CN113368604B - Nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material and preparation method and application thereof - Google Patents
Nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material and preparation method and application thereof Download PDFInfo
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000835 fiber Substances 0.000 claims abstract description 36
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- 229910000271 hectorite Inorganic materials 0.000 claims abstract description 33
- 238000001914 filtration Methods 0.000 claims abstract description 26
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 25
- 229920005610 lignin Polymers 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 14
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000011148 porous material Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 42
- 239000011259 mixed solution Substances 0.000 claims description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- 239000003513 alkali Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 10
- 238000006722 reduction reaction Methods 0.000 claims description 10
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229940094522 laponite Drugs 0.000 claims description 8
- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 7
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- 230000002045 lasting effect Effects 0.000 abstract description 20
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- 229910021641 deionized water Inorganic materials 0.000 description 3
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 3
- 244000052616 bacterial pathogen Species 0.000 description 2
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- 231100000252 nontoxic Toxicity 0.000 description 2
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- 241000711573 Coronaviridae Species 0.000 description 1
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
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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
- B01D39/02—Loose filtering material, e.g. loose fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0028—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions provided with antibacterial or antifungal means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/30—Particle separators, e.g. dust precipitators, using loose filtering material
-
- 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
-
- 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
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
- Y02A50/2351—Atmospheric particulate matter [PM], e.g. carbon smoke microparticles, smog, aerosol particles, dust
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Filtering Materials (AREA)
Abstract
The invention discloses a nano-cellulose/glass fiber/immobilized nano-silver lasting antibacterial filter material, and a preparation method and application thereof. The method comprises the following steps: preparing an immobilized nano-silver composite antibacterial agent by using lignin as a reducing agent and hectorite as an immobilized template; the glass fiber is used as a filter material substrate, the nano cellulose and the oxidized nano cellulose are used as a flexible and aperture regulator and a dispersing agent, and are mixed with the immobilized nano silver antibacterial agent, and the filter material is obtained through suction filtration and freeze drying. The method has simple process and easy industrialization, and the obtained filter material has pore canal distribution with different hierarchical structures, higher porosity and relatively compact fiber stacking density. In the filter material, the release rate of the immobilized nano silver serving as the antibacterial agent is lower than 15 wt% in 30 days, and the antibacterial agent is slowly released to ensure the antibacterial durability of the filter material. When the material is applied to a filtering system, the constructed hierarchical pore structure has a hierarchical filtering effect, and the filtering efficiency of pollutants can be improved.
Description
Technical Field
The invention belongs to the field of filtration, and particularly relates to a nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material, and a preparation method and application thereof.
Background
In recent years, industrial production, automobile exhaust and a large amount of exhaust gas generated by daily combustion cause serious air pollution problems, and particularly, fine particles (PM2.5) with the diameter of less than 2.5 mu m enter the human body along with the respiratory system of the human body, thereby causing serious threats to human health. Although the traditional glass fiber filtering material can realize effective filtering of polluted particles, the pore structure of the filtering material formed by the traditional glass fiber filtering material is homogeneous, and the pressure resistance is higher when smaller particles are intercepted; and the glass fiber has poor mechanical property, is easy to be brittle, has poor wear resistance and is not beneficial to processing (Building and Environment, 2020, 183, 107182-.
The nano-cellulose is a flexible nano-material with negative charges, and can enhance the electronegativity of the surface of the glass fiber, improve the flexibility of the glass fiber filtering material and improve the mechanical property of the glass fiber filtering material. In addition, the unmodified nano-cellulose is insoluble in water, the TEMPO oxidized nano-cellulose has hydrophilicity, and a hierarchical micro-nano structure is designed by adjusting the ratio of two nano-celluloses with different characteristics, so that the effect of graded filtration can be achieved, and the aim of filtering air with high efficiency and low resistance is fulfilled.
