CN116289203A - Preparation method of PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane - Google Patents
Preparation method of PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane Download PDFInfo
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- CN116289203A CN116289203A CN202310157253.9A CN202310157253A CN116289203A CN 116289203 A CN116289203 A CN 116289203A CN 202310157253 A CN202310157253 A CN 202310157253A CN 116289203 A CN116289203 A CN 116289203A
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Abstract
The invention belongs to the technical field of nanofiber membranes, and particularly relates to a preparation method of a PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane. The invention prepares PVA and PAA into spinning solution, adopts multi-unit electrostatic spinning and heat treatmentThe device is used for preparing the primary crosslinking PVA/PAA nanofiber membrane by a one-step method, and the primary crosslinking modification of the PVA nanofiber is realized by utilizing the condensation reaction between the hydroxyl of the PVA and the carboxyl of the PAA in the spinning and heat treatment processes. The Chinese herbal medicine has natural antibacterial active ingredients, and the active extract ingredients of the Chinese herbal medicine are combined with the PVA/PAA nanofiber membrane in a pad dyeing mode, so that antibacterial and antiviral properties of the nanofiber membrane can be endowed, and the primary crosslinking PVA/PAA nanofiber membrane can be subjected to secondary crosslinking by utilizing the active extract substances of the Chinese herbal medicine, so that the water stability of the PVA fiber is further improved. The nanofiber membrane provided by the invention has good air filtration performance and excellent antibacterial property, and is used for PM 0.3 Has a filtration rate of 97.3% for PM 1.0 And PM 2.5 The filtration rate of (C) was 100% and the air resistance was only 87Pa.
Description
Technical Field
The invention belongs to the technical field of nanofiber membranes, and particularly relates to a preparation method of a PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane.
Background
Clean air is the essential material basis for life, particulate Matter (PM) is an important index for measuring air quality, scientists PM2.5 indicate the content of the particulate matter in each cubic meter of air, the higher the PM2.5 value is, the more serious the air pollution is, and PM1 refers to the particulate matter with the kinetic diameter of less than or equal to 1 micron in the atmosphere, which is also called as lung-entering particulate matter. PM1 has small particle size, is rich in a large amount of toxic and harmful substances, has long residence time in the atmosphere and long conveying distance, and has larger influence on human health and atmospheric environment quality. PM is a serious threat to human health and may cause acute and chronic respiratory diseases. The PM pollution is removed, the viruses and harmful bacteria in the air also pose serious threat to the physical health of people, and the viruses are extremely easy to mutate and are almost impossible to completely kill due to the biological characteristics of the viruses. The harm of PM, bacteria, viruses and the like in the air to human bodies is blocked by the air filter, and the method becomes the key point of the current scientific research. The air filter covers a wide range of products, wherein the mask is the best choice for physical protection during daily travel of people because the mask can effectively resist ultrafine air particles carrying SARS-CoV-2.4 and other viruses, however, the secondary transmission of bacteria in the air filter is still harmful to human health.
The electrostatic spinning nanofiber membrane has the advantages of superfine diameter, large specific surface area, high porosity, strong electrostatic adsorption capacity and the like, and is widely applied to the field of air filtration. Under the action of the electric field, the polymer solution is stretched into fine jets and rapidly solidifies to form nanofibers. The current electrospun nanofiber material is easy to realize higher filtration efficiency, but is difficult to effectively reduce pressure drop due to the compact stacking characteristic. It is well known that the smaller the fiber diameter, the more advantageous is high performance air filtration. In addition, functional nanofiber membranes are also of great interest due to their better combination of properties. Among them, since the filter is easily contaminated with various pathogens, for example, it is reported that viruses can survive for more than 4 days in the inner layer and more than 7 days in the outer layer of a general surgical mask, bacterial pathogens can survive for 190 days on textile materials made of cotton, poly/cotton and polypropylene, which causes concern about the potential risk of secondary transmission through contact with contaminated respiratory masks. In particular, it is considered that the continuously exhaled air may cause a moist environment inside the mask, which may promote the propagation and growth of bacteria. Generally, different antibacterial and antiviral materials are mixed into the electrospinning solution, and the electrospinning nanofiber membrane with antibacterial performance can be obtained. However, the addition of antimicrobial agents tends to hinder the formation of charged droplets and the splitting of fibers, thereby affecting the spinning process, especially in large-scale industrial processes. At the same time, the expensive functional dopants, the use of large amounts of organic solvents and the complex solution stirring process also limit its large-scale application. Because of the above technical problems, development of an air filter with high efficiency, low resistance and strong antibacterial activity and a preparation method matched with the air filter for sustainable industrial production are needed.
