CN117504440A - Antibacterial PP synthetic cotton fiber filter material and application thereof - Google Patents
Antibacterial PP synthetic cotton fiber filter material and application thereof Download PDFInfo
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- CN117504440A CN117504440A CN202311471200.0A CN202311471200A CN117504440A CN 117504440 A CN117504440 A CN 117504440A CN 202311471200 A CN202311471200 A CN 202311471200A CN 117504440 A CN117504440 A CN 117504440A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 58
- 239000000463 material Substances 0.000 title claims abstract description 48
- 229920000742 Cotton Polymers 0.000 title claims abstract description 40
- 239000004743 Polypropylene Substances 0.000 claims abstract description 80
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 44
- -1 polypropylene Polymers 0.000 claims abstract description 40
- 229920001155 polypropylene Polymers 0.000 claims abstract description 40
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 18
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000967 suction filtration Methods 0.000 claims abstract description 11
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 10
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims abstract description 10
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims abstract description 10
- 239000011976 maleic acid Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001125 extrusion Methods 0.000 claims abstract description 5
- 238000002074 melt spinning Methods 0.000 claims abstract description 5
- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 claims description 23
- 229960003500 triclosan Drugs 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 19
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- HFBMWMNUJJDEQZ-UHFFFAOYSA-N acryloyl chloride Chemical compound ClC(=O)C=C HFBMWMNUJJDEQZ-UHFFFAOYSA-N 0.000 claims description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 8
- 230000003472 neutralizing effect Effects 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 5
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 5
- 230000000241 respiratory effect Effects 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000005457 ice water Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000009987 spinning Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 13
- 230000000694 effects Effects 0.000 description 9
- 230000029058 respiratory gaseous exchange Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 4
- 210000002345 respiratory system Anatomy 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
- 239000005543 nano-size silicon particle Substances 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000005653 Brownian motion process Effects 0.000 description 2
- 235000005775 Setaria Nutrition 0.000 description 2
- 241000232088 Setaria <nematode> Species 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000005537 brownian motion Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 244000179970 Monarda didyma Species 0.000 description 1
- 235000010672 Monarda didyma Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011738 major mineral Substances 0.000 description 1
- 235000011963 major mineral Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2055—Carbonaceous material
-
- 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
-
- 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
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2027—Metallic material
-
- 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
- B01D46/0001—Making filtering elements
-
- 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
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
Abstract
The invention discloses an antibacterial PP synthetic cotton fiber filter material, which comprises the following steps: (1) Adding sodium carbonate, nano graphene and nano titanium dioxide into the aqueous solution of nitric acid, performing ultrasonic dispersion, continuously adding nano diatomite, stirring for 4-6 hours at 70-75 ℃, performing suction filtration, and performing vacuum drying to obtain a composite nano filler; (2) Dissolving polypropylene in diethyl ether, adding an organic antibacterial agent, glycidyl methacrylate, maleic acid and tert-butyl peroxide, uniformly mixing, reacting for 1-2h at 85-87 ℃, and carrying out suction filtration, washing and drying to obtain modified polypropylene; (3) Uniformly mixing the composite nano filler, the inorganic antibacterial agent, the modified polypropylene and the polypropylene, adding the mixture into a screw extruder for melt extrusion, and using electrostatic spinning equipment for melt spinning to obtain the antibacterial PP synthetic cotton fiber filter material. The antibacterial PP synthetic cotton fiber filter material prepared by the invention has good antibacterial effect and high breaking strength.
Description
Technical Field
The invention belongs to the technical field of medical instruments, and particularly relates to an antibacterial PP synthetic cotton fiber filter material and application thereof.
Background
Pathogenic microorganisms in the respiratory tract mainly take water as a carrier, a filter medium (a filter membrane) in a respiratory system filter can be made of polypropylene composite materials and the like, the hydrophobic performance is good, the pore diameter is small, pressure difference exists between a machine port of the respiratory system filter and two ends of a patient port, and filter pores in the filter medium can filter particles in gas, prevent bacteria and viruses suspended in air from passing through and accept water vapor, but not allow liquid water to pass through.
