10 kV, 15 kV, 20 kV, 25kV, etc. The polarization distance is 1-50mm, such as 10mm, 20mm, 30mm, 40mm, etc. The polarization time is 1-60min, such as 5 min, 10 min, 15 min, 20 min, 25 min, 30min, 40 min and 50 min.
In a third aspect of the invention, there is provided an antibacterial method or a method of enhancing antibacterial effect, sometimes referred to herein simply as the "method of the invention", comprising the step of using a composition according to the invention, either in vitro or in vivo. Examples of in vitro methods include methods for inhibiting or reducing bacterial activity in a product, for example, by adding a composition of the invention to the product, and the like. Preferably, the method of the invention further comprises the step of varying at least the temperature of the composition within a defined temperature interval. The temperature range is a range that is determined according to the actual application and the components of the composition. Preferably, the curie temperature of the inorganic particles is within the temperature interval.
The method of the present invention can be used for inhibiting, reducing or killing various bacteria including gram-positive bacteria represented by Streptococcus mutans or gram-negative bacteria represented by Escherichia coli.
Examples
1. Batching ball mill
With BaCO 3 、SrCO 3 And TiO 2 The powder is used as a raw material, the raw material ratios of different components are calculated according to the stoichiometric ratio of table 1, the raw material powder is weighed and put into a ball milling tank, zirconia ball milling beads are added, wet ball milling is adopted, and absolute ethyl alcohol is used as a ball milling medium. Pouring 2/3 of absolute ethyl alcohol in the volume of the ball milling tank, and ball milling for 8-12 h on a horizontal ball mill at the rotating speed of 150 r/min. And pouring the uniformly mixed original powder and absolute ethyl alcohol into a clean glass vessel, and putting the glass vessel into a vacuum drying oven at the temperature of 80 ℃ for drying for 2 hours.
2. Presintering and secondary ball milling
Pouring the dried mixed powder into a crucible, putting the crucible into a muffle furnace, and performing a pre-sintering process under the air, wherein the sintering process comprises the following steps: heating to 1300 ℃ at the speed of 3 ℃/min and preserving the heat for 2 h. And (3) putting the pre-sintered powder into a mortar for grinding for 30min, pouring the powder into a ball milling tank, carrying out secondary ball milling on a planetary ball mill, carrying out ball milling for 8-12 h at the speed of 300 r/min, and enabling a ball milling medium to grind and crush the pre-sintered powder by the high-speed rotation of the planetary ball mill so as to enable the powder to be more uniform and fine. And pouring the secondary ball-milling powder into a clean glass vessel, and drying in a vacuum drying oven at 80 ℃ to obtain the secondary ball-milling powder.
3. Granulating and sieving
Preparing a 5% polyethylene glycol aqueous solution (PVA) as a plasticizer, adding the PVA as a plasticizer into the secondary ball-milling powder for granulation, adding the PVA with the mass being 15% of the mass of the secondary ball-milling powder, grinding the mixture of the PVA and the powder in a mortar for 30min, removing oversize powder and undersize powder through 100-mesh and 200-mesh sieves, and remaining powder with proper particle size for tabletting and forming.
4. Tabletting and forming
In the experiment, an automatic mechanical dry pressing method is adopted to tablet the powder, a proper amount of sieved powder is poured into a die, the powder is extruded and molded through an upper smooth gasket and a lower smooth gasket, the pressurizing parameter of the automatic tablet press is set to be 10 MPa, the pressure is maintained for 1 min, and finally, the cylindrical BST pyroelectric ceramic green sheet with the thickness of about 1 mm and the diameter of about 10mm is obtained from the die.
5. Sintering
Sintering is the most important process in the preparation process of the pyroelectric ceramic. Due to the fact that PVA is added in the experimental process, the PVA volatilizes along with the rise of the temperature in the sintering process, if the temperature rise is too fast, cracking and deformation of the ceramic chip can be caused, the process of keeping the temperature at 600 ℃ for 3 hours and discharging glue needs to be added in the sintering procedure, and the temperature rise rate cannot be too fast before discharging glue. In addition, in order to ensure that the pyroelectric ceramic sample prepared by sintering has high compactness and good crystallinity, various parameters such as the temperature rise rate, the sintering temperature, the heat preservation time and the like of the muffle furnace need to be controlled. Through experimental exploration, the sintering procedure is finally determined as follows: heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 3 h at the temperature of 600 ℃ for binder removal, heating to 1350-1450 ℃ at the speed of 3 ℃/min, preserving heat for 4 h, cooling to 600 ℃ at the speed of 3 ℃/min, and then cooling to room temperature along with the furnace to obtain the BST pyroelectric ceramic.
6. Post-treatment
And (3) grinding the surface of the sample by using sand paper or a polishing machine, removing the surface layer and flattening the upper surface and the lower surface. Ultrasonically cleaning the polished BST pyroelectric ceramic, coating a silver electrode by a screen printing method, transferring a sample to a muffle furnace, keeping the temperature at 600 ℃ for 15 min at the heating rate of 3 ℃/min, and then putting the BST pyroelectric ceramic sample with the prepared electrode into silicon oil for polarization. Parameters of the corona polarization treatment include polarization voltage 25kV, polarization distance 30mm, and polarization time 30min.
