CN108325398A - A kind of preparation method of pollution-resistant membrane material - Google Patents
A kind of preparation method of pollution-resistant membrane material Download PDFInfo
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- CN108325398A CN108325398A CN201810122053.9A CN201810122053A CN108325398A CN 108325398 A CN108325398 A CN 108325398A CN 201810122053 A CN201810122053 A CN 201810122053A CN 108325398 A CN108325398 A CN 108325398A
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- pollution
- membrane material
- resistant membrane
- preparation
- styrene
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Classifications
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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
-
- 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
- B01D67/0002—Organic membrane manufacture
-
- 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
-
- 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
- B01D69/06—Flat membranes
-
- 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
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to membrane material preparing technical field more particularly to a kind of preparation methods of pollution-resistant membrane material, include the following steps：Solution is prepared, membranous type casting, is post-processed, hydrophilic modifying：Blend film is immersed in Nano silver solution, pollution-resistant membrane material is obtained after dry.The present invention has good anti-microbial property, to bacterium, growth and breeding of the microorganism on membrane material surface has significant inhibiting effect, specifically, the test of antibacterial ring size is carried out to film using pseudomonas aeruginosa, the results showed that pollution-resistant membrane material of the invention has good anti-microbial property；The pollution-resistant membrane material of the present invention not only has the characteristics of hydrophobic material PVDF high temperature resistants, good mechanical performance and chemical stability, and has the hydrophilicity of styrene, the excellent combination property of film.
Description
Technical field
The invention belongs to membrane material preparing technical field more particularly to a kind of preparation methods of pollution-resistant membrane material.
Background technology
Fouling membrane normally behave as system operation for a period of time after, the flux of film declines, and producing water water quality is deteriorated.Once hair
Filming pollutes, and in order to ensure that the requirement of system water yield must just improve driving pressure, is continually backwashed, this not only increases
The operating cost of system is added, and the use of the backwash process of strong acid and strong base has been also that a kind of damaging film properties restored
Journey can shorten the service life of film.
Research finds that film surface and hydrophobicity solute and the interaction between solute ions are to cause the master of fouling membrane
Want reason.Therefore, improve membrane superficial tissue, the hydrophily and film surface of membrane material are electrically to prepare the main way of pollution-resistant membrane
Diameter.Due to mechanical performance, thermal stability and the chemical stability that Kynoar (PVDF) is excellent, and the easily properties such as film forming,
It is set to be widely used in film industry.
But Kynoar (PVDF) film surface cannot form hydrogen bond between water, show extremely strong hydrophobicity, easily
By protein contamination, development of the PVDF in seperation film application field is seriously constrained.During water process, protein is easy to
It is adsorbed on pvdf membrane surface or blocks fenestra, to reduce water flux and influence separating effect, it is most important that, gather inclined fluorine at present
The antibacterial effect of ethylene composite membrane is undesirable, seriously constrains application of the film in separation field.Therefore, a kind of comprehensive performance is prepared
Excellent pollution-resistant membrane material is of great significance.
Invention content
The defect that it is an object of the invention to overcome the antibacterial effect of prior art pvdf membrane undesirable provides a kind of anti-pollution
Contaminate the preparation method of membrane material.
The present invention provides a kind of preparation methods of pollution-resistant membrane material, include the following steps：
(1) prepared by solution：Styrene is mixed with the polymer of polyvinylidene fluoride with diluent, is thermally formed and is mixed
Liquid；
(2) membranous type is cast：Required shape will be made on homogeneous phase solution blade coating to tablet or doughnut；
(3) it post-processes：It is cooling, be separated, extracted with ethyl alcohol and remove diluent, obtain microcellular structure i.e. styrene with
The blend film of polyvinylidene fluoride；
(4) hydrophilic modifying：Blend film is immersed in Nano silver solution, pollution-resistant membrane material is obtained after dry.Nano silver is molten
Film surface formation hydrophilic antimicrobial layer is being blended in nano silver particles in liquid.Nano silver has good hydrophily and anti-microbial property,
Blend film is immersed in Nano silver solution, on the one hand can improve the hydrophily on blend membraness surface, hydrophilic improvement can
To effectively reduce organic pollution in the adherency that film surface is blended, the contamination resistance of blend film is effectively improved, on the other hand, is received
Rice silver continuously can discharge silver ion to aqueous systems, effectively improve the antibacterial ability of blend film.
Specifically, in (1), the preparation method of the polymer of styrene and polyvinylidene fluoride includes the following steps：
S1：At normal temperatures, porous glass tube is placed in hydrogen peroxide and impregnates, cleans, porous glass tube is then put into benzene
In the mixture of ethylene and polyvinylidene fluoride；
S2：Under vacuum conditions, porous glass tube dry 1-3h at 120-140 DEG C；
S3：At room temperature, catalyst, the mixture generation of styrene and polyvinylidene fluoride are added into porous glass tube
The polymer of styrene and polyvinylidene fluoride is finally made in polymerisation.
Specifically, in S1, in the mixture of styrene and polyvinylidene fluoride, styrene and polyvinylidene fluoride
Mass ratio is 1：1.
