CN113598193B - Light nano antibacterial material and preparation method and application thereof - Google Patents
Light nano antibacterial material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 31
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002657 fibrous material Substances 0.000 claims abstract description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000002114 nanocomposite Substances 0.000 claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000003385 bacteriostatic effect Effects 0.000 claims abstract description 15
- 239000004202 carbamide Substances 0.000 claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 12
- 239000004642 Polyimide Substances 0.000 claims abstract description 11
- 229920001721 polyimide Polymers 0.000 claims abstract description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 10
- RTFMGYRAUWLAJG-UHFFFAOYSA-N dimethoxy-methyl-prop-2-enoxysilane Chemical compound CO[Si](C)(OC)OCC=C RTFMGYRAUWLAJG-UHFFFAOYSA-N 0.000 claims abstract description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 claims 1
- 239000008399 tap water Substances 0.000 abstract description 18
- 235000020679 tap water Nutrition 0.000 abstract description 18
- 239000002086 nanomaterial Substances 0.000 abstract description 17
- 241000282414 Homo sapiens Species 0.000 abstract description 5
- 230000036541 health Effects 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- -1 acyloxy propyl trimethoxy silane Chemical compound 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 10
- 230000003287 optical effect Effects 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 235000020188 drinking water Nutrition 0.000 description 3
- 239000003651 drinking water Substances 0.000 description 3
- 239000002384 drinking water standard Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 2
- 241000607142 Salmonella Species 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 206010005003 Bladder cancer Diseases 0.000 description 1
- 208000015634 Rectal Neoplasms Diseases 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 208000007097 Urinary Bladder Neoplasms Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 206010038038 rectal cancer Diseases 0.000 description 1
- 201000001275 rectum cancer Diseases 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical compound CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 description 1
- 201000005112 urinary bladder cancer Diseases 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- General Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Zoology (AREA)
- Water Supply & Treatment (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Agronomy & Crop Science (AREA)
- Environmental Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Toxicology (AREA)
- Inorganic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a light nano antibacterial material and a preparation method and application thereof, belonging to the technical field of nano materials. The preparation method specifically comprises the following steps: reacting the product obtained by the reaction of titanium sulfate, KOH and urea with polyimide fiber in NaOH solution to obtain TiO2Nanocomposite fiber material, then adding the TiO2The nano composite fiber material reacts with gamma-methacrylic acid acyloxy propyl trimethoxy silane and vinyl methyl trimethoxy silane in an organic solvent to obtain modified TiO2Nano composite fiber material in AgNO3Soaking in the solution to obtain the light nano antibacterial material. The prepared light nano bacteriostatic material can be used for tap water bacteriostatic treatment, has an excellent bacteriostatic effect, does not have the problem of heavy metal exceeding, and can meet the requirement of human health.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a light nano antibacterial material and a preparation method and application thereof.
Background
Ensuring the safety and sanitation of water quality is one of the most challenging problems facing human beings at present. At present, the traditional method for treating municipal tap water is a chlorination method, chlorine is easily dissolved in water and is combined with the water to generate hypochlorous acid and hydrochloric acid, the method has the characteristics of convenience in use, low cost and the like, and the chlorine can be remained in the water (residual chlorine), so that the effects of continuous sterilization and disinfection are achieved. However, the use of chlorination processes produces many by-products with long-term deleterious effects, including trihalomethanes and haloacetic acids, among others, and epidemiological studies have shown that bladder cancer, rectal cancer, and the like may be associated with drinking water containing such by-products.
Nanotechnology has wide application in environmental science, and provides new materials, processes and technical support for environmental science. Nanotechnology has shown great superiority and potential application value in pollutant monitoring and water treatment, and compared with traditional environment detection and water treatment method, it has incomparable advantages.
At present, the development of nano antibacterial materials is continuously carried out, but the problems of excessive heavy metals, inapplicability to drinking water systems, incapability of being well applied to terminal water and the like still exist when the existing nano antibacterial materials are applied to water body bacteriostasis, so that the technical problem to be solved at present is to provide a nano material which has an excellent antibacterial effect and is applicable to tap water bacteriostasis.
Disclosure of Invention
The invention aims to provide a light nano bacteriostatic material, a preparation method and application thereof, which are used for solving the problems in the prior art so as to realize safe and efficient bacteriostatic action on tap water.