The filtering principle of the respiratory system filter mainly comprises interception effect, inertia effect, diffusion effect and electrostatic effect. Interception effect: when larger particles move to the surface of the fiber along the streamline, the larger particles are intercepted by the mechanical screening action of the filter material and deposited, and the principle is shown in figure 1; inertial effect: when the mass of the particles is large or the speed is large, and the particles are separated from the streamline due to the inertia effect and impact on the surface of the filter material when the streamline turns, the principle is shown in figure 2 because the adsorption force stays on the impact surface; diffusion effect: the principle of the Brownian motion of the particles generated by the collision of the gas molecular thermal motion on the particles is shown in fig. 3, wherein the Brownian motion of the particles is diffused and displaced into the filter fiber to be adsorbed, and the smaller the particles are, the more remarkable the particles are; electrostatic adsorption effect: the particles are adsorbed and deposited by the electrostatic action of the filter material, the principle of which is shown in fig. 4.
The disposable respiratory filter consists of an upper cover 1, a lower cover 3, a filter material 2 and a mouthpiece 4. The mouthpiece is used for maintaining the opening state of a patient during oral surgery or examination, preventing unexpected occlusion, and is matched with a filter for use. The filtering material of the existing disposable breathing filter is mainly PP cotton, and is made of polypropylene fibers for artificial chemical fibers, but the antibacterial performance of the existing polypropylene material cannot meet long-time use requirements.
Disclosure of Invention
The invention aims to provide an antibacterial PP synthetic cotton fiber filter material which has good antibacterial effect, can prolong antibacterial time and is suitable for being used as a filter material of a disposable breathing filter.
In order to achieve the above object, the present invention provides the following technical solutions:
the preparation method of the antibacterial PP synthetic cotton fiber filter material comprises the following steps of:
(1) Adding sodium carbonate, nano graphene and nano titanium dioxide into 3-5wt% of aqueous solution of nitric acid, performing ultrasonic dispersion for 15-20min at 55-60 ℃, continuously adding nano diatomite, stirring for 4-6h at 70-75 ℃, performing suction filtration, and performing vacuum drying to obtain composite nano filler;
(2) Dissolving polypropylene in diethyl ether, continuously adding an organic antibacterial agent, glycidyl methacrylate, maleic acid and tert-butyl peroxide, uniformly mixing, reacting for 1-2h at 85-87 ℃, pouring the product into acetone for precipitation, and obtaining modified polypropylene after suction filtration, washing and drying;
(3) Adding 5-8 parts by weight of composite nano filler, 1-2 parts by weight of inorganic antibacterial agent, 15-20 parts by weight of modified polypropylene and 80-90 parts by weight of polypropylene into a high-speed mixer, uniformly mixing, adding into a screw extruder for melt extrusion, and then using an electrostatic spinning device for melt spinning to obtain the antibacterial PP synthetic cotton fiber filter material.
Further, the preparation method of the organic antibacterial agent comprises the following steps: dissolving triclosan in a carbon tetrachloride solution, adding 98wt% of concentrated sulfuric acid, reacting for 4-6 hours at 4-5 ℃, separating, purifying and neutralizing to obtain triclosan sulfonate; dissolving triclosan sulfonate in water, adding acryloyl chloride, reacting in ice-water bath for 2-4 h, and neutralizing with sodium hydroxide to neutrality.
Further, the inorganic antibacterial agent is a nano silver antibacterial agent. Purchased from bergamot science and technology limited, model: nano silver antibacterial agent KEPUYIN-J67. The invention uses nano silver antibacterial agent, organic antibacterial agent and polypropylene to cooperate with the antibacterial effect best.
Further, the polypropylene was purchased from Shanghai bridge micro chemical technology Co., ltd, medical grade PP GM1600E.
The filter material of the disposable respiratory filter has reduced antibacterial property after contacting water molecules for a long time in the actual use process. According to the invention, the modified polypropylene grafted with the organic antibacterial agent is compounded with the polypropylene, and the inorganic antibacterial agent is added, so that the prepared antibacterial PP synthetic cotton fiber filter material has excellent water molecule resistance, and the condition that the antibacterial property of the existing filter material is reduced after long-time use is improved. According to the invention, the organic antibacterial agent and the inorganic antibacterial agent act on polypropylene, the organic antibacterial agent is grafted with the polypropylene, and then the organic antibacterial agent is compounded with the inorganic antibacterial agent and the unmodified polypropylene, so that the antibacterial effect is remarkably improved through a series of treatments, and particularly, the problem that the antibacterial property of the filter material is reduced due to the influence of water molecules after long-term use is solved, so that the disposable breathing filter can maintain good antibacterial effect for a long time.
