CN115852590B - Natural antibacterial antistatic nanofiber membrane and preparation method and application thereof - Google Patents
Natural antibacterial antistatic nanofiber membrane and preparation method and application thereof Download PDFInfo
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- CN115852590B CN115852590B CN202211187681.8A CN202211187681A CN115852590B CN 115852590 B CN115852590 B CN 115852590B CN 202211187681 A CN202211187681 A CN 202211187681A CN 115852590 B CN115852590 B CN 115852590B
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Abstract
The invention discloses a natural antibacterial antistatic nanofiber membrane, a preparation method and application thereof. The novel nanofiber membrane is prepared by using natural polymer substances and nano silver particles through electrostatic spinning. Compared with the prior art, the self-cleaning agent has higher antibacterial property, better biocompatibility and electrostatic adsorption self-cleaning function, and can be widely used in various fields such as facial masks, skin beauty and medical film coating.
Description
Technical Field
The invention relates to the field of antibacterial materials, in particular to a nanofiber membrane prepared from an antibacterial high polymer material and a nano substance and a preparation method thereof, wherein the nanofiber membrane is applicable to composite structure nanofiber substrates of all human bodies.
Background
The nanofiber prepared by adopting the electrostatic spinning technology has the characteristics of large specific surface area and high porosity, and can be widely applied in various fields by utilizing synthetic or natural polymer substances. The nanofiber prepared by adopting the electrostatic spinning is formed into a three-dimensional porous net in a molten net form at the same time of fiber generation, and is used as an efficient super-energy separation material, a medical material, an artificial blood vessel and a nano composite material due to the characteristics of large specific surface area and high porosity.
When the polymer is applied to the fields of skin beauty and medical polymer materials, the stability of the materials in biology, chemistry, physics, mechanics, sterilization stability and molding processing is required to be ensured. From the small aspect, the characteristics of no toxicity, stability and safety to human body are required to be considered. That is, in order to block the movement of bacteria or viruses, and to smoothly discharge water vapor generated from the skin while blocking the movement of microorganisms by forming a porous film having an appropriate pore size, it is required to further improve the performance based on the conventional products, and a film capable of improving the moisture transfer rate and the air permeability and maximally improving the antibacterial property from the physical and chemical aspects has been developed.
In view of this, there is a need for developing various nanofiber products which can fully exhibit the above-mentioned advantages of nanofibers and can be applied to skin beauty and medical polymers.
The information in the background section is only for the purpose of illustrating the general background of the invention and is not to be construed as an admission or any form of suggestion that such information forms the prior art that is well known to those of ordinary skill in the art.
Disclosure of Invention
In order to solve at least part of the technical problems in the prior art, the invention provides a natural antibacterial antistatic nanofiber membrane, 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 method for preparing a natural antibacterial antistatic nanofiber membrane, comprising the steps of:
(1) Doping nano silver particles into a biodegradable polymer solution to obtain a composite solution; and
(2) The composite solution is made to flow through the capillary outlet under the action of high voltage and is collected to the collecting device to form nanometer fiber film on the surface of the collecting device, with the distance between the capillary outlet and the collecting device being 5-20cm.
In certain embodiments, the method for preparing a natural antibacterial antistatic nanofiber membrane according to the present invention, wherein the nano silver particles are treated silver particles, the treatment comprising adding 0.01-0.1mol/L of aqueous dopamine solution to the nano silver particles and reacting for 5-10 hours under stirring.
In certain embodiments, the natural antibacterial antistatic nanofiber membrane according to the present invention may be prepared by a method wherein the amount of the nano silver particles is 0.5 to 10% of the weight of the biodegradable polymer.
In certain embodiments, the method for preparing a natural antibacterial antistatic nanofiber membrane according to the present invention, wherein the biodegradable polymer is selected from at least one of the group consisting of collagen, gelatin, alginate, hyaluronic acid, chitosan, and copolyesters of hydroxybutyric acid and hydroxyvaleric acid.
In certain embodiments, the method for preparing a natural antibacterial antistatic nanofiber membrane according to the present invention, wherein the solvent of the biodegradable polymer solution comprises at least one of dimethylformamide, tetrahydrofuran, water, isopropanol, dichloromethane and chloroform.
In certain embodiments, the method of preparing a natural antibacterial antistatic nanofiber membrane according to the present invention, wherein the high voltage electricity is 1-20kv.