However, pathogenic bacteria and viruses are often attached to air particles, the filter medium can prevent the air particles from entering a human body, but the pathogenic bacteria and the viruses remained in the filter material have the chance of invading and infecting people, and particularly, the current new coronavirus has a random outbreak all over the world, so that attention and requirements of people on antibacterial and antiviral properties are increased. Therefore, the air filtering material with long-acting sterilization and virus killing functions better meets the requirements of human health. The nano silver combines the dual advantages of the inorganic antibacterial material and the nano antibacterial material, is a broad-spectrum antibacterial agent and has no drug resistance. The antibacterial agent is added into the nano-cellulose/glass fiber filter material as an antibacterial agent, and can enhance the lasting antibacterial activity of the filter material. However, the binding force between the nano silver and the filter material substrate is weak, and the nano silver is easy to leak or release too much when being directly added. The hectorite is two-dimensional nano clay, the surface of which has negative charges and the edge of which has positive charges, and can be used as a bridge between nano silver and a fiber filter material base to fix the nano silver in the filter material base so as to achieve the effect of lasting antibiosis. In addition, the interweaving of the one-dimensional and two-dimensional nano materials is beneficial to the formation of the hierarchical structure of the filtering material, so that the filtering efficiency of the filtering material can be further promoted.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material, and a preparation method and application thereof.
The invention aims to provide a nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material aiming at the defects of the prior art, in particular to a nano-cellulose/glass fiber/immobilized nano-silver filter material which is nontoxic, has durable antibacterial activity, and can filter efficiently and precisely.
The invention also aims to provide a preparation method of the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material. The preparation method adopts lignin as a reducing agent and hectorite as an immobilized template to prepare the immobilized nano-silver composite antibacterial agent; then, the glass fiber is used as a filter material substrate, the nano-cellulose and the oxidized nano-cellulose are used as a flexible pore regulator and a dispersing agent, and are mixed with the immobilized nano-silver antibacterial agent, and the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material is prepared by suction filtration and freeze-drying. The nano-cellulose/glass fiber/immobilized nano-silver lasting antibacterial filter material is a nontoxic antibacterial filter material with lasting antibacterial activity.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of a nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material, which comprises the following steps:
(1) adding the silver ammonia solution into the hectorite solution under the stirring state, and uniformly mixing to obtain a hectorite-silver ammonia mixed solution;
(2) dropwise adding an alkali lignin solution into the hectorite-silver ammonia mixed solution obtained in the step (1) under a stirring state to obtain a reaction solution, and carrying out reduction reaction to obtain a hectorite immobilized nano silver compound (namely a hectorite immobilized nano silver compound antibacterial agent);
(3) dispersing glass fiber, nano cellulose and oxidized nano cellulose in deionized water, and performing ultrasonic dissociation until the dispersion is uniform to obtain a fiber mixed solution;
(4) and (3) uniformly mixing the fiber mixed solution in the step (3) and the hectorite immobilized nano-silver composite antibacterial agent in the step (2), filtering, taking a precipitate, and performing freeze-drying molding to obtain the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material.
Further, the concentration of the silver ammonia solution in the step (1) is 0.001-5 mol/L; the concentration of the hectorite (with the diameter of 25nm) solution is 0.1-12 g/L; the volume ratio of the silver ammonia solution to the hectorite solution is 1:1-1: 100.
Further, the concentration of the alkali lignin solution in the step (2) is 1-10 g/L; the addition amount of the alkali lignin solution accounts for 10-50% of the total volume of the reaction solution.
Further, the temperature of the reduction reaction in the step (2) is 50-90 ℃; the time of the reduction reaction is 30 to 120 minutes.
And (3) the alkali lignin solution in the step (2) is obtained by dissolving alkali lignin in deionized water.
Preferably, in the step (2), the laponite immobilized nano silver complex may be dialyzed with deionized water until no silver ion is detected.
Further, the diameter of the glass fiber in the step (3) is 0.5-10 μm; the diameter of the nano-cellulose is 0.5-3 μm; the diameter of the oxidized nano-cellulose is 0.1-1 μm, and the oxidation degree of the oxidized nano-cellulose is 0.7-1.2%; the mass of the nano-cellulose is 5-40% of that of the glass fiber; the mass of the oxidized nano-cellulose is 5-40% of the mass of the glass fiber. .
Preferably, the nanocellulose of step (3) has a fiber mean diameter of 1.5 μm.
Preferably, the oxidized nanocellulose obtained in step (3) has a fiber average diameter of 600nm and a degree of oxidation of 0.95%.
Further, in the fiber mixed solution in the step (3), the mass fraction of the glass fiber is 0.5-10%.
