CN106000126B - Bacteriostatic film and its preparation method and application based on nano zine oxide - Google Patents
Bacteriostatic film and its preparation method and application based on nano zine oxide Download PDFInfo
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- CN106000126B CN106000126B CN201610512043.7A CN201610512043A CN106000126B CN 106000126 B CN106000126 B CN 106000126B CN 201610512043 A CN201610512043 A CN 201610512043A CN 106000126 B CN106000126 B CN 106000126B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/26—Polyalkenes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
Abstract
The present invention provides a kind of bacteriostatic film based on nano zine oxide, preparation method is：Sucrose solution is heated, through centrifugal drying after cooling, obtains carbon ball；Carbon ball is mixed with zinc nitrate aqueous solution, is aged, filters, cleans, centrifugal drying after ultrasonic disperse, obtain ZnO microsphere presoma；ZnO microsphere presoma is carried out to different calcination processings, obtains the nano zine oxide microballoon of different structure；The nano zine oxide microballoon of any structure and dry membrane material are mixed with casting solution, on a glass by casting solution casting, scraper is scraped to film forming, after room temprature evaporation, glass plate is placed in deionized water and be exchanged film forming to get finished product, can be used as bacteriostatic film or ultrafiltration membrane application；The present invention by the nano zine oxide microballoon of different structure it is miscellaneous enter film in, not only have good bacteriostasis property, also high flux and retention, and the mechanical tensile strength having had.
Description
(1) technical field
The invention belongs to membrane separation and purification technology fields, and in particular to a kind of novel bacteriostatic film based on nano zine oxide
And its preparation method and application.
(2) background technology
Ultrafiltration and microfiltration film is since unique physicochemical properties are widely used in Chemical Decomposition, food, biological medicine,
Fields such as environmental project, but membrane biological pollution can cause membrane permeability to reduce, operating cost increase, thus prepare possess it is antibacterial
The hybridized film of performance is extremely urgent.
It is a kind of method preparing high performance bacteriostatic film well, inorganic antibacterial that inorganic antibacterial material hydridization, which is entered in film,
Material relative to organic anti-bacterial material has that safe, persistence is strong, anti-microbial property is stable and heat-resist etc. excellent
Point.Inorganic antibacterial material includes mainly two major classes, and one kind is photocatalyst-type semiconductor anti-biotic material, and another kind of lived containing antibacterial
The inorganic antibacterial material of property metal (such as silver, copper, zinc).Since the sterilizing function of photocatalyst-type semiconductor anti-biotic material must be borrowed
Help illumination that could realize, which greatly limits its application ranges；The inorganic antibacterial material of the metallics containing antibacterial activity
Material is then current research and the most widely used.
As a kind of metal oxide being used for antibacterial earliest, zinc oxide has good safety and stability, beautiful
Food Drug Administration of state is considered one of the zinc compound of 5 kinds of safety, and zinc oxide series anti-biotic material is of low cost,
Using also increasingly wider, and the zinc oxide of Nano grade also has good application prospect.Currently, the oxygen of micron and Nano grade
Change zinc to be promoted, Nano grade particle has been used as antiseptic, and being incorporated in hospital with wallpaper uses；Since zinc oxide has
Good ultraviolet absorption ability, it is also applied in suncream；And because its preferable antibacterial effect is also applied to manually
The fields such as dental surface overlay film, weaving；Or it is used for treating central nervous system disease as trial drug.
However, inorganic particle it is miscellaneous enter film in can be lost in some metal ions, the decline and two of bacteriostasis property can be caused in this way
Secondary pollution, therefore how to prepare the bacteriostatic film with high bacteriostatic activity and high stability is still a challenge.
(3) invention content
The bacteriostatic film and its preparation method and application based on nano zine oxide that the object of the present invention is to provide a kind of, the present invention
The bacteriostatic film has good bacteriostasis property, and flux is promoted after adding inorganic filler, and rejection increases, and mechanical stretching is strong
Degree rises.
The present invention is turned by preparing the nano zine oxide microballoon of several different structures using carbon ball as template by phase
The method of changing obtains plate membrane.
