CN113398661A - Novel ZIF-8 nano mask inner core and preparation method thereof - Google Patents

Novel ZIF-8 nano mask inner core and preparation method thereof Download PDF

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Publication number
CN113398661A
CN113398661A CN202110613670.0A CN202110613670A CN113398661A CN 113398661 A CN113398661 A CN 113398661A CN 202110613670 A CN202110613670 A CN 202110613670A CN 113398661 A CN113398661 A CN 113398661A
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zif
inner core
preparation
drying
mask
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CN113398661B (en
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朱丽英
沈博文
王鑫龙
江凌
赵倩如
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Nanjing Tech University
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Nanjing Tech University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • A—HUMAN NECESSITIES
    • A41—WEARING APPAREL
    • A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
    • A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
    • A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
    • A—HUMAN NECESSITIES
    • A41—WEARING APPAREL
    • A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D31/00—Materials specially adapted for outerwear
    • A41D31/04—Materials specially adapted for outerwear characterised by special function or use
    • A41D31/30—Antimicrobial, e.g. antibacterial
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10—Filtering material manufacturing
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention relates to a novel ZIF-8 nano mask inner core and a preparation method thereof, wherein the preparation method comprises the following steps: soaking the non-woven fabric in a polydopamine aqueous solution for 12-13h, and then cleaning and drying; and then soaking the mixture in a polyvinyl alcohol aqueous solution dispersed with ZIF-8 nano particles, stirring for 5-6 h, and then cleaning and drying to obtain the zinc oxide. The novel ZIF-8 nanometer mask inner core can effectively prevent bacteria with aerogel from contacting and spreading, and the ZIF-8 nanometer material can effectively kill the bacteria. The preparation method disclosed by the invention is environment-friendly, low in cost and high in commercial value.

