CN108479429A - It is a kind of to utilize nanometer Fe3O4The preparation method of modified PVDF microfiltration membranes and its utilization - Google Patents
It is a kind of to utilize nanometer Fe3O4The preparation method of modified PVDF microfiltration membranes and its utilization Download PDFInfo
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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- B01D71/32—Polyalkenyl halides containing fluorine atoms
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- C02F3/00—Biological treatment of water, waste water, or sewage
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Abstract
Pass through the loading nanometer Fe on traditional pvdf membrane material3O4Particle is modified film, promotes the hydrophily of film.And due to Fe3O4It is conductive, in antimicrobial treatment process, the conductor of inter-species direct electron transfer is can be used as, inter-species electron transfer efficiency is improved, to increase the methane production of microorganism in anaerobic biological reactor.Further, since in anaerobic biological reactor, when microbiological treatment pollutant, will produce a certain amount of organic acid, the H that organic acid ionizes out+Meeting and Fe3O4It reacts, generates Fe2+And Fe3+。Fe2+It can promote the growth of microorganism, Fe3+With oxidisability, pollutant can be aoxidized, can both promote the degradation effect of microbe.With nanometer Fe3O4Modified PVDF microfiltration membranes promote the degradation treatment effect of microorganism parachlorphenol substance, and the chloro base on pollutant is made to be detached from from phenyl ring, reduce pollutant toxicity, improve the biodegradability of pollutant.
Description
Technical field
The present invention relates to organic wastewater biological treatment fields, and in particular to a kind of to be modified PVDF micro-filtrations using nanometer Fe_3O_4
The preparation method of film and its utilization in anaerobic biological treatment.
Background technology
Anaerobic Microbiological Treatment Technology is processing high concentration, effective ways difficult to degrade, organic wastewater.But due to anaerobic organism
Processing system is still faced with operation stability difference and the low problem of Operating ettectiveness, and anaerobic biological treatment is applied to practical height
There is also larger difficulty for concentration, difficult to degrade, treatment of Organic Wastewater.It can effectively be promoted and be detested using anaerobic membrane bioreactor
Oxygen biological treatment system stability and process performance.
Currently used membrane material has Kynoar（PVDF）, PVDF materials are a kind of those semi-crystalline materials, fusing point 172
DEG C, 112 ~ 145 DEG C of heat distortion temperature can stablize use in -40 ~ 150 DEG C of temperature ranges.When temperature reaches 316 DEG C or more
When, PVDF can just be decomposed.Since it is with characteristics such as excellent chemical stability, thermal stability and easy film forming, PVDF is in film
Preparation field has a wide range of applications.The membrane module made by PVDF materials is usually used in membrane distillation, gas purification, organic solvent essence
System etc., and there is preferable treatment effect and stability.
Pvdf membrane is a kind of hydrophobic film, has high mechanical strength, and toughness is high, has Thief zone to gas and liquid
Property, it is common membrane filtration material both at home and abroad the features such as high-low temperature resistant.To macromolecular, bacterium, the impurity such as silt have good
Treatment effect.It is dirty during being filtered to pollutant using film but since the casting solution of pvdf membrane is organic solution
Organic pollution in water can be attached on pvdf membrane, to form one layer of cake layer.This can cause the permeability of film to decline, shadow
Ring treatment effect of the film to pollutant.Especially in membrane bioreactor, due in membrane bioreactor, microbiological treatment mistake
It will produce a large amount of EPS in journey, when being filtered, these EPS can be adhered to film surface, under the permeability for leading to film
Drop, improves the osmotic pressure of film, or even can cause the damage of film.
The membrane material of tradition application can not reinforced anaerobic treatment process to the process performance of pollutant, and conventional film has
Stronger hydrophobicity, is easy to form cake layer, causes the permeability of film to decline, improves the osmotic pressure of film.
Invention content
This patent develops a kind of biological treatment effect that can promote membrane material to anaerobic biological treatment and inhibition
The membrane material of the formation of fouling membrane.