Specifically, in S3, catalyst is gaseous ammonium carbonate, and the quality of catalyst is 1mg.
Specifically, in step (1), diluent is the mixture of polyethylene glycol and polyethylene glycol oxide, polyethylene glycol with it is poly-
The volume ratio of ethylene oxide is 0.6：0.8.
Specifically, in (3), the mass percent of ethyl alcohol is 70%,
Specifically, in (4), the concentration of Nano silver solution is 100-1000mg/L, and blend film is immersed in Nano silver solution
In dip time be 10-24h.
Specifically, in (4), the preparation method of Nano silver solution includes the following steps：Under the conditions of pH value is 10-12,
The Nano silver solution being prepared by restoring silver-colored ammonia, this preparation method can reduce the reunion of nano-Ag particles.
Beneficial effects of the present invention：(1) present invention has good anti-microbial property, and to bacterium, microorganism is in membrane material table
The growth and breeding in face has significant inhibiting effect, specifically, carries out the test of antibacterial ring size to film using pseudomonas aeruginosa,
The result shows that the pollution-resistant membrane material of the present invention has good anti-microbial property；(2) present invention improves pvdf membrane hydrophily, with
The hydrophilic improvement of pvdf membrane, permeability of the membrane, resistance tocrocking and stability are preferably improved, pollution-resistant membrane material
The coverage rate on its surface is high and steady in a long-term after surface is handled by hydrophilic modifying, and pollution-resistant membrane material is not impregnated with molten in nano silver
Film pure water flux in liquid is about 100L/ (m2H), and pollution-resistant membrane material is immersed in the film pure water flux in Nano silver solution
It is 400L/ (m2H) more than, the pure water-flowing amount of film is effectively increased, the overall performance of film is improved, expand film applies model
It encloses；(3) pollution-resistant membrane material of the invention not only has hydrophobic material PVDF high temperature resistants, good mechanical performance and chemical stabilization
The characteristics of property, and have the hydrophilicity of styrene, the excellent combination property of film.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of pollution-resistant membrane material of the present invention；
Fig. 2 is the antibacterial effect figure of pollution-resistant membrane material 1 prepared by the embodiment of the present invention 1.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
A kind of preparation method of pollution-resistant membrane material (flow chart of preparation method is shown in Fig. 1), includes the following steps：
(1) prepared by solution：Styrene is mixed with the polymer of polyvinylidene fluoride with diluent, is thermally formed and is mixed
Liquid, diluent are the mixtures of polyethylene glycol and polyethylene glycol oxide, and the volume ratio of polyethylene glycol and polyethylene glycol oxide is 0.6：
0.8；
(2) membranous type is cast：Required shape will be made on homogeneous phase solution blade coating to tablet or doughnut；
(3) it post-processes：It is cooling, it is separated, is extracted with 70% ethyl alcohol and remove diluent, obtain microcellular structure i.e. benzene second
The blend film of alkene and polyvinylidene fluoride；
(4) hydrophilic modifying：Blend film is immersed in Nano silver solution, dip time is 10-24h, Nano silver solution
Concentration is 100mg/L, obtains pollution-resistant membrane material 1 after dry, the film pure water flux of pollution-resistant membrane material 1 is up to 400L/ (m2·
h)。
In (1), the preparation method of the polymer of styrene and polyvinylidene fluoride includes the following steps：
S1：At normal temperatures, porous glass tube is placed in hydrogen peroxide and impregnates, cleans, porous glass tube is then put into benzene
In the mixture of ethylene and polyvinylidene fluoride, the mass ratio of styrene and polyvinylidene fluoride is 1：1；
S2：Under vacuum conditions, porous glass tube dry 3h at 140 DEG C；
S3：At room temperature, gaseous ammonium carbonate, the mixing of styrene and polyvinylidene fluoride are added into porous glass tube
Polymerisation, the final polymer for obtaining styrene and polyvinylidene fluoride occur for object.
The preparation method of Nano silver solution, includes the following steps：Under the conditions of pH value is 10-12, by restoring silver-colored ammonia system
Standby obtained Nano silver solution.
Antibacterial effect figure such as Fig. 2 of pollution-resistant membrane material 1.
Antibacterial experiment method：The pseudomonas aeruginosa suspension for preparing 100mL first, is then cultivated in 30 DEG C of shaking tables
12 hours, draw 100 μ L suspension, with spreading rod suspension on agar plate.
Pollution-resistant membrane material 1 made from embodiment 1 is cut into the disk of a diameter of 25mm.Disk is irradiated with ultraviolet light, is shone
It is 30min or more to penetrate the time, then disk is placed in the agar plate surface for being inoculated with pseudomonas aeruginosa, at 37 DEG C
For 24 hours, discovery has antibacterial ring size phenomenon to lower heat insulating culture.Figure it is seen that foring a ratio at diaphragm and on the outside of diaphragm
It is good to illustrate that pollution-resistant membrane material produced by the present invention has for the more regular non-growth district of apparent bacterium, i.e. antibacterial ring size
Antibacterial effect.