Further, the volume ratio of triclosan to carbon tetrachloride solution is 1: (5-8).
Further, the molar ratio of triclosan to concentrated sulfuric acid is 1: (1.2-1.4).
Further, the molar ratio of triclosan sulfonate to acryloyl chloride is 1: (2-3).
Further, the mass ratio of the organic antibacterial agent, polypropylene, glycidyl methacrylate, maleic acid and benzoyl peroxide in the step (2) is (0.1-0.2): 1: (1.2-1.5): (2.4-2.6): (0.3-0.5).
Further, the molar ratio of sodium carbonate to ferric nitrate is (0.6-0.8): 1, a step of; the mass ratio of the sodium carbonate to the nano graphene to the nano titanium dioxide to the nano diatomite is 1: (4-6): (1-3): (17-23).
Further, the specific surface area of the nano graphene is 200-300m 2 And/g, purchased from Qianfeng nanometer.
Further, the particle size of the nano titanium dioxide: 20-40nm; specific surface area: 77.37m 2 /g。
Further, the average grain diameter of the nano diatomite is 8-13 mu m, the silicon dioxide is more than or equal to 89.2wt%, the aluminum oxide is less than or equal to 3.8wt%, and the ferric oxide is less than or equal to 1.45wt%. Purchased from Qingdao Setaria silicon industries, inc.
On the premise of improving the antibacterial property, the antibacterial PP synthetic cotton fiber filter material has better fracture resistance when being used as a filter material of a disposable breathing filter. The system of the invention is added with the composite nano filler, thereby improving the breaking strength of the antibacterial PP synthetic cotton fiber filter material. The hypothesis is that the composite nano filler optimizes the interaction force of the polymer molecular interface, so that the breaking strength of the antibacterial PP synthetic cotton fiber filter material is improved. The inventors have also unexpectedly found that when nano graphene, nano titanium dioxide and nano kieselguhr of a specific surface area and particle size are used to be compounded in a specific ratio, the composite nano filler can improve the antibacterial performance of the antibacterial PP synthetic cotton fiber filter material. It is hypothesized that the composite nano-filler improves the dispersion performance of the system, so that the organic antibacterial agent and the inorganic antibacterial agent can better exert the synergistic effect with polypropylene.
Further, the voltage range of the electrostatic spinning equipment is 15-25KV, the syringe injection rate is 2-4mL/h, and the heating temperature of the spinning solution is kept at 100-200 ℃.
Further, the thickness of the antibacterial PP synthetic cotton fiber filter material is 1-3mm.
The invention also provides application of the antibacterial PP synthetic cotton fiber filter material in preparation of a disposable breathing filter.
Compared with the prior art, the invention has the advantages that:
1. the antibacterial PP synthetic cotton fiber filter material provided by the invention has a good antibacterial effect, can prolong antibacterial time, can maintain excellent breaking strength, and is very suitable for being used as a filter material of a disposable breathing filter.
2. According to the invention, the modified polypropylene grafted with the organic antibacterial agent is compounded with the polypropylene, and the inorganic antibacterial agent is added, so that the prepared antibacterial PP synthetic cotton fiber filter material has excellent water washing resistance, and the condition that the antibacterial property of the existing filter material is reduced after long-time use is improved.
3. The system of the invention is added with the composite nano filler, thereby improving the breaking strength of the antibacterial PP synthetic cotton fiber filter material. The inventors have also unexpectedly found that when nano graphene, nano titanium dioxide and nano kieselguhr of specific surface area and particle size are used, the composite nano filler improves the antibacterial performance of the antibacterial PP synthetic cotton fiber filter material.
Drawings
FIG. 1 is a schematic diagram of direct interception;
FIG. 2 is a schematic view of an inertial collision;
FIG. 3 is a diffusion interception schematic;
FIG. 4 is a schematic illustration of electrostatic adsorption;
fig. 5 is a schematic view of the structure of a single-use respiratory filter.