Further, the mass of the laponite immobilized nano-silver composite antibacterial agent in the step (4) is 0.1-5% of the mass of the glass fiber in the step (3).
The invention provides a nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material prepared by the preparation method. The material is a continuous three-dimensional net structure formed by cellulose, the average aperture of meshes is 0.05-2 mu m, the porosity is 80-99%, the filtering efficiency of the filtering material to particles with the particle size of 0.1-10 mu m is more than or equal to 95%, and the resistance pressure drop is 10-150 Pa; the release rate of the nano silver is lower than 15 wt% in 30 days.
The nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material provided by the invention can be applied to the preparation of air conditioner filter elements or air purifier filter element materials as an air filter material.
According to the preparation method provided by the invention, a novel nano-cellulose/glass fiber/immobilized nano-silver lasting antibacterial filter material is obtained by utilizing the insolubility of unmodified nano-cellulose and the enhancement effect of the insolubility of the unmodified nano-cellulose on the surface electronegativity of glass fibers, the hydrophilicity of TEMPO oxidized nano-cellulose and the surface and interface effects of hectorite nano-particles and glass fibers.
The material has the advantages of graded filtration, high precision, high air permeability, low resistance, long service life and the like, the problem of weak bonding strength between the nano-cellulose and the glass fiber is effectively solved by adding the oxidized nano-cellulose, and the mechanics of the glass fiber is improved; the immobilized nano silver is used as the antibacterial agent, so that the antibacterial effect is good, the range is wide, and the prepared filter material has stable and efficient antibacterial performance; the release rate of nano-silver is controlled by utilizing the adsorption and solidification effects of hectorite, the sterilization period of validity of the filter material is prolonged, and the application of the glass fiber in the field of filtration is expanded.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the preparation method provided by the invention, the adopted hectorite is nano-scale lamellar clay, and has the advantages of wide source, low cost, safety, no toxicity and stable performance;
(2) according to the preparation method provided by the invention, the nano-silver particles are fixed by utilizing the adsorption and immobilization effects of the hectorite, and when the nano-cellulose/glass fiber/immobilized nano-silver lasting antibacterial filter material prepared by mixing the nano-silver particles with the glass fiber, the nano-cellulose and the oxidized nano-cellulose is used for air filtration, the nano-silver particles with the antibacterial effect can be released in a small amount and continuously for a long time, so that the application of the nano-silver as an antibacterial agent in the field of filtration is expanded;
(3) according to the preparation method provided by the invention, the negative electricity of the surface of the glass fiber can be enhanced by taking the nano-cellulose as a flexible nano-material with negative charges, the nano-cellulose has hydrophobicity, the TEMPO oxidized nano-cellulose has hydrophilicity, a hierarchical micro-nano structure is designed by adjusting the proportion of the nano-cellulose with two characteristics, and the prepared filter material has the performances of graded filtration, high barrier and low resistance, so that the filtering target of high efficiency and low resistance to air is realized;
(4) the preparation method has simple process, wide raw material source and low energy consumption, and is beneficial to large-scale industrial production;
(5) the nano-cellulose/glass fiber/immobilized nano-silver lasting antibacterial filter material provided by the invention has the advantages that the release of nano-silver is less than 15 wt% in 30 days, the nano-silver lasting antibacterial effect is excellent, and the requirements of air filter materials can be effectively met.
Drawings
Fig. 1 is a graph of the cumulative release rate data for nanosilver from the nanocellulose/glass fibre/immobilized nanosilver filter material prepared in example 3.