In certain embodiments, the natural antibacterial antistatic nanofiber membrane according to the present invention may be prepared in a concentration of 0.5 to 10% by weight in the biodegradable polymer solution.
In certain embodiments, the method for preparing a natural antibacterial antistatic nanofiber membrane according to the present invention further comprises (3) subjecting the nanofiber membrane to a direct current electric field treatment at a field strength of 0.1-10kV/mm for 5-60min.
In a second aspect of the invention, there is provided a natural antibacterial antistatic nanofiber membrane prepared by the method of the first aspect.
In a third aspect of the invention, there is provided the use of a natural antibacterial antistatic nanofibrous membrane for the preparation of cosmetic and medical antibacterial products of the skin.
In certain embodiments, the products include paper diapers, facial masks, sanitary napkins, make-up removal cottons, bedsheets, nursing films, and wound repair materials.
The invention prepares the novel nanofiber membrane by using natural polymer substances and nano silver particles through electrostatic spinning. Compared with the existing product, the product has higher antibacterial property, better biocompatibility and electrostatic adsorption self-cleaning function, and can be widely used in various fields such as facial masks, skin beauty and medical film coating.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions 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. In addition, for numerical ranges in the present invention, it is understood that the upper and lower limits of the ranges and each intermediate value therebetween are specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, 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 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.
Herein, the term "natural antibacterial antistatic nanofiber membrane" refers to a membrane material composed of fine fibers having a fiber diameter of less than 500nm while being filled with nano silver particles inside the fine fibers of the membrane. The nano fiber is doped with silver particles, so that the nano fiber film has antibacterial activity or the antibacterial activity of the film material is enhanced. In addition, the film material has an antistatic function due to the conductivity of the silver particles. The natural antibacterial antistatic nanofiber membrane is sometimes abbreviated herein as "nanofiber membrane".
[ preparation method ]
In a first aspect of the present invention, there is provided a method for preparing a natural antibacterial antistatic nanofiber membrane, comprising at least the following steps (1) and (2), and optionally step (3):
(1) Doping nano silver particles into a biodegradable polymer solution to obtain a composite solution;
(2) The composite solution is enabled to generate jet flow through a capillary outlet under the action of high-voltage electricity and is collected to a collecting device, so that a nanofiber membrane is formed on the surface of the collecting device, wherein the distance between the capillary outlet and the collecting device is 5-20cm;
(3) And (3) carrying out direct current electric field treatment on the nanofiber membrane for 5-60min under the field intensity of 0.1-10 kV/mm.
In the invention, the doping of nano silver particles is beneficial to the functionalization of fibers, such as antibacterial activity and antistatic property. Nano silver particles refer to silver microparticles having diameters in the nano range. Preferably, the average diameter of the silver nanoparticles is generally less than the diameter of the nanofibers, preferably less than 1/2, preferably 1/3 of the diameter of the nanofibers. For example, the average diameter of the nano silver particles is 200nm or less, preferably 150nm or less, more preferably 100nm or less, such as 80, 60, 40nm.
In the invention, the nano silver particles are preferably particles subjected to surface treatment, so that the compatibility of the nano silver particles with biopolymers is improved, and the fiber strength reduction caused by nano particle doping is reduced. Preferred surface treatments include dopamine surface modification, for example, dopamine film polymerized on the surface of silver particles by chemical oxidative polymerization, enzyme catalyzed oxidative polymerization, electrochemical polymerization or photopolymerization of dopamine. An exemplary treatment method comprises adding silver particles to 0.01-0.1mol/L aqueous dopamine solution, stirring at 40-80deg.C for 6-12 hr, and then performing ultrasonic vibration for 1-15 min.
In the present invention, the amount of the nano silver particles is generally 0.5 to 10%, preferably 0.5 to 8%, more preferably 1 to 5% based on the weight of the biodegradable polymer. If the amount of the nano silver particles is too low, the antistatic or antibacterial effect of the resulting film material tends to be lowered, even without the antistatic effect or the desired antibacterial effect is not achieved. On the other hand, if the amount of the nano silver particles is too high, the fiber strength tends to decrease and the formation of the fiber at the time of preparation is affected.