The present invention adopts the following technical scheme that：
A kind of bacteriostatic film based on nano zine oxide, is prepared as follows to obtain：
(1) sucrose solution of a concentration of 1~3mol/L is placed in 3~5h of heat treatment at 100~150 DEG C, is passed through after cooling
Centrifugal drying obtains carbon ball；
(2) carbon ball obtained by step (1) and the zinc nitrate aqueous solution of a concentration of 0.5~5mol/L are pressed into feed liquid mass ratio 1：30
~50 mixing, ultrasonic disperse (50KHz, 0.5h) are aged 5~8h afterwards, filter, filter cake second alcohol and water (preferred volume ratio 1：1)
Mixed solution stirring and washing, centrifugal drying obtain ZnO microsphere presoma；
(3) ZnO microsphere presoma obtained by step (2) is pressed into one of following method respectively and carries out calcination processing, obtained not
Isostructural nano zine oxide microballoon：
(a) 500 DEG C are warming up to the rate of 2 DEG C/min, and calcine 2h at such a temperature, obtain core-shell type nano zinc oxide
Microballoon；
(b) 500 DEG C are warming up to the rate of 1 DEG C/min, and calcine 2h at such a temperature, it is micro- to obtain single wall nano zinc oxide
Ball；
(4) organic solvent is added with dry membrane material in the nano zine oxide microballoon of any structure obtained by step (3)
In, it stirs evenly, stands (0.5~1h), ultrasonic deaeration (50KHz, 0.5~1h), obtain casting solution；
The mass ratio of the nano zine oxide microballoon and membrane material is 1：15~160；The volume of the organic solvent is used
Amount is calculated as 5~16mL/g with the quality of membrane material；
The membrane material is one of following：Polyethylene, polypropylene, polysulfones, polyether sulfone, Kynoar, polyvinyl chloride,
Polypropylene is fine, cellulose acetate；
The organic solvent is DMAC N,N' dimethyl acetamide, N,N-dimethylformamide, tetrahydrofuran, N- methylpyrroles
The mixed solvent of one or more of alkanone arbitrary proportion；
(5) casting solution obtained by step (4) being cast on the glass plate of clean dried, scraper is scraped to film forming, room temperature (20~
30 DEG C) evaporation 2~10s after, glass plate is placed in deionized water and carries out being exchanged film forming, obtain described in based on nano oxygen
Change the bacteriostatic film of zinc.
Bacteriostatic film produced by the present invention based on nano zine oxide can be used as bacteriostatic film or ultrafiltration membrane application.
Advantages of the present invention：By the nano zine oxide microballoon of different structure it is miscellaneous enter film in, not only have good bacteriostasis property,
Also high flux and retention, and the mechanical tensile strength having had.
(4) it illustrates
Fig. 1 is the scanning electron microscope (SEM) photograph of core-shell type nano ZnO microsphere in embodiment 1；
Fig. 2 is the surface of core-shell type nano ZnO microsphere/polysulfones hybridized film in embodiment 1；
Fig. 3 is single wall nano ZnO microsphere transmission electron microscope picture in embodiment 2；
Fig. 4 is the cross-section diagram of single wall nano ZnO microsphere/polysulfones hybridized film in embodiment 2；
Fig. 5 is the scanning electron microscope (SEM) photograph of Zinc oxide nanoparticle in comparative example.
(5) specific implementation mode
The present invention is described in detail with reference to specific embodiment, but the present invention is not limited to the following embodiments,
It does not depart from the content of present invention and range, change all should include within the technical scope of the present invention.
Embodiment 1：Core-shell type nano ZnO microsphere/polysulfones hybridized film
(1) by the sucrose solution 40mL input reaction kettles of 3mol/L, it is heated to 150 DEG C in an oven, keeps the temperature 5h, it is cooling
Afterwards, the substance centrifugal drying in reaction kettle is stayed overnight, obtains carbon ball 1g.
(2) 0.6g carbon balls is taken to be added in the zinc nitrate solution of 30mL 5mol/L, 50KHz ultrasonic disperse 0.5h, and be aged
6h is filtered later, filter cake water and ethyl alcohol volume ratio 1：1 mixed solution cleaning (30mL × 3), centrifugal drying is overnight, obtains
ZnO microsphere presoma 0.8g.
(3) gained ZnO microsphere presoma is put into Muffle furnace and is calcined, temperature program is set as：With 2 DEG C/min's
Rate is warming up to 500 DEG C, and calcines 2h at 500 DEG C, obtains core-shell type nano ZnO microsphere.