In the figure, 1, an upper cover, 2, a filter material, 3, a lower cover, 4, a mouthpiece, D, an outer diameter, L and a height.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides an antibacterial PP synthetic cotton fiber filter material, and the preparation method of the antibacterial PP synthetic cotton fiber filter material comprises the following steps:
(1) Adding sodium carbonate, nano graphene and nano titanium dioxide into 4wt% of aqueous solution of nitric acid, performing ultrasonic dispersion for 17min at 57 ℃, continuously adding nano diatomite, stirring for 5h at 72 ℃, performing suction filtration, and performing vacuum drying to obtain composite nano filler;
(2) Dissolving polypropylene in diethyl ether, continuously adding an organic antibacterial agent, glycidyl methacrylate, maleic acid and tert-butyl peroxide, uniformly mixing, reacting for 1.5 hours at 86 ℃, pouring the product into acetone for precipitation, and obtaining modified polypropylene after suction filtration, washing and drying;
(3) Adding 6 parts by weight of composite nano filler, 1.5 parts by weight of inorganic antibacterial agent, 17 parts by weight of modified polypropylene and 85 parts by weight of polypropylene into a high-speed mixer, uniformly mixing, adding into a screw extruder for melt extrusion, and then using an electrostatic spinning device for melt spinning to obtain the antibacterial PP synthetic cotton fiber filter material.
The preparation method of the organic antibacterial agent comprises the following steps: dissolving triclosan in a carbon tetrachloride solution, adding 98wt% of concentrated sulfuric acid, reacting for 5 hours at 5 ℃, separating and purifying, and neutralizing to obtain triclosan sulfonate; dissolving triclosan sulfonate in water, adding acryloyl chloride, reacting for 3h in ice water bath, and neutralizing with sodium hydroxide to neutrality.
The inorganic antibacterial agent is a nano silver antibacterial agent.
Volume ratio of triclosan to carbon tetrachloride solution 1:7.
the molar ratio of triclosan to concentrated sulfuric acid is 1:1.3.
the molar ratio of triclosan sulfonate to acryloyl chloride is 1:2.6.
the mass ratio of the organic antibacterial agent to the polypropylene to the glycidyl methacrylate to the maleic acid to the benzoyl peroxide in the step (2) is 0.12:1:1.4:2.5:0.4.
the molar ratio of sodium carbonate to ferric nitrate is 0.7:1, a step of; the mass ratio of the sodium carbonate to the nano graphene to the nano titanium dioxide to the nano diatomite is 1:5:2:18.
the specific surface area of the nano graphene is 200-300m 2 /g。
Particle size of the nano titanium dioxide: 20-40nm; specific surface area: 77.37m 2 /g。
The average grain diameter of the nano diatomite is 8-13 mu m, the silicon dioxide is more than or equal to 89.2wt%, the aluminum oxide is less than or equal to 3.8wt%, and the ferric oxide is less than or equal to 1.45wt%.
The voltage range of the electrostatic spinning equipment is 20KV, the syringe injection rate is 3mL/h, and the heating temperature of the spinning solution is kept at 160 ℃.
The thickness of the antibacterial PP synthetic cotton fiber filter material is 2mm.
Example 2
The embodiment provides an antibacterial PP synthetic cotton fiber filter material, and the preparation method of the antibacterial PP synthetic cotton fiber filter material comprises the following steps:
(1) Adding sodium carbonate, nano graphene and nano titanium dioxide into 3wt% of aqueous solution of nitric acid, performing ultrasonic dispersion for 17min at 55 ℃, continuously adding nano diatomite, stirring for 5h at 72 ℃, performing suction filtration, and performing vacuum drying to obtain composite nano filler;
(2) Dissolving polypropylene in diethyl ether, continuously adding an organic antibacterial agent, glycidyl methacrylate, maleic acid and tert-butyl peroxide, uniformly mixing, reacting for 1.5 hours at 86 ℃, pouring the product into acetone for precipitation, and obtaining modified polypropylene after suction filtration, washing and drying;
(3) Adding 8 parts by weight of composite nano filler, 2 parts by weight of inorganic antibacterial agent, 15 parts by weight of modified polypropylene and 90 parts by weight of polypropylene into a high-speed mixer, uniformly mixing, adding into a screw extruder for melt extrusion, and then using an electrostatic spinning device for melt spinning to obtain the antibacterial PP synthetic cotton fiber filter material.
The preparation method of the organic antibacterial agent comprises the following steps: dissolving triclosan in a carbon tetrachloride solution, adding 98wt% of concentrated sulfuric acid, reacting for 5 hours at 5 ℃, separating and purifying, and neutralizing to obtain triclosan sulfonate; dissolving triclosan sulfonate in water, adding acryloyl chloride, reacting for 3h in ice water bath, and neutralizing with sodium hydroxide to neutrality.