Detailed Description
The following examples are included to further illustrate the practice of the invention, but are not intended to limit the practice or protection of the invention. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of a nano-cellulose glass fiber lasting antibacterial filter material comprises the following specific steps:
(1) preparing 0.1g/L hectorite (diameter 25nm) solution, adding 5mL of 0.001mol/L silver ammonia solution into 40mL of the hectorite solution under stirring, and uniformly mixing to obtain a hectorite-silver ammonia mixed solution;
(2) adding an alkali lignin solution with the concentration of 1g/L into the hectorite-silver ammonia mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume of the alkali lignin solution is 10% of the volume of the reaction solution, performing a reduction reaction at the reaction temperature of 50 ℃ for 30 minutes to obtain a hectorite immobilized nano-silver composite antibacterial agent for later use;
(3) dispersing glass fiber (fiber diameter is 0.5 μm), nano cellulose (fiber average diameter is 0.5 μm) and oxidized nano cellulose (fiber average diameter is 100nm, oxidation degree is 0.7%) in water, wherein the mass of the nano cellulose is 5% of that of the glass fiber; the mass of the oxidized nano-cellulose is 35% of the mass of the glass fiber; ultrasonically dissociating until the fiber is uniformly dispersed to obtain a fiber mixed solution; in the fiber mixed solution, the mass fraction of the glass fiber is 0.5%;
(4) and (4) adding 0.1% of hectorite immobilized nano silver composite antibacterial agent (relative to the mass fraction of the glass fiber) into the fiber mixed solution obtained in the step (3) under the stirring state, uniformly mixing, performing suction filtration, and performing freeze-drying to obtain the nano cellulose/glass fiber/immobilized nano silver lasting antibacterial filter material.
In the nano-cellulose/glass fiber/immobilized nano-silver filter material prepared in example 1, the hectorite and the fiber have good immobilization efficiency on double immobilization of nano-silver, so that the nano-silver can be slowly and continuously released to achieve a lasting antibacterial effect, as shown in fig. 1.
Example 2
A preparation method of a nano-cellulose glass fiber lasting antibacterial filter material comprises the following specific steps:
(1) preparing 1g/L hectorite (diameter 25nm) solution, adding 5mL of 0.1mol/L silver ammonia solution into 40mL of the hectorite solution under stirring, and uniformly mixing to obtain a hectorite-silver ammonia mixed solution;
(2) adding an alkali lignin solution with the concentration of 2g/L into the hectorite-silver ammonia mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume of the alkali lignin solution is 10% of the volume of the reaction solution, performing a reduction reaction at the reaction temperature of 60 ℃ for 60 minutes to obtain a hectorite immobilized nano-silver composite antibacterial agent for later use;
(3) dispersing glass fiber (fiber diameter is 1 μm), nano-cellulose (fiber average diameter is 0.8 μm) and oxidized nano-cellulose (fiber average diameter is 500nm, oxidation degree is 0.8%) in water, wherein the mass of the nano-cellulose is 10% of that of the glass fiber; the mass of the oxidized nano-cellulose is 30% of that of the glass fiber; ultrasonically dissociating until the fiber is uniformly dispersed to obtain a fiber mixed solution; in the fiber mixed solution, the mass fraction of the glass fiber is 1 percent;
(4) and (3) adding 1% of laponite immobilized nano-silver composite antibacterial agent (relative to the mass fraction of the glass fiber) into the fiber mixed solution obtained in the step (3) under the stirring state, uniformly mixing, performing suction filtration, and freeze-drying to obtain the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material.
In the nano-cellulose/glass fiber/immobilized nano-silver filter material prepared in example 2, the laponite and the fiber have good immobilization efficiency for double immobilization of nano-silver, so that the nano-silver can be slowly and continuously released to achieve a lasting antibacterial effect, as shown in fig. 1.
Example 3
The preparation method of the nano-cellulose glass fiber lasting antibacterial filter material comprises the following specific steps:
(1) preparing a hectorite (diameter 25nm) solution with the concentration of 6g/L, adding 5mL of a silver-ammonia solution with the concentration of 1mol/L into 40mL of the hectorite solution under stirring, and uniformly mixing to obtain a hectorite-silver-ammonia mixed solution;
(2) adding an alkali lignin solution with the concentration of 5g/L into the hectorite-silver ammonia mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume of the alkali lignin solution is 10% of the volume of the reaction solution, performing a reduction reaction at the reaction temperature of 80 ℃ for 90 minutes to obtain a hectorite immobilized nano-silver composite antibacterial agent for later use;
(3) dispersing glass fiber (fiber diameter is 5 μm), nano-cellulose (fiber average diameter is 1.5 μm) and oxidized nano-cellulose (fiber average diameter is 800nm, oxidation degree is 0.95%) in water, wherein the mass of the nano-cellulose is 20% of that of the glass fiber; the mass of the oxidized nano-cellulose is 20% of that of the glass fiber; ultrasonically dissociating until the fiber is uniformly dispersed to obtain a fiber mixed solution; in the fiber mixed solution, the mass fraction of the glass fiber is 5 percent;
(4) and (4) adding 2.5% of hectorite immobilized nano silver composite antibacterial agent (relative to the mass fraction of the glass fiber) into the fiber mixed solution obtained in the step (3) under the stirring state, uniformly mixing, performing suction filtration, and freeze-drying to obtain the nano cellulose/glass fiber/immobilized nano silver lasting antibacterial filter material.