Description

Novel ZIF-8 nano mask inner core and preparation method thereof
Technical Field
The invention belongs to the field of air filtration, and particularly relates to a formula of a novel ZIF-8 nano mask inner core and a preparation method thereof.
Background
Because the disposable gauze mask that the impact of new crown epidemic situation brought is not enough in supply, the function of original gauze mask probably can not satisfy people's daily demand, and the waste of resource is also very easily brought in a large amount of gauze mask supplies. Therefore, it is imperative to improve the sustainable utility and antibacterial protection of masks.
Disclosure of Invention
The invention aims to provide a novel ZIF-8 nano mask inner core, which is formed by loading polydopamine, polyvinyl alcohol and ZIF-8 on non-woven fabrics, can improve the antibacterial effect of a mask, and can enable the mask to have the recycling capability. The poly-dopamine is adopted, so that the antibacterial capacity of the mask inner core can be improved, and the non-woven fabric is easy to load other materials due to easy functionalization of the poly-dopamine. The added polyvinyl alcohol improves the hydrophobicity of the mask inner core, and the viscosity of the polyvinyl alcohol can better adhere the ZIF-8 material to the non-woven fabric fibers. ZIF-8 is a high-efficiency antibacterial material, and the addition of ZIF-8 can greatly improve the antibacterial ability of the nano mask inner core. Compared with patent CN 111974090A, ZIF-8 nanometer mask provides stronger antibacterial ability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a novel ZIF-8 nanometer mask inner core comprises the following steps:
(1) soaking the non-woven fabric in a polydopamine aqueous solution for 12-13h, and then cleaning and drying;
(2) and (2) soaking the non-woven fabric obtained in the step (1) in a polyvinyl alcohol aqueous solution dispersed with ZIF-8 nano particles, stirring for 5-6 h, and then cleaning and drying to obtain the zinc oxide/.
The antibacterial ability of the nano mask inner core can be improved by adding the polydopamine, the surface of the polydopamine is easy to functionalize, and the polydopamine coating on the surface of the non-woven fabric is beneficial to subsequent loading of other materials. In addition, polydopamine also has better biocompatibility.
The added polyvinyl alcohol can improve the hydrophobicity of the nano mask inner core, and in addition, the polyvinyl alcohol has higher viscosity, so that the nano material can be more tightly adhered to the non-woven fabric fiber.
Preferably, the ZIF-8 nanoparticles are obtained by the following method:
(0) and (3) sealing and stirring zinc ions and 2-methylimidazole in the solution for 12-13h, and then separating out solids to obtain the zinc-manganese-zinc composite material.
Preferably, the solvent of the solution in step (0) is methanol.
Preferably, the molar ratio of the zinc ions to the 2-methylimidazole in the step (0) is 1: 8-9.
Preferably, the separation in step (0) is separation by centrifugation. Preferably, the rotating speed of the centrifuge is 9000-10000 rpm, and the temperature of the centrifuge is 25-30 ℃.
Preferably, step (0) further comprises a step of drying the separated solid. The drying is carried out for 24-25h at the temperature of 50-70 ℃.
Preferably, the concentration of the aqueous solution of polydopamine in the step (1) is 1-1.2 mg/mL.
Preferably, the cleaning in step (1) is cleaning with ethanol.
Preferably, the drying in the step (1) is natural drying at 25-30 ℃.
Preferably, the concentration of the ZIF-8 nanoparticles in the aqueous solution in the step (2) is 1-1.2 mg/mL, and the concentration of the polyvinyl alcohol is 1-1.2 mg/mL.
Preferably, the washing in the step (2) is washing with ethanol.
Preferably, the drying in the step (2) is natural drying at 25-30 ℃.
The invention also provides the mask inner core prepared by the method.
According to the invention, the non-woven fabric is used as a raw material, and the ZIF-8 nano material with high-efficiency antibacterial effect is loaded on the non-woven fabric to prepare the nano mask inner core, so that the nano mask inner core has higher hydrophobicity, the probability of contact with bacteria is reduced, and better antibacterial capability is achieved.
The invention has the beneficial effects that:
the novel ZIF-8 nanometer mask inner core prepared by the invention is used as an inner core arranged in the mask middle layer, has strong hydrophobicity, reduces the probability of bacteria penetrating through the mask, has strong sterilization effect, and further improves the service life and the reuse rate of the mask. The preparation method is green and environment-friendly, the raw material cost is low, the sustainable utilization of resources is improved, the production quality of the mask is improved, and the practical performance of the mask is promoted.
Drawings
Fig. 1 is a scanning electron microscope image of the core of the non-woven mask of example 1 and the core of the novel ZIF-8 nano mask. Wherein A is the image of the inner core of the common non-woven fabric mask, and B is the image of the inner core of the novel ZIF-8 nanometer mask.
FIG. 2 is a schematic contact angle of the novel ZIF-8 nano-mask core and the control core of example 1. Wherein A is the contact angle of the control inner core and the water drop, and B is the contact angle of the novel ZIF-8 nano mask inner core and the control inner core and the water drop.
FIG. 3 is a graph showing the results of repeated antibacterial experiments on the inner core of the novel ZIF-8 nano mask in example 1.
Fig. 4 is a graph showing the result of the biocompatibility test between the inner core of the novel ZIF-8 nano mask and human fibroblasts in example 1.
Detailed Description
Example 1
(1) Soaking the non-woven fabric in a polydopamine aqueous solution for 12 hours, then cleaning the non-woven fabric with ethanol, and naturally drying the non-woven fabric at 25-30 ℃; the concentration of the aqueous solution of polydopamine was 1 mg/mL.
(2) Preparing ZIF-8 nanoparticles: and (2) hermetically stirring zinc ions and 2-methylimidazole in methanol for 13 hours, wherein the molar ratio of the zinc ions to the 2-methylimidazole is 1: 8. And then, separating out solid, namely ZIF-8 nano particles, by adopting a centrifugal machine at the rotating speed of 9000 rpm. Then drying for 25h at 50 ℃.