To promote film contamination resistance, enrichment of the pollutant in film surface is reduced, this patent research uses nanometer Fe3O4It is right
Pvdf membrane is modified, and promotes the stain resistance of membrane module, extends the usage time of membrane module.By in traditional pvdf membrane material
Upper loading nanometer Fe3O4Particle is modified film, promotes the hydrophily of film.And due to Fe3O4It is conductive, in micro- life
In object processing procedure, the conductor of inter-species direct electron transfer is can be used as, improves inter-species electron transfer efficiency, to increase anaerobism life
The methane production of microorganism in object reactor.Further, since in anaerobic biological reactor, when microbiological treatment pollutant, will produce
A certain amount of organic acid, the H that organic acid ionizes out+Meeting and Fe3O4It reacts, generates Fe2+And Fe3+。Fe2+It can promote micro- life
The growth of object, Fe3+With oxidisability, pollutant can be aoxidized, can both promote the degradation of microbe
Effect.
The present invention uses nanometer Fe_3O_4 as the raw material being blended, and not only promotes PVDF microfiltration membranes hydrophilies, reduces to film table
The pollution in face also promotes the operation of bioreactor, accelerates treatment effeciency of the bioreactor to pollutant.With nanometer Fe3O4
Modified PVDF microfiltration membranes promote the degradation treatment effect of microorganism parachlorphenol substance, make the chloro base on pollutant from phenyl ring
It is detached from, reduces pollutant toxicity, improve the biodegradability of pollutant.
Utilize nanometer Fe3O4The preparation method of modified PVDF microfiltration membranes, comprises the steps of：
A. it takes in a certain amount of PVDF mergings container, with 60 DEG C of temperature, drying to constant weight in air dry oven.It will be dried to
The PVDF of constant weight be placed in drier be cooled to room temperature it is spare；
B. by the PVDF powder and nanometer Fe after drying3O4Mixing is placed in a reaction flask, and is added thereto a certain amount of
DMAc keeps certain gross mass, obtains mixed solution A；
C. reaction bulb is positioned on magnetic stirring apparatus, is reacted with the mixing speed of 100rpm/min under 60 DEG C of constant temperatures
For a period of time, after the PVDF in solution A to be mixed is completely dissolved, stops stirring, obtain mixed solution B；Magnetic stirring apparatus can be by perseverance
Warm ultrasound substitutes.
D. the mixed solution B that PVDF is completely dissolved is placed at 60 DEG C continue heat 3-6h be then placed in ripe under room temperature
Change deaeration 1d, obtains casting solution C；
E. casting film is carried out using the casting solution C after the completion of curing：Casting solution C is poured on non-woven fabrics, and one is scraped using film-casting machine
Determine the film of thickness, and non-woven fabrics is dipped into coagulating bath, make the casting solution gel solidification on its surface, obtains nanometer Fe3O4Change
The PVDF microfiltration membranes of property.
Directly casting solution C can also be poured on unorganic glass plate, using glass bar or self-control scraper in glass plate
On casting solution C scraped into certain thickness, then glass plate is put into togerther together with the casting solution on glass plate in coagulating bath, makes casting
Film liquid forms a film in coagulating bath, obtains nanometer Fe3O4Modified PVDF microfiltration membranes.
Nanometer Fe3O4Particle requirement grain size≤100nm, nanometer Fe3O4Commercially available commercialization, can also come according to the following steps
It prepares：
A. by FeCl2And FeCl3The solution of mixed dissolution is used heating water bath to certain reaction by mixed dissolution in proportion
Temperature is stirred using magnetic stirring apparatus with certain rotating speed, while to a certain concentration NH is wherein slowly added dropwise with 10DS-13·
H2O, until pH value of solution to alkalinity, obtains mixed solution C；Magnetic stirring apparatus can be substituted by thermostatic ultrasonic.