In the present invention, the biodegradable polymer is generally a naturally derived biopolymer, which has excellent biocompatibility or absorbability and biodegradability. Examples of such biopolymers include, but are not limited to, collagen, gelatin, alginate, hyaluronic acid, chitosan, and copolyesters of hydroxybutyric acid and hydroxyvaleric acid. The present invention may use a combination of one or more of the above polymers. In certain embodiments, the present invention uses copolyesters of hydroxybutyrate and hydroxyvalerate (i.e., β -hydroxybutyrate-co- β -hydroxyvalerate, PHBV) as biopolymers of natural origin. Preferably, the molar ratio of hydroxyvalerate in PHBV is 40% or less, preferably 20% or less, more preferably 10% or less, for example 5%, 4%, 3%, 2%, 1%. The higher the molar ratio of hydroxyvalerate, the lower the tensile strength tends to be, and even the fibers of the desired strength are not obtained.
In the present invention, the amount of the biodegradable polymer to be used can be freely selected depending on the nature of the polymer component, the nature of the solvent, the desired fiber diameter, and the like. Typically 0.5-10% by weight. For example 1% -8%, 2% -6%, 4% -6%. When the polymer is a copolyester of hydroxybutyric acid and hydroxyvaleric acid, its concentration is generally 0.8-1.5%, so that a fiber with a diameter of 100-200nm is obtained. If the amount is too large, the viscosity of the solution tends to increase, so that the diameter of the resulting fiber becomes large.
In the present invention, the solvent for dissolving the biopolymer includes dimethylformamide, tetrahydrofuran, water, isopropyl alcohol, methylene chloride and chloroform. One kind of the above-mentioned materials may be used in the present invention, or two or more kinds may be used in combination. The amount of the solvent to be used is not limited as long as the concentration of the biopolymer in the resulting solution can be controlled within a desired range.
In the present invention, the high voltage electricity may be generated by known devices, and the high voltage electricity is generally 1 to 20kV, for example, 2kV, 4kV, 6kV, 10kV, 15kV, 16kV, 18kV, etc.
In the invention, the nanofiber membrane obtained in the steps (1) and (2) can be further subjected to a strong direct current electric field treatment, so that the antibacterial property of the nanofiber membrane is further improved. The reason why the antibacterial property is improved by the treatment of the strong direct current electric field is not clear, probably because the treatment changes the crystallization mode in the polymer materials such as PHBV and the like and improves the piezoelectric constant, thereby leading the polymer materials to have certain antibacterial activity. And meanwhile, doped silver particles are further combined, so that the antibacterial effect of the nanofiber membrane is greatly improved.
Example 1
This example is an exemplary method of preparing a natural antimicrobial antistatic nanofiber membrane. The main raw materials of this example are as follows: the copolyester PHBV of hydroxybutyric acid and hydroxyvaleric acid has the number average molecular weight Mn=45 ten thousand and the mass fraction of the hydroxyvaleric acid is 2%; the average diameter of the dopamine-coated nano silver particles is 50nm.
The preparation method comprises the following steps:
the nano silver particles are added into a solution of PHBV with concentration of 2wt% in dichloromethane according to the amount of 2wt% of PHBV, fully stirred, and subjected to ultrasonic treatment to obtain a composite solution.
The composite solution was added to a syringe connected to the outlet of the capillary, a 10kv high pressure was generated using a direct current high pressure generator JG50-1, while a pressure was applied to the composite solution by a propeller pump, thereby forming a jet stream of 0.5ml/L, and the fibers were collected by a metal collecting plate at a distance of 10cm from the outlet of the capillary to form a net-shaped nanofiber membrane.
Example 2
This example is an exemplary method of preparing a natural antimicrobial antistatic nanofiber membrane. The main raw materials of this example are as follows: the copolyester PHBV of hydroxybutyric acid and hydroxyvaleric acid has the number average molecular weight Mn=45 ten thousand and the mass fraction of the hydroxyvaleric acid is 3%; the average diameter of the dopamine-coated nano silver particles is 50nm.
The preparation method comprises the following steps:
the nano silver particles are doped into a PHBV solution with the concentration of 2wt% in dichloromethane according to the amount of 2wt% of PHBV, fully stirred, and subjected to ultrasonic treatment to obtain a composite solution.
The composite solution was added to a syringe connected to the capillary outlet, a 10kv high pressure was generated using a direct current high pressure generator JG50-1, while a pressure was applied to the composite solution by a propeller pump to form a 0.5ml/L jet, and fibers were collected by a metal collecting plate 10cm from the capillary outlet to form a net-shaped nanofiber membrane. Next, a DC electric field of 1kV/mm was applied to the net-shaped nanofiber membrane for a treatment time of 30 minutes.