The graph of the cumulative release rate of the nano-silver in the nano-cellulose/glass fiber/immobilized nano-silver filter material prepared in example 3 is shown in fig. 1, and it can be seen from fig. 1 that the release rate of the nano-silver in the nano-cellulose/glass fiber/immobilized nano-silver filter material is low, and the cumulative release rate in 30 days is only 14.43%, which indicates that the double immobilization of the laponite and the fiber on the nano-silver has a good immobilization efficiency, so that the nano-silver is slowly and continuously released, and a lasting antibacterial effect is achieved.
Example 4
A preparation method of a nano-cellulose glass fiber lasting antibacterial filter material comprises the following specific steps:
(1) preparing a hectorite (diameter is 25nm) solution with the concentration of 12g/L, adding 5mL of a silver ammonia solution with the concentration of 5mol/L into 40mL of the hectorite solution under stirring, and uniformly mixing to obtain a hectorite-silver ammonia mixed solution;
(2) adding an alkali lignin solution with the concentration of 10g/L into the hectorite-silver ammonia mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume of the alkali lignin solution is 10% of the volume of the reaction solution, carrying out reduction reaction at the reaction temperature of 90 ℃ for 120 minutes to obtain a hectorite immobilized nano-silver composite antibacterial agent for later use;
(3) dispersing glass fiber (fiber diameter is 10 μm), nano-cellulose (fiber average diameter is 3 μm) and oxidized nano-cellulose (fiber average diameter is 1 μm, oxidation degree is 1.2%) in water, wherein the mass of the nano-cellulose is 40% of that of the glass fiber; the mass of the oxidized nano-cellulose is 40% of that of the glass fiber; ultrasonically dissociating until the fiber is uniformly dispersed to obtain a fiber mixed solution; in the fiber mixed solution, the mass fraction of the glass fiber is 10 percent;
(4) and (3) adding 5% of laponite immobilized nano-silver composite antibacterial agent (relative to the mass fraction of the glass fiber) into the fiber mixed solution obtained in the step (3) under the stirring state, uniformly mixing, performing suction filtration, and freeze-drying to obtain the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material.
In the nano-cellulose/glass fiber/immobilized nano-silver filter material prepared in example 4, the laponite and the fiber have good immobilization efficiency for double immobilization of nano-silver, so that the nano-silver can be slowly and continuously released to achieve a lasting antibacterial effect, as shown in fig. 1.
The above examples are only preferred embodiments of the present invention, which are intended to illustrate the present invention, but not to limit the present invention, and those skilled in the art should be able to make changes, substitutions, modifications, etc. without departing from the spirit of the present invention.
Claims (10)
1. A preparation method of a nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material is characterized by comprising the following steps:
(1) adding the silver ammonia solution into the hectorite solution under the stirring state, and uniformly mixing to obtain a hectorite-silver ammonia mixed solution;
(2) dropwise adding an alkali lignin solution into the hectorite-silver ammonia mixed solution obtained in the step (1) under a stirring state to obtain a reaction solution, and carrying out reduction reaction to obtain a hectorite immobilized nano-silver composite antibacterial agent;
(3) dispersing glass fiber, unmodified nano-cellulose and oxidized nano-cellulose in water, and performing ultrasonic dissociation until the dispersion is uniform to obtain a fiber mixed solution;
(4) and (3) uniformly mixing the fiber mixed solution in the step (3) and the hectorite immobilized nano-silver composite antibacterial agent in the step (2), filtering, taking a precipitate, and performing freeze-drying molding to obtain the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material.