(3) And (2) soaking the non-woven fabric obtained in the step (1) in a polyvinyl alcohol aqueous solution in which ZIF-8 nano particles are dispersed, stirring for 6 hours, cleaning with ethanol, and naturally drying at 25-30 ℃ to obtain the novel ZIF-8 nano mask inner core. The concentration of ZIF-8 nanoparticles was 1.2mg/mL and the concentration of polyvinyl alcohol was 1 mg/mL.
And (2) soaking the non-woven fabric obtained in the step (1) in water dispersed with ZIF-8 nano particles, stirring for 6 hours, cleaning with ethanol, and naturally drying at 25-30 ℃ to obtain the control inner core.
(4) Respectively placing the common non-woven fabric mask inner core and the novel ZIF-8 nanometer mask inner core on a copper seat conducting gel special for a scanning electron microscope, and treating by using a metal spraying instrument. The results of observation using a scanning electron microscope are shown in FIG. 1.
Fig. 1A is an image of a common non-woven fabric mask inner core, fig. 1B is an image of a novel ZIF-8 nano mask inner core, it can be seen that a ZIF-8 nano material is well attached to non-woven fabric fibers, and the image result of a scanning electron microscope proves the successful preparation of the novel ZIF-8 nano mask inner core.
(5) Respectively cutting the inner core of the novel ZIF-8 nano mask and the comparison inner core into small pieces, placing on a contact angle measuring instrument placing table, and paving.
And (3) respectively contacting water drops with the surfaces of the novel ZIF-8 nano mask inner core and the control inner core by using a syringe, wherein the volume of each water drop is 20-21 mu L. The contact angles of the water drop and the new ZIF-8 nano mask inner core and the control inner core were measured using a contact angle measuring instrument, and the results are shown in fig. 2.
FIG. 2A shows the contact angle of the control core with a water droplet, at an angle of 77-80 °; FIG. 2B is a graph showing the contact angles of the inner core and the control inner core of the novel ZIF-8 nano mask with water drops at an angle of 105-108 degrees. The contact angles of the novel ZIF-8 nano mask inner core and the comparison inner core to water are improved, which shows that the hydrophobicity of the novel ZIF-8 nano mask inner core and the comparison inner core is improved, bacteria are transmitted in the air in the form of aerogel, and the possibility of the bacteria contacting with a human body is reduced.
(6) Culturing Escherichia coli as experimental strain, preparing LB liquid culture medium to culture Escherichia coli, inoculating Escherichia coli into LB liquid culture medium, culturing for 12-13h to obtain Escherichia coli in stationary phase, and determining that Escherichia coli is about 1-1.1 × 10^9 CFU.
Cutting the inner core of the novel ZIF-8 nano mask to 0.2-0.25 pi cm3Coli was diluted to 1-1.1X 10^5 CFU. The novel ZIF-8 nano mask inner core and an escherichia coli diluted solution are cultured together for 3 hours and then inoculated on an LB solid culture medium. After culturing for 12-13h, observing and counting the colony number of the LB solid culture medium.
The preparation method of the LB liquid culture medium comprises the steps of adding 10-11g of sodium chloride, 10-11g of peptone and 5-5.5g of yeast powder into 1-1.1L of sterile water. Then placing the mixture into a sterilization pot for sterilization for 30-35min at the temperature of 120 ℃ and 121 ℃. The preparation method of the LB solid culture medium comprises the steps of adding 10-11g of sodium chloride, 10-11g of peptone, 5-5.5g of yeast powder and 20-21g of agar powder into 1-1.1L of sterile water. Then placing the mixture into a sterilization pot for sterilization for 30-35min at the temperature of 120 ℃ and 121 ℃. Then the mixture is transferred to a biological culture dish to be cooled while the mixture is hot.
The antibacterial effect is shown in fig. 3, the antibacterial effect of the inner core of the novel ZIF-8 nano mask repeatedly used in the water solution is maintained at 100% after 5 times of repeated use, and the antibacterial effect is reduced after 6 times of repeated use, but still maintained at a high antibacterial level.
(7) Human skin fibroblasts were cultured as a sample, and the frozen cells were inoculated into DMEM-H medium containing 10% bovine serum.
Culturing at 37-38 deg.C in 5% carbon dioxide for 24-25 hr to make cells grow adherently.
Cells were then washed with trypsin to allow the cells to slough off the wall. The cell solution was seeded onto 96-well plates using a density of 5000 cells/well and then cultured for an additional 24-25 h.
Adding novel ZIF-8 nano mask inner cores with different concentrations into the cell solution, and measuring the survival rate of the cells after 24-25 h.
The results are shown in FIG. 4, where the cells involved are human skin fibroblasts. Human skin fibroblast survival rate decreased slightly with increasing concentration. The human skin fibroblast survival rate was about 80% when the concentration was increased to 200. mu.g/ml.
As can be seen, the novel ZIF-8 nanometer mask inner core has good biocompatibility and can not cause harm to human bodies.
Example 2
(1) Soaking the non-woven fabric in a polydopamine aqueous solution for 13h, then cleaning with ethanol, and naturally drying at 25-30 ℃; the concentration of the aqueous solution of polydopamine was 1.2 mg/mL.
(2) Preparing ZIF-8 nanoparticles: and (2) hermetically stirring zinc ions and 2-methylimidazole in methanol for 12 hours, wherein the molar ratio of the zinc ions to the 2-methylimidazole is 1: 9. And then, separating out solid by adopting a centrifugal machine at the rotating speed of 10000rpm, namely the ZIF-8 nano particles. Then drying for 24h at 70 ℃.
(3) And (2) soaking the non-woven fabric obtained in the step (1) in a polyvinyl alcohol aqueous solution in which ZIF-8 nano particles are dispersed, stirring for 5 hours, cleaning with ethanol, and naturally drying at 25-30 ℃ to obtain the novel ZIF-8 nano mask inner core. The concentration of ZIF-8 nanoparticles was 1mg/mL and the concentration of polyvinyl alcohol was 1.2 mg/mL.