In order to achieve the purpose, the invention provides the following scheme:
one of the purposes of the invention is to provide a preparation method of a light nano antibacterial material, which comprises the following steps:
(1) dissolving titanium sulfate in a KOH solution, then adding urea, and reacting to obtain a product A;
(2) reacting the product A with polyimide fibers in NaOH solution to obtain TiO2A nanocomposite fiber material;
(3) subjecting the TiO to a reaction2Adding the nano composite fiber material, gamma-methacryloxypropyltrimethoxysilane and vinyl methyltrimethoxysilane into an organic solvent, carrying out ultrasonic treatment, and reacting at 73-75 ℃ for 2-3h to obtain modified TiO2A nanocomposite fiber material;
(4) subjecting the modified TiO to2Nano composite fiber material in AgNO3Soaking in the solution to obtain the light nano antibacterial material.
Further, the molar ratio of the urea to the titanium sulfate is 1: 1; the reaction conditions after urea addition were: reacting for 45-48h at 180-185 ℃.
Further, the mass ratio of the product A to the polyimide fiber is 1-1.2: 5.
Further, the concentration of the NaOH solution is 10-12 mol/L.
Further, the reaction temperature in the step (2) is 182-185 ℃, and the reaction time is 20-24 h.
Further, the TiO2The mass ratio of the nano composite fiber material to the gamma-methacryloxypropyltrimethoxysilane and the vinyl methyltrimethoxysilane is 10:1.8-2: 3-3.4.
Further, the time of the ultrasonic treatment in the step (3) is 0.3-0.5 h.
Further, the AgNO3The concentration of the solution is 1-1.2 mol/L; the soaking time in the step (4) is 30-45 min.
The invention also aims to provide the optical nano antibacterial material obtained by the preparation method.
The invention also aims to provide the application of the light nano antibacterial material in water treatment bacteriostasis.
Further, the water treatment bacteriostasis is tap water treatment bacteriostasis.
The invention discloses the following technical effects:
the invention uses polyimide fiber as a framework, and TiO generated in the reaction process2The fiber and the polyimide fiber framework form physical crosslinking, so that an extremely rich fiber structure is formed, and the fiber has a huge specific surface area; and then, gamma-methacryloxypropyltrimethoxysilane (KH-570) and vinyl methyltrimethoxysilane are used for modifying the material in the presence of a solvent, so that the light bacteriostasis performance of the final product is greatly improved.
The material can be directly compounded with the silver solution after being modified, the current situation that silver is prepared into silver nanoparticles firstly and then a fiber composite material is prepared in the prior art is improved, the prepared optical nano antibacterial material can be used for tap water antibacterial treatment, has an excellent antibacterial effect, does not have the problem that heavy metal exceeds the standard, meets the regulation of national drinking water standard GB5749-2006, and can meet the requirement of human health.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
A light nano material for tap water bacteriostasis is prepared by the following steps:
(1) dissolving 4g of titanium sulfate in 20mL of KOH solution with the concentration of 20mol/L, placing the solution in a water bath kettle at the temperature of 75 ℃ to be stirred and dissolved for 35min, adding urea (the molar ratio of the urea to the titanium sulfate is 1:1), continuously stirring for 25min, and then reacting for 48h at the temperature of 180 ℃ to obtain a product A;
(2) taking 10g of the prepared product A to be put into 12mol/L NaOH solution, then adding 50g of polyimide fiber, and reacting for 24h at 185 ℃ to obtain TiO2A nanocomposite fiber material;
(3) taking TiO210g of composite fiber material, 1.8g of gamma-methacryloxypropyltrimethoxysilane (KH-570) and 3g of vinyl methyltrimethoxysilane are added into 400mL of tert-butyl alcohol, the reaction system is subjected to ultrasonic treatment for 0.3h, and then the mixture reacts for 2h at 73 ℃ to obtain modified TiO2A nanocomposite fiber material;
(4) modified TiO2Placing the nano composite fiber material in AgNO with the concentration of 1.2mol/L3And (5) performing solution treatment for 30min to obtain the light nano material for tap water bacteriostasis.