In general, most polymers can be electrospun to produce high efficiency filter materials such as Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polystyrene (PS). However, a large amount of organic reagents are generally used in the preparation process, and organic solvents remain in the nanofibers to pose a threat to human health. The polyvinyl alcohol (PVA) has the advantages of low cost, good water solubility, no toxicity, good biocompatibility, good spinnability and good industrial application prospect. The nanofiber membrane cannot be used as a stable air filter in a high humidity environment due to the poor water resistance of the pure PVA nanofiber. Polyacrylic acid (PAA) has more polar functional groups, is soluble in water, has no toxicity and good biocompatibility. Can be mutually miscible with PVA at a certain temperature, and is easy to induce condensation reaction, so that the crosslinking degree and the water resistance of PVA are improved. Secondly, the PVA/PAA material can be further crosslinked by utilizing high-density hydrogen bonds between the PVA and the PAA and physical entanglement of polymer chains, and the surface of the composite PVA/PAA material still has rich non-composite hydroxyl and/or carboxylic acid groups, and can establish hydrogen bonds, coordination bonds and van der Waals interactions with the surfaces of other substances, so that the functionalization of the composite PVA/PAA material can be customized.
In order to realize the antibacterial performance of the air filter, the selection of a proper antibacterial preparation is important to ensure the non-toxicity and biocompatibility of the air filter. The antibacterial Chinese herbal medicine is a naturally occurring antibacterial substance, and refers to Chinese herbal medicine with obvious antibacterial or bactericidal effect, such as rhizoma coptidis, radix scutellariae, cortex phellodendri, flos lonicerae, herba houttuyniae, folium isatidis, radix isatidis, herba violae, rheum officinale, cortex fraxini, purslane, garlic, flos chrysanthemi indici, fructus forsythiae, dayflower, scandent hop, herba patriniae, selfheal, humifuse euphorbia herb, bottom of rotundifolia, dandelion, radix sophorae flavescentis, chinese pulsatilla and the like. The herbal medicines are decocted in folk application, and single or compound medicines are used for treating various infectious diseases, so that the clinical practice experience is abundant, and the toxicity and biocompatibility of the herbal medicines are verified. The rhizoma coptidis is a dried rhizome of rhizoma coptidis of Ranunculaceae, and is called rhizoma coptidis because the rhizome is in a form of beads and yellow, so the rhizoma coptidis is a clinically common antibacterial and antiviral traditional Chinese medicine. The coptis has a wide antibacterial spectrum, has a certain inhibition effect on gram-positive bacteria, gram-negative bacteria, various influenza viruses and fungi, and has a good antibacterial effect because the main component is isoquinoline alkaloid, wherein the berberine has a high content and is also called berberine. On the basis of the antibacterial substance, by which method it is effectively combined with the air filter and acts, it is also very important.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane, which is simple and efficient, and the prepared nanofiber membrane has excellent water stability, antibacterial and antiviral properties, and excellent mechanical properties and filtering properties.
The invention is realized by the following technical scheme:
the preparation method of the PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane comprises the following steps:
(1) Preparing spinning solution: adding PVA powder into deionized water at 80-100 ℃ for uniform mixing to obtain PVA solution, cooling to room temperature, adding PAA into the PVA solution for uniform mixing to obtain spinning solution;
(2) And (3) electrostatic spinning: carrying out electrostatic spinning on the spinning solution, and collecting nanofibers by using a receiving curtain to obtain a PVA/PAA nanofiber membrane;
(3) And (3) heat crosslinking treatment: carrying out heat treatment on the PVA/PAA nanofiber membrane to obtain a primary crosslinked PVA/PAA nanofiber membrane;
(4) Pad dyeing: the antibacterial traditional Chinese medicine modified solution is utilized to carry out three-soaking three-rolling process modification on the PVA/PAA nanofiber membrane subjected to primary crosslinking, the modified PVA/PAA nanofiber membrane is pre-dried, and then a baking machine is used for carrying out secondary heat crosslinking treatment, so that the water-stable antibacterial traditional Chinese medicine composite nanofiber membrane can be obtained.