Claims (10)

1. A preparation method of a novel ZIF-8 nanometer mask inner core is characterized by comprising the following steps:
(1) soaking the non-woven fabric in a polydopamine aqueous solution for 12-13h, and then cleaning and drying;
(2) and (2) soaking the non-woven fabric obtained in the step (1) in a polyvinyl alcohol aqueous solution dispersed with ZIF-8 nano particles, stirring for 5-6 h, and then cleaning and drying to obtain the zinc oxide/.
2. The preparation method according to claim 1, wherein the ZIF-8 nanoparticles are obtained by a method comprising:
(0) and (3) sealing and stirring zinc ions and 2-methylimidazole in the solution for 12-13h, and then separating out solids to obtain the zinc-manganese-zinc composite material.
3. The method according to claim 2, wherein the solvent of the solution in the step (0) is methanol.
4. The method according to claim 2, wherein the molar ratio of zinc ions to 2-methylimidazole in the step (0) is 1:8 to 9.
5. The method according to claim 2, wherein the separation in the step (0) is a separation by centrifugation.
6. The method according to claim 5, wherein the rotation speed of the centrifuge is 9000 to 10000rpm, and the temperature of the centrifuge is 25 to 30 ℃.
7. The preparation method according to claim 2, wherein the step (0) further comprises a step of drying the separated solid, wherein the drying is drying at 50-70 ℃ for 24-25 h.
8. The preparation method according to claim 1, wherein the concentration of the aqueous solution of polydopamine in step (1) is 1-1.2 mg/mL.
9. The preparation method according to claim 1, wherein the concentration of the ZIF-8 nanoparticles in the aqueous solution in the step (2) is 1 to 1.2mg/mL, and the concentration of the polyvinyl alcohol is 1 to 1.2 mg/mL.
10. A mask core produced by the method of any one of claims 1 to 9.
CN202110613670.0A 2021-06-02 2021-06-02 ZIF-8 nano mask inner core and preparation method thereof Active CN113398661B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104051691A (en) * 2014-06-06 2014-09-17 中国第一汽车股份有限公司 Preparation method of polydopamine-based modified composite polymer diaphragm
CN106178999A (en) * 2016-07-08 2016-12-07 山东大学 A kind of preparation method of LBL self-assembly metallic organic framework composite membrane
CN109577005A (en) * 2018-11-28 2019-04-05 吉林大学 A kind of preparation method and applications of the ZIF-8 functionalized nano-fiber film of poly-dopamine modification
CN110777537A (en) * 2019-11-04 2020-02-11 北京理工大学 ZIF-8/non-woven fabric composite material and preparation method thereof
CN111905816A (en) * 2020-07-08 2020-11-10 武汉纺织大学 ZIF-8 functional fabric and preparation method thereof
US20200406248A1 (en) * 2019-06-26 2020-12-31 Xergy Inc. Anionic membranes incorporating functional additives
WO2021066742A1 (en) * 2019-09-30 2021-04-08 National University Of Singapore Polycrystalline metal-organic framework membranes for separation of mixtures

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104051691A (en) * 2014-06-06 2014-09-17 中国第一汽车股份有限公司 Preparation method of polydopamine-based modified composite polymer diaphragm
CN106178999A (en) * 2016-07-08 2016-12-07 山东大学 A kind of preparation method of LBL self-assembly metallic organic framework composite membrane
CN109577005A (en) * 2018-11-28 2019-04-05 吉林大学 A kind of preparation method and applications of the ZIF-8 functionalized nano-fiber film of poly-dopamine modification
US20200406248A1 (en) * 2019-06-26 2020-12-31 Xergy Inc. Anionic membranes incorporating functional additives
WO2021066742A1 (en) * 2019-09-30 2021-04-08 National University Of Singapore Polycrystalline metal-organic framework membranes for separation of mixtures
CN110777537A (en) * 2019-11-04 2020-02-11 北京理工大学 ZIF-8/non-woven fabric composite material and preparation method thereof
CN111905816A (en) * 2020-07-08 2020-11-10 武汉纺织大学 ZIF-8 functional fabric and preparation method thereof

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