B. mixed solution C magnetic stirring apparatus is continuing at a certain temperature with the rotating speed of 200-500rpm/min to stir
40min-60min is mixed, makes to form black particle object in solution, is then allowed to stand 1-2h, obtains mixed solution D；
C. a small amount of surfactant is added into mixed solution D, mixed solution is then placed in ultrasonic disperse 6- in ultrasonic machine
9h obtains mixed solution E；
D. after completing ultrasound, a certain amount of ethyl alcohol is added into mixed solution E, will be made in mixed solution E using magnet later
Black particle detached, then the black particle separated is rinsed using deionized water, until cleaning solution is in neutrality；
E. by Fe3O4After particle is rinsed with deionized water, the grinding rate grinding with 200-300rpm/min is placed in grinding pot
For a period of time, later with after washes of absolute alcohol 2-3 times, drying in a vacuum can be obtained nanometer Fe3O4。
Nanometer Fe3O4Utilization of the Modified Membrane in anaerobic biological treatment：
Antiphen is handled using nanometer Fe_3O_4 modified PVDF membrane reinforced anaerobic biological treatment system, microorganism can be promoted to double chlorine
The degradation treatment effect of phenol improves the gas production rate and yield of methane in biological treatment system.Simultaneously in microbial cultivation process
In, existing nanometer Fe_3O_4 can release Fe2+ and Fe3+ under the action of microorganism.Wherein, Fe2+ is that microorganism is necessary
One of nutrient.Suitable Fe2+ is added can promote biological growth rate in anaerobic organism system to a certain extent, by force
Microorganism conversion methane efficiency in change system.And the Fe2+ generated in system can be sent out with chlorophenols under certain condition
Raw redox reaction, makes the chloro base on pollutant be detached from from phenyl ring, to make the reduction of pollutant toxicity, improves pollutant
Biodegradability, process performance and treatment effeciency of the further enhancement microbiological to pollutant.
In anaerobic biological treatment, Fe3O4 can be used as the carrier of Direct electron transfer between microorganism, and it is anti-to improve anaerobism
The electron transfer efficiency between microorganism in processing procedure is answered, unnecessary conversion process is reduced.By the way that Fe3O4 is added, can contract
Electronic transfer process between short acetogen and methanogen.When Fe3O4 is added, acetogen and methanogen mainly lead to
Cross the electronic transfer process between H2 two kinds of microorganisms of progress that acetogen generates in acid process.H2 can not possibly be completely from production
Acetic acid bacteria is transferred to methanogen, therefore in electron transfer process, and the H2 as electronics transfer carrier will appear a certain amount of
Loss, to reduce the gas production of methane.When Fe3O4 is added in reactor, since Fe3O4 has stronger magnetic and leads
Electrically, the electronics transfer carrier that two kinds of microorganisms can be formed by Fe3O4 carries out the direct electron transfer process between microorganism,
To reduce the loss of electrons in electron transfer process, methane production is improved.
Specific implementation mode
It elaborates below to the present invention according to specific implementation mode.Experimental method used in following embodiments is such as
It is conventional method without specified otherwise.The materials, reagents and the like used in the following examples unless otherwise specified can be from business
Approach obtains.
Nanometer Fe3O4Preparation：
1. by FeCl2And FeCl3With 1:Mixed solution is used heating water bath to certain reaction temperature by 2 ratio mixed dissolution
Degree, is stirred using magnetic stirring apparatus with certain rotating speed, while to a certain concentration NH is wherein slowly added dropwise with 10DS-13·H2O,
Until pH value of solution to alkalinity, obtains mixed solution C.
2. mixed solution C is continuing with magnetic stirring apparatus at a certain temperature with the rotating speed of 200-500rpm/min to stir
40min-60min is mixed, makes to form black particle object in solution, is then allowed to stand 1-2h, obtains mixed solution D.
3. a small amount of surfactant is added into mixed solution D, mixed solution is then placed in ultrasound point in ultrasonic machine
6-9h is dissipated, mixed solution E is obtained.
4. after completing ultrasound, a certain amount of ethyl alcohol is added into mixed solution E, it later will be in mixed solution E using magnet
The black particle made is detached, and then rinses the black particle separated using deionized water, until cleaning solution is in
It is neutral.