Preferably, in the step (1), the concentration of the PVA solution is controlled to be 8-12wt%, and mechanical stirring is required for preparing the PVA solution for 5-10 hours;
the PAA is added in an amount of 20% to 100% by mass of PVA, preferably the PAA has a molecular weight of 800, and the PAA may be added in the form of a solution or powder, preferably a PAA solution having a concentration of 50% by weight is used.
Preferably, in the step (2), the receiving distance of the electrostatic spinning is 15-30cm, and the spinning voltage is 20-40kv; the electrostatic spinning process comprises a needle-containing, needleless or centrifugal electrostatic spinning process, wherein:
the needle electrostatic spinning process comprises the following steps: the inner diameter of the spinning needle is 0.33mm, the spinning voltage is 20-40kv, the injection speed is 0.3-1mL/h, the spinning time is 2-8h, the temperature is controlled to be 20-40 ℃, and the humidity is 30% -60%.
Preferably, in the step (3), the heat crosslinking treatment temperature is 100-180 ℃ and the time is 3-30min.
Preferably, in the step (4), the concentration of the antibacterial traditional Chinese medicine modified solution is 5-20wt%, and the antibacterial traditional Chinese medicine comprises berberine, curcumin or isochlorogenic acid;
the process of three-soaking and three-rolling comprises the following steps: at room temperature, the padding pressure is controlled to be 1-2kg/cm 2 The rotation speed of a roller is 2rpm, the antibacterial traditional Chinese medicine modifying solution is placed between two rollers, a padder is utilized to pad the fiber membrane, the fiber membrane is extruded and rolled through the two rollers three times in sequence, the antibacterial traditional Chinese medicine modifying solution is padded, and the nanofiber membrane is modified;
pre-drying: preventing berberine modified solution from 'migration', wherein the temperature is 60-80deg.C, and the time is 1-3min;
baking: the temperature is 100-180deg.C, and the time is 1-5min;
washing and drying: washing with deionized water for three times to remove unbound berberine in the fibrous membrane, and drying at 60deg.C in a forced air drying oven for 5min.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method is simple and efficient, and the nascent PVA/PAA nanofiber membrane with the fiber diameter of about 120-250 nanometers can be prepared by regulating and controlling spinning process parameters and the feeding ratio of PVA and PAA. Through a heat treatment process, the PVA/PAA nanofiber membrane with excellent water stability can be obtained, and through a water soaking experiment, the prepared PVA/PAA nanofiber membrane is free from obvious swelling and dissolution phenomena. Meanwhile, the solution system is suitable for various electrostatic spinning process technologies such as needle-free, needleless and centrifugal.
2. The nanofiber membrane provided by the invention has excellent antibacterial property, is nontoxic and high in biocompatibility, and is subjected to antibacterial modification post-treatment by using a berberine modified solution, but is not limited to berberine, and is also suitable for effective extracts of Chinese herbal medicines such as common andrographis herb, radix isatidis, baical skullcap root, honeysuckle, lightyellow sophora root and the like. The berberine belongs to a natural cationic dye with positive charges, the PVA/PAA nanofiber membrane is modified after being subjected to antibacterial action through a pad dyeing process of three padding and three padding, and the berberine is tightly combined on the surface of the PVA/PAA nanofiber by utilizing rich non-coordinated hydroxyl and/or carboxylic acid groups on the surface of the PVA/PAA fiber to carry out complex reaction with the berberine, so that the mutual integration optimization of covalent bond-hydrogen bond-Van der Waals acting force is realized, the crosslinking degree and the water stability of the nanofiber membrane are further improved, and the nanofiber membrane is endowed with excellent antibacterial property.