Example 3
This example is another exemplary method of preparing a natural antimicrobial antistatic nanofiber membrane. The main raw materials of this example are as follows: hydroxybutyric acid and hydroxyvalerate copolyester PHBV with number average molecular weight Mn=45 ten thousand and mass fraction of hydroxyvalerate 1.5%; the average diameter of the dopamine-coated nano silver particles is 60nm.
The preparation method comprises the following steps:
the nano silver particles are doped into a PHBV solution with the concentration of 2wt% in dichloromethane according to the amount of 1wt% of PHBV, fully stirred, and subjected to ultrasonic treatment to obtain a composite solution.
The composite solution was added to a syringe connected to the capillary outlet, a 10kv high pressure was generated using a direct current high pressure generator JG50-1, while a pressure was applied to the composite solution by a propeller pump to form a 0.5ml/L jet, and the ordered fibers were collected by a winding drum at a distance of 10cm from the capillary outlet to form a nanofiber membrane.
Comparative example
A nanofiber membrane was prepared in the same manner as in example 1, except that the material composition or treatment was changed as shown in table 1.
Test case
Coli was used as the test bacteria. The concentrated bacterial solution in the stationary phase is diluted to a desired concentration with physiological saline. And (3) taking 50 mu L of fungus liquid to drop on one side of the membrane material, covering a glass slide, and lightly pressing to uniformly disperse the fungus liquid. Sealing with sealing film, and culturing in incubator at 37deg.C for 1-2 hr. The bacterial fluid was diluted each time with a blank.
The membrane material and the glass slide after a certain period of culture are immersed in 10mL of physiological saline and shaken well. Dripping 100 μl of fungus onto culture medium, spreading, sealing, and culturing at 37deg.C for 12 hr. Then, the medium was taken out, colonies were counted, and the sterilization rate was calculated. The results are shown in Table 1.
TABLE 1
Note that: 1 represents the weight based on PHBV.
While the 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. Various modifications or changes may be made to the exemplary embodiments of the present disclosure without departing from the scope or spirit of the 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 (6)
1. The preparation method of the natural antibacterial antistatic nanofiber membrane is characterized by comprising the following steps of:
(1) Doping nano silver particles into a biodegradable polymer solution to obtain a composite solution, wherein the biodegradable polymer is copolyester of hydroxybutyric acid and hydroxyvaleric acid, the molar ratio of the hydroxyvaleric acid in the copolyester is below 10%, the concentration of the biodegradable polymer solution is 0.8-1.5wt%, the nano silver particles are treated silver particles, the treatment comprises adding 0.01-0.1mol/L of dopamine aqueous solution into the nano silver particles, stirring and reacting for 5-10 hours at the temperature of 40-80 ℃, and then carrying out ultrasonic oscillation for 1-15 minutes, so that a polymerized dopamine film is formed on the surface of the silver particles;
(2) Jet flow is generated from the composite solution through a capillary outlet under the action of high voltage of 1-20kv and is collected to a collecting device, so that a nanofiber membrane is formed on the surface of the collecting device, wherein the distance between the capillary outlet and the collecting device is 5-20cm; and
(3) And (3) carrying out direct current electric field treatment on the nanofiber membrane for 5-60min under the field intensity of 0.1-10 kV/mm.
2. The method for preparing a natural antibacterial antistatic nanofiber membrane according to claim 1, wherein the doping amount of the nano silver particles is 0.5-10% of the weight of the biodegradable polymer.
3. The method for preparing a natural antibacterial and antistatic nanofiber membrane according to claim 1, wherein the solvent of the biodegradable polymer solution comprises at least one of dimethylformamide, tetrahydrofuran, water, isopropanol, dichloromethane and chloroform.
4. A natural antibacterial antistatic nanofiber membrane prepared by the method according to any one of claims 1 to 3.
5. The use of the natural antibacterial antistatic nanofiber membrane according to claim 4 for preparing a skin cosmetic and medical antibacterial product.
6. Use according to claim 5, wherein the products comprise paper diapers, facial masks, sanitary napkins, makeup-removing cottons, bedsheets, nursing films and wound repair materials.
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