Example 2
A light nano material for tap water bacteriostasis is prepared by the following steps:
(1) dissolving 4g of titanium sulfate in 20mL of KOH solution with the concentration of 20mol/L, placing the solution in a water bath kettle at the temperature of 75 ℃ to be stirred and dissolved for 35min, adding urea (the molar ratio of the urea to the titanium sulfate is 1:1), continuously stirring for 25min, and then reacting for 45h at the temperature of 182 ℃ to obtain a product A;
(2) taking 12g of the prepared product A to be put into 10mol/L NaOH solution, then adding 50g of polyimide fiber, and reacting for 20h at 182 ℃ to obtain TiO2A nanocomposite fiber material;
(3) taking TiO210g of composite fiber material, 2g of gamma-methacryloxypropyltrimethoxysilane (KH-570) and 3.4g of vinyl methyltrimethoxysilane are added into 400mL of tert-butyl alcohol, the reaction system is subjected to ultrasonic treatment for 0.5h, and then the mixture is reacted for 3h at 75 ℃ to obtain modified TiO2A nanocomposite fiber material;
(4) modified TiO2Placing the nano composite fiber material in AgNO with the concentration of 1mol/L3And (5) soaking in the solution for 45min to obtain the light nano material for inhibiting the bacteria of the tap water.
Example 3
A light nano material for tap water bacteriostasis is prepared by the following steps:
(1) dissolving 4g of titanium sulfate in 20mL of KOH solution with the concentration of 20mol/L, placing the solution in a water bath kettle at the temperature of 75 ℃ to be stirred and dissolved for 35min, adding urea (the molar ratio of the urea to the titanium sulfate is 1:1), continuously stirring for 25min, and then reacting for 46h at the temperature of 185 ℃ to obtain a product A;
(2) taking 11g of the prepared product A, adding the product A into 11mol/L NaOH solution, then adding 50g of polyimide fiber, and reacting for 22h at 183 ℃ to obtain TiO2A nanocomposite fiber material;
(3) taking TiO210g of composite fiber material, 1.9g of gamma-methacryloxypropyltrimethoxysilane (KH-570) and ethylene3.2g of methyl trimethoxy silane is added into 400mL of tertiary butanol, the reaction system is subjected to ultrasonic treatment for 0.4h, and then the mixture is reacted for 3h at 73 ℃ to obtain modified TiO2A nanocomposite fiber material;
(4) modified TiO2Placing the nano composite fiber material in AgNO with the concentration of 1.1mol/L3And (5) performing 43min in the solution to obtain the light nano material for inhibiting the bacteria of the tap water.
Example 4
A light nano material for tap water bacteriostasis is prepared by the following steps:
(1) dissolving 4g of titanium sulfate in 20mL of KOH solution with the concentration of 20mol/L, placing the solution in a water bath kettle at the temperature of 75 ℃ to be stirred and dissolved for 35min, adding urea (the molar ratio of the urea to the titanium sulfate is 1:1), continuously stirring for 25min, and then reacting for 47h at the temperature of 183 ℃ to obtain a product A;
(2) taking 10g of the prepared product A to be put into 10mol/L NaOH solution, then adding 50g of polyimide fiber, and reacting for 23h at 184 ℃ to obtain TiO2A nanocomposite fiber material;
(3) taking TiO210g of composite fiber material, 2g of gamma-methacryloxypropyltrimethoxysilane (KH-570) and 3.3g of vinyl methyltrimethoxysilane are added into 400mL of tert-butyl alcohol, the reaction system is subjected to ultrasonic treatment for 0.3h, and then the mixture is reacted for 2h at 74 ℃ to obtain modified TiO2A nanocomposite fiber material;
(4) modified TiO2Placing the nano composite fiber material in AgNO with the concentration of 1mol/L3And (5) performing solution treatment for 35min to obtain the light nano material for tap water bacteriostasis.
Comparative example 1
The difference from example 1 is that vinylmethyltrimethoxysilane is not added.
Comparative example 2
The difference from example 1 is that step (3) is omitted.
Firstly, testing the photocatalytic bacteriostatic performance of the optical nano material:
respectively adding 20mL of bacterial liquid with the same concentration into 6 50mL flasks, respectively adding 5g of the light nano antibacterial materials prepared in the examples 1-4 and the comparative examples 1-2,the light intensity is 1245 muW/cm2After ultraviolet light with the wavelength of 390nm is irradiated for 3 hours, the bacteriostatic rate of the optical nano bacteriostatic material to different strains is counted, a flat plate counting method is adopted for the bacteriostatic rate statistics, and the calculation formula is as follows:
wherein A is0The bacterial colony number of the original bacterial liquid is shown, and A is the bacterial colony number of the bacterial liquid after bacteriostasis.