(4) the core-shell type nano ZnO microsphere 0.23g of preparation and dry polysulfones 3.65g are dissolved in 20mL N, N diformazans
It in yl acetamide, is stirred until homogeneous, stands 0.5h, 50Kz ultrasound deaeration 0.5h, obtain casting solution；
(5) regulating environmental humidity is 50%, temperature is 25 DEG C, and casting solution is cast on the glass plate of clean dried, is scraped
Knife is scraped to film forming, after room temprature evaporation 10s, glass plate is placed in deionized water and carries out being exchanged film forming, obtains hud typed receive
Rice ZnO microsphere/polysulfones hybridized film.
Will diaphragm cleaning, it is dry after cut out as the disk of a diameter of 8mm, carry out before bacteriostatic experiment that irradiation is gone out in the UV lamp
Bacterium 30min；Bactericidal test is：By 0.2mL (106A/mL) fresh E. coli and staphylococcus aureus bacterium solution it is uniform
It is coated on LB solid mediums；Diaphragm is respectively placed in the culture medium of Escherichia coli and staphylococcus aureus, at 37 DEG C
Culture for 24 hours, observes bacterial clump growing state, and hybridized film and blank film are compared and measure inhibition zone size.
The measurement of membrane flux is carried out under the conditions of 0.1MPa, and 0.2MPa precompressed 30min is carried out before testing.Pure water tests 1h
After replace with BSA (0.2g L-1) 30min is run, carrying out pure water flux test after pure water rinsing 30min.
Prepared core shell type zinc oxide microballoon/polysulfones hybridized film inhibition zone reaches 8.9mm, and pure water flux is up to
139.6L/m2H is 85.7% to BSA solution rejections, and mechanical strength is promoted to 5.19Mpa.
Embodiment 2：Single wall nano ZnO microsphere/polysulfones hybridized film
The present embodiment and embodiment 1 the difference is that：Temperature program is set as in step (3)：With the speed of 1 DEG C/min
Rate is warming up to 500 DEG C, and calcines 2h at 500 DEG C, obtains single wall nano ZnO microsphere, and other conditions are all identical, final to make
Obtain single wall nano ZnO microsphere/polysulfones hybridized film.
Test condition reaches with embodiment 1, prepared single wall nano ZnO microsphere/polysulfones hybridized film inhibition zone
10.2mm, pure water flux are up to 142.1L/m2H is 87.3% to BSA solution rejections, and mechanical strength is promoted to
4.97Mpa。
Embodiment 3：Core-shell type nano ZnO microsphere/polyethylene hybridized film
The present embodiment and embodiment 1 the difference is that：Step (4) flat sheet membranes material changes polyethylene into, other
Part is all identical, finally obtained core-shell type nano ZnO microsphere/polyethylene hybridized film.
Test condition reaches with embodiment 1, prepared core-shell type nano ZnO microsphere/polyethylene hybridized film inhibition zone
9.1mm, pure water flux are up to 118.1L/m2H is 90.3% to BSA solution rejections, and mechanical strength is promoted to
5.02Mpa。
Comparative example
This comparative example difference from example 1 is that：Temperature program is set as in step (3)：With the speed of 5 DEG C/min
Rate is warming up to 500 DEG C, and calcines 4h at 500 DEG C, obtains Zinc oxide nanoparticle, and other conditions are all identical, and oxygen is finally made
Change zinc nanoparticles/polysulfones hybridized film, obtained hybridized film is in spite of good fungistatic effect, but its zinc ion leakage rate is
Three times of core-shell type nano ZnO microsphere/polysulfones hybridized film, be twice of single wall nano ZnO microsphere/polysulfones hybridized film,
This illustrates that core-shell type nano ZnO microsphere/polysulfones hybridized film and single wall nano ZnO microsphere/polysulfones hybridized film of the present invention are gathered around
There are very low zinc ion release and good stability.