3. The nanofiber membrane has antibacterial and water stability, is free of organic solvent participation in the whole process, is suitable for the existing factory continuous process processing equipment, has a huge industrial application prospect, and has important application potential in the fields of antibacterial air filters, medical dressings, drug release and the like.
4. The traditional Chinese medicine composite nanofiber membrane prepared by the invention has good hydrophilicity, good moisture permeability and air permeability, and good mechanical property and filtering property, and the filtering efficiency of the coptis modified PVA/PAA nanofiber membrane can realize PM 0.3 Has a filtration rate of 97.3% for PM 1.0 The filtration rate of (C) is 100%, for PM 2.5 The filtration rate of (C) was 100%, and the resistance was only 87Pa.
Drawings
FIG. 1 is a scanning electron microscope image of a traditional Chinese medicine composite nanofiber membrane prepared in example 1;
FIG. 2 is a scanning electron microscope image of the traditional Chinese medicine composite nanofiber membrane prepared in example 1 after a soaking test;
FIG. 3 is a graph showing the results of the antibacterial test.
Detailed Description
To further illustrate the method and effect of the present invention, the present invention is further illustrated below with reference to examples. If specific conditions are not indicated in the examples, they are generally conventional conditions, or recommended by the reagent company; the reagents, consumables, etc. used in the following examples, except as specified, were commercially available, and berberine was purchased from the chemical technology of the front-end chemical Co., ltd.
Example 1
The preparation method of the PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane comprises the following steps:
(1) Preparing spinning solution: adding PVA powder into deionized water at 80 ℃ for uniform mixing, preparing PVA solution with the weight percent of 10%, cooling to room temperature, and adding PAA solution with the concentration of 50% by weight into the PVA solution for uniform mixing, wherein the mass percent of the PAA is 20% of the mass of the PVA, so as to obtain spinning solution;
(2) And (3) electrostatic spinning: spinning a PVA/PAA nanofiber membrane on a collector by using a needle electrostatic spinning technology, wherein the spinning voltage is set to be 20kV, the injection speed is set to be 0.3mL/h, the spinning time is 6h, the temperature is 30 ℃, and the humidity is 40%;
(3) And (3) heat treatment: placing the PVA/PAA nanofiber membrane into a blast drying oven for primary heat crosslinking treatment, wherein the temperature is 120 ℃ and the time is 10min, so as to obtain a primary crosslinked PVA/PAA nanofiber membrane;
(4) Pad dyeing: modifying the primarily crosslinked PVA/PAA nanofiber membrane by using berberine modified solution with the mass concentration of 10wt%, and pre-drying the modified PVA/PAA nanofiber membrane at the temperature of 60 ℃ for 3min; then a baking machine is used for carrying out secondary heat treatment, the temperature is set to be 100 ℃, the time is set to be 2min, deionized water is used for cleaning for three times, so as to remove unbound berberine in the fiber membrane, and the fiber membrane is dried in a blast drying box at 60 ℃ for 5min, thus obtaining the water-stable antibacterial traditional Chinese medicine composite nanofiber membrane, wherein:
the process of three-soaking and three-rolling comprises the following steps: at room temperature, the padding pressure is controlled to be 2kg/cm 2 The rotating speed of the roller is 2rpm, the berberine modified solution is placed between two rollers, padding treatment is carried out on the fiber membrane by using a padder, the fiber membrane is extruded and rolled by the two rollers three times in sequence, and the berberine modified solution is padded to modify the nanofiber membrane.
The prepared traditional Chinese medicine composite nanofiber membrane is subjected to ventilation rate of 2m by using a Topas filter material tester 2 And (3) carrying out a filtration performance test at/h, wherein the filtration efficiency is 93.7%, and the air resistance is only 143Pa.