The bacteriostatic rates of the nano bacteriostatic materials prepared in examples 1 to 4 and comparative examples 1 to 2 on escherichia coli, salmonella and pseudomonas aeruginosa are shown in table 1.
TABLE 1
| Escherichia coli (%) | Salmonella (%) | Pseudomonas aeruginosa (%) | |
| Example 1 | 96.68±0.23 | 95.56±0.14 | 92.26±0.09 |
| Example 2 | 96.87±0.12 | 95.63±0.21 | 91.98±0.12 |
| Example 3 | 96.41±0.21 | 95.11±0.23 | 92.04±0.16 |
| Example 4 | 97.85±0.29 | 96.48±0.15 | 93.67±0.21 |
| Comparative example 1 | 80.51±0.14 | 79.28±0.22 | 78.85±0.24 |
| Comparative example 2 | 68.89±0.25 | 65.45±0.19 | 66.16±0.16 |
Second, testing the bacteriostasis of the optical nano material in the actual tap water
Municipal tap water was selected as a water sample, and the bacteriostatic performance of the bacteriostatic optical nano-materials of examples 1 to 4 was tested by a filtration membrane method, and the results are shown in table 2.
TABLE 2
Third, silver loss resistance performance test of light nano antibacterial material
According to the regulation of national drinking water standard GB5749-2006, the content of Ag (I) in a drinking water system is not more than 0.05mg/L, so that the lower the release amount of silver in the material is, the better the performance of the material is, and the smaller the pollution to the environment and the harm to human bodies are.
The test method comprises the following steps: 5g of the light nano bacteriostatic materials prepared in examples 1 to 4 were respectively put into 1L of municipal tap water, and water samples were taken out every 5 days, and Ag released from the light nano materials+The concentration was measured by Graphite Furnace Atomic Absorption Spectrometry (GFAAS).
And (3) testing results: the 90-day monitoring result of the silver loss resistance of the optical nano material shows that the content of silver released by the optical nano material in tap water is not more than 0.005mg/L and is far less than 0.05mg/L specified by the national drinking water standard GB5749-2006, and the requirement of human health can be met.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. A preparation method of a light nano antibacterial material is characterized by comprising the following steps:
(1) dissolving titanium sulfate in a KOH solution, then adding urea, and reacting to obtain a product A;
(2) reacting the product A with polyimide fibers in NaOH solution to obtain TiO2A nanocomposite fiber material;
(3) subjecting the TiO to a reaction2Adding the nano composite fiber material, gamma-methacryloxypropyltrimethoxysilane and vinyl methyltrimethoxysilane into an organic solvent, carrying out ultrasonic treatment, and reacting at 73-75 ℃ for 2-3h to obtain modified TiO2A nanocomposite fiber material;
(4) subjecting the modified TiO to2Nano composite fiber material in AgNO3Soaking in the solution to obtain the light nano antibacterial material.
2. The process according to claim 1, wherein the molar ratio of urea to titanium sulphate is 1: 1; the reaction conditions after urea addition were: reacting for 45-48h at 180-185 ℃.
3. The production method according to claim 1, wherein the mass ratio of the product a to the polyimide fiber is 1 to 1.2: 5.
4. The method according to claim 1, wherein the concentration of the NaOH solution is 10-12 mol/L.
5. The method as claimed in claim 1, wherein the reaction temperature in step (2) is 182 ℃ to 185 ℃ and the reaction time is 20 to 24 hours.
6. The method of claim 1, wherein the TiO is selected from the group consisting of2The mass ratio of the nano composite fiber material to the gamma-methacryloxypropyltrimethoxysilane to the vinyl methyltrimethoxysilane is 10:1.8-2: 3-3.4.
7. The method of claim 1, wherein the time of the ultrasonic treatment in step (3) is 0.3 to 0.5 h.
8. The method of claim 1, wherein the AgNO3The concentration of the solution is 1-1.2 mol/L; the soaking time in the step (4) is 30-45 min.
9. The light nano bacteriostatic material obtained by the preparation method according to any one of claims 1 to 8.
10. Use of the photonanometerism material of claim 9 for water treatment bacteriostasis.
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