5. by Fe3O4After particle is rinsed with deionized water, it is placed in the grinding rate with 200-300rpm/min in grinding pot
Grinding a period of time, later with after washes of absolute alcohol 2-3 times, drying in a vacuum can be obtained nanometer Fe3O4.And it will obtain
Nanometer Fe3O4It is put in spare in brown bottle.
Fe3O4Modified film preparation：
1. taking in a certain amount of PVDF mergings container, with 60 DEG C of temperature, drying to constant weight in air dry oven.It will be dried to
The PVDF of constant weight be placed in drier be cooled to room temperature it is spare.
2. the PVDF powder after 15g is dried and 0 ~ 5g nanometer Fes3O4Mixing is placed in 100mL reaction bulbs, and thereto
A certain amount of DMAc is added, it is 100g to make reaction gross mass, obtains mixed solution A.
3. reaction bulb is positioned on magnetic stirring apparatus, with the mixing speed of 100rpm/min under 60 DEG C of constant temperatures
Reaction for a period of time, after the PVDF in solution A to be mixed is completely dissolved, stops stirring, obtains mixed solution B.
Continue to heat 3-6h 4. the mixed solution B that PVDF is completely dissolved is placed at 60 DEG C.Then, casting solution C is placed in
Deaeration 1d is cured under room temperature, obtains casting solution C.
5. carrying out casting film using the casting solution C after the completion of curing.Casting solution C is poured on non-woven fabrics, is scraped using film-casting machine
Go out certain thickness film, and non-woven fabrics is dipped into coagulating bath, make the casting solution gel solidification on its surface, obtains nanometer
Fe3O4Modified PVDF microfiltration membranes.
Nanometer Fe3O4Utilization of the Modified Membrane in anaerobic biological treatment：
1. establishing anaerobic membrane biosystem processing system.Membrane module is established using porous clear water pvdf membrane is met, carries out anaerobic organism training
It supports.
2. under anaerobic, carrying out microculture with 37 DEG C of temperature.Other reaction conditions are as follows：
Microculture substance：Glucose 4686.03mg/L (COD: N: P=800: 5: 1)；
NaCl 100mg/L；
MgCl2•6H2O 100mg/L；
CaCl250mg/L；
FeCl2•4H2O 2mg/L;
H3BO3 0.05mg/L;
ZnCl2 0.05mg/L;
CuCl2•2H2O 0.038mg/L;
MnCl2•4H2O 0.05mg/L;
(NH4)6Mo7O24•4H2O 0.05mg/L;
AlCl3 0.05mg/L;
CoCl2•6H2O 0.05mg/L;
NiCl2•6H2O 0.092mg/L;
Na2SeO3•5H2O 0.1mg/L。
Chlorophenols concentration：10mg/L.
3. COD and chlorophenols concentration in results of regular determination processing water outlet, gas production and methane proportion in the period.
It determines in nanometer Fe3O4Under the conditions of existing, the treatment effect and anaerobic membrane biosystem of AnMBR processing system parachlorphenol class waste water
Fouling membrane situation caused by reactor.
PVDF:Poly (vinylidene fluoride), Kynoar
DMAc:Dimethylacetamide, n,N-dimethylacetamide
EPS：Extracellular polymeric substance, extracellular polymeric.
Claims (5)
1. a kind of utilizing nanometer Fe3O4The preparation method of modified PVDF microfiltration membranes, comprises the steps of：
A. it takes in a certain amount of PVDF mergings container, with 60 DEG C of temperature, drying to constant weight in air dry oven, will be dried to
The PVDF of constant weight be placed in drier be cooled to room temperature it is spare；
B. by the PVDF powder and nanometer Fe after drying3O4Mixing is placed in a reaction flask, and a certain amount of DMAc is added thereto,
Certain gross mass is kept, mixed solution A is obtained；
C. reaction bulb is positioned on magnetic stirring apparatus, is reacted with the mixing speed of 100rpm/min under 60 DEG C of constant temperatures
For a period of time, after the PVDF in solution A to be mixed is completely dissolved, stops stirring, obtain mixed solution B；
D. the mixed solution B that PVDF is completely dissolved is placed at 60 DEG C and continues to heat 3-6h, then, it is de- to be placed in curing under room temperature
1d is steeped, casting solution C is obtained；
E. casting film is carried out using the casting solution C after the completion of curing：Casting solution C is poured on non-woven fabrics, and one is scraped using film-casting machine
Determine the film of thickness, and non-woven fabrics is dipped into coagulating bath, make the casting solution gel solidification on its surface, obtains nanometer Fe3O4Change
The PVDF microfiltration membranes of property.