The inorganic antibacterial agent is a nano silver antibacterial agent.
Volume ratio of triclosan to carbon tetrachloride solution 1:5.
the molar ratio of triclosan to concentrated sulfuric acid is 1:1.2.
the molar ratio of triclosan sulfonate to acryloyl chloride is 1:3.
the mass ratio of the organic antibacterial agent to the polypropylene to the glycidyl methacrylate to the maleic acid to the benzoyl peroxide in the step (2) is 0.1:1:1.5:2.4:0.5.
the molar ratio of sodium carbonate to ferric nitrate is 0.6:1, a step of; the mass ratio of the sodium carbonate to the nano graphene to the nano titanium dioxide to the nano diatomite is 1:4:3:20.
the specific surface area of the nano graphene is 200-300m 2 /g。
Particle size of the nano titanium dioxide: 20-40nm; specific surface area: 77.37m 2 /g。
The average grain diameter of the nano diatomite is 8-13 mu m, the silicon dioxide is more than or equal to 89.2wt%, the aluminum oxide is less than or equal to 3.8wt%, and the ferric oxide is less than or equal to 1.45wt%.
The voltage range of the electrostatic spinning equipment is 20KV, the syringe injection rate is 3mL/h, and the heating temperature of the spinning solution is kept at 160 ℃.
Comparative example 1
The difference between this comparative example and example 1 is: the preparation method of the composite nano filler comprises the following steps: adding sodium carbonate, nano graphene and nano silicon carbide into 4wt% of aqueous solution of nitric acid, performing ultrasonic dispersion for 20min at 56 ℃, continuously adding nano kaolin, stirring for 5h at 72 ℃, performing suction filtration, and performing vacuum drying to obtain the composite nano filler. The mass ratio of the sodium carbonate to the nano graphene to the nano silicon carbide to the nano diatomite is 1:3:5:18. the nano silicon carbide is purchased from Zhejiang Zhi titanium nano micro new material Co., ltd, and the particle size is 50nm. The nanokaolin was 3.25 microns and was purchased from stone house major mineral products limited.
Comparative example 2
The difference between this comparative example and example 1 is: the specific surface area of the nano graphene is 50-100m 2 And/g, purchased from Qianfeng nanometer. Particle size of the nano titanium dioxide: 70-90nm; specific surface area: 52.14m 2 And/g. Purchased from qinfeng nano. The average grain diameter of the nano diatomite is 15-18 mu m, the silicon dioxide is more than or equal to 87.5wt percent, and the oxide is threeLess than or equal to 3.8wt% of aluminum and less than or equal to 1.45wt% of ferric oxide. Purchased from Qingdao Setaria silicon industries, inc. The mass ratio of the sodium carbonate to the nano graphene to the nano titanium dioxide to the nano diatomite is 1:2:5:18.
comparative example 3
The difference between this comparative example and example 1 is: 3 parts by weight of a composite nanofiller, 4 parts by weight of an inorganic antibacterial agent, 30 parts by weight of a modified polypropylene and 70 parts by weight of polypropylene were added to a high-speed mixer.
Comparative example 4
The difference between this comparative example and example 1 is: the inorganic antibacterial agent is zinc oxide.
Comparative example 5
The difference between this comparative example and example 1 is: the mass ratio of the organic antibacterial agent to the polypropylene to the glycidyl methacrylate to the maleic acid to the benzoyl peroxide in the step (2) is 0.25:1:1.1:2.3:0.25.
performance testing
Referring to GB/T20944.2-2007, the antibacterial rates of the products of examples and comparative examples were determined; the products of examples and comparative examples were washed with water 50 times and then the antibacterial rate was measured. The breaking strength of the products of examples and comparative examples was determined with reference to T24218.3-2010. The control group was Ningbo Hua Kun filter material in a disposable respiratory filter from medical instruments limited.