Example 2
The preparation method of the PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane comprises the following steps:
(1) Preparing spinning solution: adding PVA powder into deionized water at 100 ℃ for uniform mixing, preparing PVA solution with the weight percent of 8%, cooling to room temperature, and adding PAA solution with the concentration of 50% by weight into the PVA solution for uniform mixing, wherein the mass percent of the PAA is 50% of the mass of the PVA, so as to obtain spinning solution;
(2) And (3) electrostatic spinning: spinning a PVA/PAA nanofiber membrane on a collector by using a needle electrostatic spinning technology, wherein the spinning voltage is set to be 40kV, the injection speed is set to be 0.3mL/h, the spinning time is 6h, the temperature is 30 ℃, and the humidity is 40%;
(3) And (3) heat treatment: placing the PVA/PAA nanofiber membrane into a blast drying oven for primary heat crosslinking treatment, wherein the temperature is 150 ℃ and the time is 30min, so as to obtain a primary crosslinked PVA/PAA nanofiber membrane;
(4) Pad dyeing: modifying the primarily crosslinked PVA/PAA nanofiber membrane by using berberine modification solution with the mass concentration of 10wt%, pre-drying the modified PVA/PAA nanofiber membrane at the pre-drying temperature of 60 ℃ for 3min, performing secondary heat treatment by using a baking machine, setting the temperature to 120 ℃ for 3min, cleaning the modified PVA/PAA nanofiber membrane with deionized water for three times to remove unbound berberine in the fiber membrane, and drying the modified PVA/PAA nanofiber membrane in a blast drying oven at the temperature of 60 ℃ for 5min to obtain the water-stable antibacterial traditional Chinese medicine composite nanofiber membrane, wherein:
the process of three-soaking and three-rolling comprises the following steps: at room temperature, the padding pressure is controlled to be 1kg/cm 2 The rotating speed of the roller is 2rpm, the berberine modified solution is placed between two rollers, padding treatment is carried out on the fiber membrane by using a padder, the fiber membrane is extruded and rolled by the two rollers three times in sequence, and the berberine modified solution is padded to modify the nanofiber membrane.
The prepared traditional Chinese medicine composite nanofiber membrane is subjected to ventilation rate of 2m by using a Topas filter material tester 2 And (3) carrying out a filtration performance test at/h, wherein the filtration efficiency is 97.3%, and the air resistance is only 87Pa.
Example 3
The preparation method of the PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane comprises the following steps:
(1) Preparing spinning solution: adding PVA powder into deionized water at 90 ℃ for uniform mixing, preparing PVA solution with the weight percent of 10%, cooling to room temperature, and adding PAA solution with the concentration of 50% by weight into the PVA solution for uniform mixing, wherein the mass percent of the PAA is 100% of the mass of the PVA, so as to obtain spinning solution;
(2) And (3) electrostatic spinning: spinning a PVA/PAA nanofiber membrane on a collector by using a needle electrostatic spinning technology, wherein the spinning voltage is set to be 30kV, the injection speed is set to be 0.5mL/h, the spinning time is 6h, the temperature is 30 ℃, and the humidity is 40%;
(3) And (3) heat treatment: placing the PVA/PAA nanofiber membrane into a blast drying oven for primary heat crosslinking treatment at 150 ℃ for 20min to obtain a primary crosslinked PVA/PAA nanofiber membrane;
(4) Pad dyeing: modifying the primarily crosslinked PVA/PAA nanofiber membrane by using berberine modification solution with the mass concentration of 8wt%, pre-drying the modified PVA/PAA nanofiber membrane at the pre-drying temperature of 60 ℃ for 3min, performing secondary heat treatment by using a baking machine, setting the temperature to 100 ℃ for 3min, cleaning the modified PVA/PAA nanofiber membrane with deionized water for three times to remove unbound berberine in the fiber membrane, and drying the modified PVA/PAA nanofiber membrane in a blast drying oven at the temperature of 60 ℃ for 5min to obtain the water-stable antibacterial traditional Chinese medicine composite nanofiber membrane, wherein:
the process of three-soaking and three-rolling comprises the following steps: at room temperature, the padding pressure is controlled to be 1kg/cm 2 The rotating speed of the roller is 2rpm, the berberine modified solution is placed between two rollers, padding treatment is carried out on the fiber membrane by using a padder, the fiber membrane is extruded and rolled by the two rollers three times in sequence, and the berberine modified solution is padded to modify the nanofiber membrane.