TABLE 1
Comparative example 1
Taking BaTiO 3 The particles are processed by corona polarization to obtain polarized BaTiO 3 Particles; parameters of the corona polarization treatment include: the polarization voltage is 25kV, the polarization distance is 35mm, and the polarization time is 30min.
Test example
1. Structural characterization
Taking different pyroelectric antibacterial particles for standby, and scanning with an X-ray diffractometer. The instrument is a German Bruker-AXS D8 Advance XRD diffractometer. CuK α rays with λ =1.5409 a were used as incident light, with a scanning range of 20-80 °, and a scanning speed of 10 °/min (about 25 ℃). The results are shown in FIG. 1. The XRD image in the range of 45 deg. -46.5 deg. was magnified (right side of FIG. 1) for a clearer analysis of the peak pattern at {200 }.
2. Characterization of microscopic Properties
The microscopic morphology of the different particles was characterized using a Scanning Electron Microscope (SEM) and the sample grain size and distribution was analyzed using Nano Measurer software. Specifically, the pyroelectric antibacterial particles are taken for standby, sprayed with gold, and a SEM image and an energy spectrum are taken through a computer. As shown in FIG. 2, the ceramic powder microscopic showed irregular particles of 50-2000 nm size with a median of about 400nm.
3. Antibacterial property
By dilution coating plate method, specifically, taking out pyroelectric particles, and performing cooling and heating cycle (25-45 deg.C) or constant temperature (37 deg.C) with 500 μ L (10) 4 CFU/mL) Streptococcus mutans/E.coli co-culture, 100. Mu.l was applied to BHI agar plates, spread evenly, and placed in a carbon dioxide incubator for 48 hours. The diluted coated plates were scanned and the antibacterial activity, i.e., the log of microbial kill = lg (blank control colony count/experimental colony count, results are shown in fig. 3 and 4.
In addition, the present invention also tested the inhibitory effect of the composition of the present invention on complex flora. It is prepared by the following steps: gargling without brushing teeth for 24 hours, collecting dental plaque on the surface of dental caries by using a sterile cotton swab, inoculating fresh dental plaque into BHI solution which is prepared in advance and sterilized at high temperature and high pressure, and diluting the bacterial liquid concentration to 2.4X10 7 CFU/ml。
In addition, the materials of examples 1-3 were tested for antimicrobial performance without polarization. The results are shown in Table 2. The specific test method is the same as before.
TABLE 2
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Many modifications and variations may be made to the exemplary embodiments of the present description without departing from the scope or spirit of the present invention. The scope of the claims is to be accorded the broadest interpretation so as to encompass all modifications and equivalent structures and functions.
Claims (7)
1. A method for improving antibacterial activity by using temperature difference change is characterized in that the temperature of a temperature-variable antibacterial composition is frequently changed by cold and heat within a temperature range of 25-45 ℃;
wherein the temperature change antibacterial composition comprises an inorganic material barium strontium titanate Ba 0.7 Sr 0.3 TiO 3 The inorganic material can enhance and improve the antibacterial or bacteriostatic effect when the temperature changes; and the temperature interval comprises the curie temperature of the inorganic material.
2. The method of claim 1, wherein the inorganic material is in the form of particles, powder, or short fibers.
3. The method of claim 1, wherein the inorganic material is a ferroelectric phase material prepared from barium carbonate, strontium carbonate, and titanium dioxide.
4. The method of claim 1, wherein the temperature-sensitive antimicrobial composition is in the form of an antimicrobial coating, a gel, or a liquid.
5. The method of claim 1, wherein the preparing method of the temperature-change antibacterial composition comprises a process of preparing an inorganic material by:
(1) Weighing ferroelectric ceramic raw materials, uniformly mixing and levigating to obtain a mixture;
(2) Calcining the mixture at high temperature, carrying out solid-phase reaction to generate an antibacterial particle precursor, and grinding to obtain pyroelectric antibacterial powder;
(3) And carrying out corona polarization treatment on the pyroelectric antibacterial powder to obtain the inorganic material, wherein the parameters of the corona polarization treatment comprise: the polarization voltage is 1-30kV, the polarization distance is 1-50mm, and the polarization time is 1-60min.
6. The method of claim 5, wherein the high temperature calcination comprises pre-sintering the mixture at 1250-1350 ℃ for 1-3 hours, cooling down the mixture to pelletization, raising the temperature to 1350-1450 ℃ in a staged temperature raising procedure for 3-5 hours, and then cooling down the mixture to room temperature in a staged temperature lowering procedure.
7. The method of claim 6, wherein the stepwise ramp-up procedure comprises ramp-up to 500-700 ℃ at 0.5-1.5 ℃/min for 2-4 hours, then ramp-up to 1350-1450 ℃ at 2-4 ℃/min, and the stepwise ramp-down procedure comprises ramp-down from 1350-1450 ℃ to 500-700 ℃ at 2-4 ℃/min, then natural cooling to room temperature.
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| CN107986775A (en) * | 2017-12-19 | 2018-05-04 | 广东工业大学 | A kind of barium strontium titanate (BST) thick film and preparation method thereof |
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| CN115252872A (en) * | 2022-09-30 | 2022-11-01 | 北京大学口腔医学院 | Antibacterial dressing based on ferroelectric material and preparation method and application thereof |
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