2. The preparation method of the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material according to claim 1, wherein the concentration of the silver ammonia solution in the step (1) is 0.001-5 mol/L; the concentration of the hectorite solution is 0.1-12 g/L; the volume ratio of the silver ammonia solution to the hectorite solution is 1:1-1: 100.
3. The preparation method of the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material according to claim 1, wherein the concentration of the alkali lignin solution in the step (2) is 1-10 g/L; the addition amount of the alkali lignin solution accounts for 10-50% of the total volume of the reaction solution.
4. The preparation method of the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material according to claim 1, wherein the temperature of the reduction reaction in the step (2) is 50-90 ℃; the time of the reduction reaction is 30 to 120 minutes.
5. The method for preparing the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material according to claim 1, wherein the diameter of the glass fiber in step (3) is 0.5-10 μm; the diameter of the unmodified nano-cellulose is 0.5-3 μm; the diameter of the oxidized nano-cellulose is 0.1-1 μm.
6. The preparation method of the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material according to claim 1, wherein the oxidation degree of the oxidized nano-cellulose is 0.7-1.2%; the mass of the unmodified nano-cellulose is 0.1-20% of that of the glass fiber; the mass of the oxidized nano-cellulose is 0.1-20% of the mass of the glass fiber.
7. The method for preparing the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material according to claim 1, wherein in the fiber mixed solution in the step (3), the mass fraction of the glass fiber is 0.5-10%.
8. The preparation method of the nano-cellulose/glass fiber/immobilized nano-silver durable antibacterial filter material according to claim 1, wherein the mass of the laponite immobilized nano-silver composite antibacterial agent in the step (4) is 0.1-5% of the mass of the glass fiber in the step (3).
9. A nano cellulose/glass fiber/immobilized nano silver durable antibacterial filter material prepared by the preparation method of any one of claims 1 to 8, wherein the material is a continuous three-dimensional network structure formed by cellulose, the average pore diameter of a mesh is 0.05 to 2 μm, the porosity is 80 to 99 percent, the filter efficiency of the filter material to particles with the particle size of 0.1 to 10 μm is more than or equal to 95 percent, and the resistance pressure drop is 10 to 150 Pa; the release rate of the nano silver is lower than 15 wt% in 30 days.
10. Use of the nanocellulose/glass fibre/immobilized nanosilver permanent antibacterial filter material of claim 9 in the preparation of air conditioner filter elements or air purifier filter element materials.
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| PCT/CN2021/097568 WO2022222232A1 (en) | 2021-04-23 | 2021-06-01 | Nano-cellulose/glass fiber/immobilized nano-silver durable anti-microbial filter material, preparation method therefor and use thereof |
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| CN103769604A (en) * | 2014-01-25 | 2014-05-07 | 华南理工大学 | Green and quick method for preparing lignin-nanosilver sol |
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| DE102007009619A1 (en) * | 2007-02-26 | 2008-08-28 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Antimicrobial textile glass fiber material, includes nanoparticulate silver in base coating, adhesive layer and antimicrobial coating |
| CN107189110A (en) * | 2017-06-23 | 2017-09-22 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of nano-cellulose reinforcing glass composite fiber membrane and preparation method thereof |
| CN107574719A (en) * | 2017-09-21 | 2018-01-12 | 成都新柯力化工科技有限公司 | A kind of antibacterial glass fibre air purification filter paper and preparation method thereof |
| CN108166322A (en) * | 2017-12-28 | 2018-06-15 | 许飞扬 | A kind of high-strength abrasion-proof high-temperature resistant antibacterial filter paper and preparation method thereof |
| CN108951106B (en) * | 2018-06-13 | 2021-02-26 | 浙江工业大学之江学院 | Antibacterial nanofiber and preparation method thereof |
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| CN103769604A (en) * | 2014-01-25 | 2014-05-07 | 华南理工大学 | Green and quick method for preparing lignin-nanosilver sol |
| CN108102152A (en) * | 2017-12-14 | 2018-06-01 | 华南理工大学 | A kind of food packaging hectorite immobilization nano silver/chitosan anti-bacteria composite membrane and preparation method and application |
| CN112516685A (en) * | 2020-11-17 | 2021-03-19 | 华东师范大学重庆研究院 | Visible light photocatalysis air purification glass fiber filter element and preparation method thereof |
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