2. a kind of as claimed in claim 1 utilize nanometer Fe3O4The preparation method of modified PVDF microfiltration membranes, step include nanometer
Fe3O4Preparation：
A. by FeCl2And FeCl3The solution of mixed dissolution is used heating water bath to certain reaction temperature by mixed dissolution in proportion
Degree, is stirred using magnetic stirring apparatus with certain rotating speed, while to a certain concentration NH is wherein slowly added dropwise with 10DS-13·H2O,
Until pH value of solution to alkalinity, obtains mixed solution C；
B. mixed solution C is continuing with magnetic stirrer at a certain temperature with the rotating speed of 200-500rpm/min
40min-60min makes to form black particle object in solution, is then allowed to stand 1-2h, obtains mixed solution D；
C. a small amount of surfactant is added into mixed solution D, mixed solution is then placed in ultrasonic disperse 6- in ultrasonic machine
9h obtains mixed solution E；
D. after completing ultrasound, a certain amount of ethyl alcohol is added into mixed solution E, will be made in mixed solution E using magnet later
Black particle detached, then the black particle separated is rinsed using deionized water, until cleaning solution is in neutrality；
E. by Fe3O4After particle is rinsed with deionized water, the grinding rate grinding with 200-300rpm/min is placed in grinding pot
For a period of time, later with after washes of absolute alcohol 2-3 times, drying in a vacuum can be obtained nanometer Fe3O4。
3. a kind of as claimed in claim 1 or 2 utilize nanometer Fe3O4The preparation method of modified PVDF microfiltration membranes, feature exist
In wherein magnetic stirring apparatus can be substituted by thermostatic ultrasonic.
4. a kind of as described in claim 1 utilize nanometer Fe3O4The preparation method of modified PVDF microfiltration membranes, which is characterized in that
In the casting film of step E, directly casting solution C can be poured on unorganic glass plate, using glass bar or self-control scraper in glass
Casting solution C is scraped into certain thickness in glass plate, is then put into togerther glass plate in coagulating bath together with the casting solution on glass plate,
So that casting solution is formed a film in coagulating bath, obtains nanometer Fe3O4Modified PVDF microfiltration membranes.
5. such as the nanometer Fe of the description of claim 1,2 or 43O4Utilization of the modified PVDF microfiltration membranes in anaerobic biological treatment,
It is characterized in that, nanometer Fe3O4Modified PVDF microfiltration membranes promote the degradation treatment effect of microorganism parachlorphenol substance.
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| PL428333A1 (en) * | 2018-12-24 | 2019-06-03 | Univ Mikolaja Kopernika W Toruniu | Method for modification of the separation material surfaces |
| CN110157021A (en) * | 2019-06-20 | 2019-08-23 | 湘潭大学 | A method of improving Kynoar heat dissipation performance |
| CN111362401A (en) * | 2020-03-18 | 2020-07-03 | 山东大学 | Utilizing micron Fe3O4Sewage treatment method for strengthening anaerobic dynamic membrane bioreactor |
| CN111826403A (en) * | 2020-06-05 | 2020-10-27 | 同济大学 | Anaerobic digestion method for organic wastes |
| CN112023724A (en) * | 2020-08-25 | 2020-12-04 | 广州大学 | Modified polyvinylidene fluoride ultrafiltration membrane and preparation method thereof |
| PL447984A1 (en) * | 2018-12-24 | 2024-05-13 | Uniwersytet Mikołaja Kopernika W Toruniu | Method of modifying the surface of separation materials |
| PL447983A1 (en) * | 2018-12-24 | 2024-05-13 | Uniwersytet Mikołaja Kopernika W Toruniu | Method of modifying the surface of separation materials |
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