The prepared traditional Chinese medicine composite nanofiber membrane is subjected to ventilation rate of 2m by using a Topas filter material tester 2 And (3) carrying out a filtration performance test at/h, wherein the filtration efficiency is 91.3%, and the air resistance is only 123Pa.
The following test was performed with the traditional Chinese medicine composite nanofiber membrane of example 1:
(1) Observing the surface morphology of the prepared nanofiber membrane by using a scanning electron microscope, and representing the fiber diameter, wherein the fiber diameter is about 120-250nm as shown in figure 1;
(2) The prepared nanofiber membrane is subjected to water soaking treatment, and the water stability of the nanofiber membrane is tested, as shown in figure 2, the nanofiber membrane is found to have no obvious swelling and dissolution phenomena, and the water stability is good;
(3) The antibacterial tests are respectively carried out on the PVA/PAA nanofiber membrane before the modification of the coptis chinensis and the nanofiber membrane after the modification of the coptis chinensis, the results are shown in figure 3, the left graph is the PVA/PAA nanofiber membrane which is primarily crosslinked, the right graph is the nanofiber membrane after the modification of the coptis chinensis, the colony number of the right graph is obviously lower than that of the left graph, the antibacterial property is obviously improved, and the berberine can be proved to endow the nanofiber membrane with excellent antibacterial property.
Claims (10)
1. A preparation method of a PVA-based water-stable antibacterial traditional Chinese medicine composite nanofiber membrane is characterized by comprising the following steps of: the method comprises the following steps:
(1) Preparing spinning solution: adding PVA powder into deionized water at 80-100 ℃ for uniform mixing to obtain PVA solution, cooling to room temperature, adding PAA into the PVA solution for uniform mixing to obtain spinning solution;
(2) And (3) electrostatic spinning: carrying out electrostatic spinning on the spinning solution, and collecting nanofibers by using a receiving curtain to obtain a PVA/PAA nanofiber membrane;
(3) And (3) heat crosslinking treatment: carrying out heat treatment on the PVA/PAA nanofiber membrane to obtain a primary crosslinked PVA/PAA nanofiber membrane;
(4) Pad dyeing: the antibacterial traditional Chinese medicine modified solution is utilized to carry out three-soaking three-rolling process modification on the PVA/PAA nanofiber membrane subjected to primary crosslinking, the modified PVA/PAA nanofiber membrane is pre-dried, and then a baking machine is used for carrying out secondary heat crosslinking treatment, so that the water-stable antibacterial traditional Chinese medicine composite nanofiber membrane can be obtained.
2. The method of preparing a nanofiber membrane according to claim 1, wherein: the PVA solution concentration is 8-12wt%.
3. The method of preparing a nanofiber membrane according to claim 1, wherein: the PAA addition amount is 20% -100% of PVA mass, and the molecular weight of PAA is 800.
4. The method of preparing a nanofiber membrane according to claim 1, wherein: the receiving distance of electrostatic spinning is 15-30cm, and the spinning voltage is 20-40kv.
5. The method of preparing a nanofiber membrane according to claim 4, wherein: the electrostatic spinning process comprises needle-containing, needleless or centrifugal electrostatic spinning process.
6. The method of preparing a nanofiber membrane according to claim 5, wherein: the needle electrostatic spinning process comprises the following steps: the inner diameter of the spinning needle is 0.33mm, the spinning voltage is 20-40kv, the injection speed is 0.3-1mL/h, the spinning time is 2-8h, the temperature is controlled to be 20-40 ℃, and the humidity is 30% -60%.
7. The method of preparing a nanofiber membrane according to claim 1, wherein: the heat crosslinking treatment temperature is 100-180 ℃ and the time is 3-30min.
8. The method of preparing a nanofiber membrane according to claim 1, wherein: the concentration of the antibacterial traditional Chinese medicine modified solution is 5-20wt%.
9. The method of preparing a nanofiber membrane according to claim 8, wherein: the antibacterial traditional Chinese medicine comprises berberine, curcumin or isochlorogenic acid.
10. The method of preparing a nanofiber membrane according to claim 1, wherein: the pre-drying temperature is 60-80 ℃ and the pre-drying time is 1-3min; the secondary heat crosslinking treatment temperature is 100-180 ℃ and the time is 1-5min.
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