Claims (7)
1. a kind of bacteriostatic film based on nano zine oxide, which is characterized in that the bacteriostatic film based on nano zine oxide is by as follows
Method is prepared：
(1) sucrose solution of a concentration of 1~3mol/L is placed in 3~5h of heat treatment at 100~150 DEG C, through centrifugation after cooling
It is dry, obtain carbon ball；
(2) carbon ball obtained by step (1) and the zinc nitrate aqueous solution of a concentration of 0.5~5mol/L are pressed into feed liquid mass ratio 1：30~50
It mixes, 5~8h, filtering is aged after ultrasonic disperse, the mixed solution stirring and washing of filter cake second alcohol and water, centrifugal drying obtains
ZnO microsphere presoma；
(3) ZnO microsphere presoma obtained by step (2) is pressed into one of following method respectively and carries out calcination processing, obtain different knots
The nano zine oxide microballoon of structure：
(a) 500 DEG C are warming up to the rate of 2 DEG C/min, and calcine 2h at such a temperature, it is micro- to obtain core-shell type nano zinc oxide
Ball；
(b) 500 DEG C are warming up to the rate of 1 DEG C/min, and calcine 2h at such a temperature, obtain single wall nano ZnO microsphere；
(4) the nano zine oxide microballoon of any structure obtained by step (3) is added with dry membrane material in organic solvent, is stirred
It mixes uniformly, stands, ultrasonic deaeration, obtain casting solution；
The mass ratio of the nano zine oxide microballoon and membrane material is 1：15~160；
The membrane material is one of following：Polyethylene, polypropylene, polysulfones, polyether sulfone, Kynoar, polyvinyl chloride, poly- third
Alkene is fine, cellulose acetate；
The organic solvent is DMAC N,N' dimethyl acetamide, N,N-dimethylformamide, tetrahydrofuran, N-Methyl pyrrolidone
One or more of arbitrary proportion mixed solvent；
(5) casting solution obtained by step (4) being cast on the glass plate of clean dried, scraper is scraped to film forming, room temprature evaporation 2~
After 10s, glass plate is placed in deionized water and carries out being exchanged film forming, obtained described based on the antibacterial of nano zine oxide
Film.
2. the bacteriostatic film based on nano zine oxide as described in claim 1, which is characterized in that in step (2), the ultrasound point
Scattered frequency is 50KHz, time 0.5h.
3. the bacteriostatic film based on nano zine oxide as described in claim 1, which is characterized in that in step (2), the ethyl alcohol and
The volume ratio of ethyl alcohol and water is 1 in the mixed solution of water：1.
4. the bacteriostatic film based on nano zine oxide as described in claim 1, which is characterized in that in step (4), the standing
Time is 0.5~1h.
5. the bacteriostatic film based on nano zine oxide as described in claim 1, which is characterized in that in step (4), the ultrasound is de-
The frequency of bubble is 50KHz, and the time is 0.5~1h.
6. the bacteriostatic film based on nano zine oxide as described in claim 1, which is characterized in that described organic molten in step (4)
The volumetric usage of agent is calculated as 5~16mL/g with the quality of membrane material.
7. the application based on the bacteriostatic film of nano zine oxide as bacteriostatic film or ultrafiltration membrane as described in claim 1.
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| CN106731876A (en) * | 2016-12-20 | 2017-05-31 | 济南大学 | Visible light catalytic flat-plate ultrafiltration membrane and preparation method based on dopen Nano ZnO |
| CN107158973A (en) * | 2017-05-19 | 2017-09-15 | 华中农业大学 | A kind of nano zinc oxide modified polyether sulfone high flux antibacterial film and preparation method |
| CN108727628B (en) * | 2018-06-14 | 2021-03-02 | 常州大学 | Nano-silver hollow microsphere/PVDF ultrafiltration membrane and preparation method thereof |
| CN110745909A (en) * | 2019-10-23 | 2020-02-04 | 李天栋 | Preparation method of nano-scale ultrafiltration biological integrated membrane |
| CN113634139A (en) * | 2021-07-16 | 2021-11-12 | 江苏大学 | Preparation method of cellulose acetate-based composite membrane and application of cellulose acetate-based composite membrane in dynamic separation and extraction of tellurium |
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| CN102259906A (en) * | 2011-06-02 | 2011-11-30 | 西北工业大学 | Method for preparing hollow zinc oxide microspheres |
| CN102974236B (en) * | 2012-12-03 | 2015-01-28 | 河海大学 | Composite flat-sheet polysulfone membrane doped with active carbon and nanometer zinc oxide and preparation method thereof |
| CN105498558B (en) * | 2015-12-17 | 2018-10-23 | 浙江工业大学 | Hybridized film of silver nanoparticles loaded and its preparation method and application |
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