TABLE 1 antibacterial efficiency measurement results (%)
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the antibacterial PP synthetic cotton fiber filter material is characterized by comprising the following steps of:
(1) Adding sodium carbonate, nano graphene and nano titanium dioxide into 3-5wt% of aqueous solution of nitric acid, performing ultrasonic dispersion for 15-20min at 55-60 ℃, continuously adding nano diatomite, stirring for 4-6h at 70-75 ℃, performing suction filtration, and performing vacuum drying to obtain composite nano filler;
(2) Dissolving polypropylene in diethyl ether, continuously adding an organic antibacterial agent, glycidyl methacrylate, maleic acid and tert-butyl peroxide, uniformly mixing, reacting for 1-2h at 85-87 ℃, pouring the product into acetone for precipitation, and obtaining modified polypropylene after suction filtration, washing and drying;
(3) Adding 5-8 parts by weight of composite nano filler, 1-2 parts by weight of inorganic antibacterial agent, 15-20 parts by weight of modified polypropylene and 80-90 parts by weight of polypropylene into a high-speed mixer, uniformly mixing, adding into a screw extruder for melt extrusion, and then using electrostatic spinning equipment for melt spinning to obtain the antibacterial PP synthetic cotton fiber filter material.
2. The antibacterial PP synthetic cotton fiber filter medium of claim 1, wherein the organic antibacterial agent is prepared by the following steps: dissolving triclosan in a carbon tetrachloride solution, adding 98wt% of concentrated sulfuric acid, reacting for 4-6 hours at 4-5 ℃, separating, purifying and neutralizing to obtain triclosan sulfonate; dissolving triclosan sulfonate in water, adding acryloyl chloride, reacting in ice-water bath for 2-4 h, and neutralizing with sodium hydroxide to neutrality to obtain the organic antibacterial agent.
3. The antibacterial PP synthetic cotton fiber filter medium of claim 1, wherein the inorganic antibacterial agent is a nano silver antibacterial agent.
4. The antibacterial PP synthetic cotton fiber filter medium of claim 2, wherein the molar ratio of triclosan to concentrated sulfuric acid is 1: (1.2-1.4).
5. The antibacterial PP synthetic cotton fiber filter medium of claim 2, wherein the molar ratio of triclosan sulfonate to acryloyl chloride is 1: (2-3).
6. The antibacterial PP synthetic cotton fiber filter medium of claim 1, wherein the mass ratio of the organic antibacterial agent, polypropylene, glycidyl methacrylate, maleic acid and benzoyl peroxide in the step (2) is (0.1-0.2): 1: (1.2-1.5): (2.4-2.6): (0.3-0.5).
7. The antibacterial PP synthetic cotton fiber filter medium of claim 1, wherein the molar ratio of sodium carbonate to ferric nitrate is (0.6-0.8): 1, a step of; the mass ratio of the sodium carbonate to the nano graphene to the nano titanium dioxide to the nano diatomite is 1: (4-6): (1-3): (17-23).
8. The antibacterial PP synthetic cotton fiber filter material of claim 7, wherein the specific surface area of the nano graphene is 200-300m 2 /g; the particle size of the nano titanium dioxide is 20-40nm; specific surface area of 77.37m 2 /g; the average grain diameter of the nano diatomite is 8-13 mu m, the silicon dioxide is more than or equal to 89.2wt%, the aluminum oxide is less than or equal to 3.8wt%, and the ferric oxide is less than or equal to 1.45wt%.
9. The antibacterial PP synthetic cotton fiber filter material of claim 1, wherein the voltage range of the electrostatic spinning equipment is 15-25KV, the syringe injection rate is 2-4mL/h, and the heating temperature of the spinning solution is kept at 100-200 ℃.
10. The use of an antibacterial PP synthetic cotton fiber filter material as claimed in any one of claims 1 to 9, characterized in that the antibacterial PP synthetic cotton fiber filter material is used for the preparation of a disposable respiratory filter.
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| CN109293838A (en) * | 2018-08-31 | 2019-02-01 | 汕头市远生实业有限公司 | A kind of novel graft antibacterial polypropylene and its preparation process |
| CN112127049A (en) * | 2020-09-30 | 2020-12-25 | 安徽灵春医用耗材有限公司 | Preparation method of polypropylene melt-blown non-woven fabric material for mask |
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| WO2017206442A1 (en) * | 2016-06-02 | 2017-12-07 | 江苏盛纺纳米材料科技股份有限公司 | Melt-blown composite nanometer antibacterial super-soft nonwoven material and preparation method |
| CN106435055A (en) * | 2016-10-25 | 2017-02-22 | 齐鲁工业大学 | Antibacterial retanning agent and preparation method thereof |
| CN109293838A (en) * | 2018-08-31 | 2019-02-01 | 汕头市远生实业有限公司 | A kind of novel graft antibacterial polypropylene and its preparation process |
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