Embodiment 2
The present embodiment and the preparation method of embodiment 1 are essentially identical, the difference is that：
Step (4) hydrophilic modifying in the preparation method of pollution-resistant membrane material：The concentration of Nano silver solution is 500mg/
L；
Step S2 in the preparation method of polymer：Under vacuum conditions, porous glass tube dry 2h at 130 DEG C；
Pollution-resistant membrane material 2 is finally made.The film pure water flux of pollution-resistant membrane material 2 is up to 410L/ (m2·h)。
Embodiment 3
The present embodiment and the preparation method of embodiment 1 are essentially identical, the difference is that：
Step (4) hydrophilic modifying in the preparation method of pollution-resistant membrane material：The concentration of Nano silver solution is 1000mg/
L；
Step S2 in the preparation method of polymer：Under vacuum conditions, porous glass tube dry 1h at 120 DEG C.
Finally obtain pollution-resistant membrane material 3.The film pure water flux of pollution-resistant membrane material 3 is up to 408L/ (m2·h)。
Comparative example
The present embodiment and the preparation method of embodiment 1 are essentially identical, the difference is that：Eliminate the hydrophilic of step (4)
It is modified.Pollution-resistant membrane material 4 is finally made.
Pollution-resistant membrane material 4 is that the film pure water flux being not impregnated in Nano silver solution is about 100L/ (m2·h).This hair
Bright pollution-resistant membrane material 1-3 films pure water flux reaches 400L/ (m2H) more than, therefore pollution-resistant membrane prepared by the present invention
Material effectively increases the pure water-flowing amount of film, improves the overall performance of film, expands the application range of film.
The above is only the section Example of the present invention, limitation in any form not done to the present invention, it is every according to
According to any simple modification that the technical spirit of the present invention makees above-described embodiment, equivalent variations and modification belong to the present invention
In technical proposal scope.
Claims (8)
1. a kind of preparation method of pollution-resistant membrane material, it is characterised in that：Include the following steps：
(1) prepared by solution：Styrene is mixed with the polymer of polyvinylidene fluoride with diluent, is thermally formed homogeneous phase solution；
(2) membranous type is cast：Required shape will be made on homogeneous phase solution blade coating to tablet or doughnut；
(3) it post-processes：It is cooling, it is separated, is extracted with ethyl alcohol and remove diluent, obtain microcellular structure i.e. styrene and gather inclined
The blend film of difluoroethylene；
(4) hydrophilic modifying：Blend film is immersed in Nano silver solution, pollution-resistant membrane material is obtained after dry.
2. the preparation method of pollution-resistant membrane material according to claim 1, it is characterised in that：In (1), styrene with it is poly-
The preparation method of the polymer of vinylidene fluoride includes the following steps：
S1：At normal temperatures, porous glass tube is placed in hydrogen peroxide and impregnates, cleans, porous glass tube is then put into styrene
With in the mixture of polyvinylidene fluoride；
S2：Under vacuum conditions, porous glass tube dry 1-3h at 120-140 DEG C；
S3：At room temperature, catalyst is added into porous glass tube, styrene polymerize with the mixture of polyvinylidene fluoride
The polymer of styrene and polyvinylidene fluoride is finally made in reaction.
3. the preparation method of pollution-resistant membrane material according to claim 2, it is characterised in that：In S1, styrene with
In the mixture of polyvinylidene fluoride, the mass ratio of styrene and polyvinylidene fluoride is 1：1.
4. the preparation method of pollution-resistant membrane material according to claim 2, it is characterised in that：In S3, catalyst is gas
The ammonium carbonate of state.
5. the preparation method of pollution-resistant membrane material according to claim 1, it is characterised in that：In step (1), diluent
It is the mixture of polyethylene glycol and polyethylene glycol oxide, the volume ratio of polyethylene glycol and polyethylene glycol oxide is 0.6：0.8.
6. the preparation method of pollution-resistant membrane material according to claim 1, it is characterised in that：In (3), the quality of ethyl alcohol
Percentage is 70%.
7. the preparation method of pollution-resistant membrane material according to claim 1, it is characterised in that：In (4), Nano silver solution
Concentration be 100-1000mg/L, it is 10-24h that blend film, which is immersed in the dip time in Nano silver solution,.
8. the preparation method of pollution-resistant membrane material according to claim 1, it is characterised in that：In (4), Nano silver solution
Preparation method, include the following steps：Under the conditions of pH value is 10-12, the Nano silver solution that is prepared by restoring silver-colored ammonia.
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Cited By (3)
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| CN110302684A (en) * | 2019-04-18 | 2019-10-08 | 宁波大学 | Antipollution forward osmosis membrane based on amination manosil AS nanotube surface adsorption of modification |
| CN110841492A (en) * | 2019-09-25 | 2020-02-28 | 长春工业大学 | Preparation method of nano-silver modified polytetrafluoroethylene microporous membrane for membrane distillation |
| CN115055208A (en) * | 2022-06-24 | 2022-09-16 | 安庆市长三角未来产业研究院 | Preparation method of two-phase flow catalytic membrane, two-phase flow catalytic membrane and application thereof |
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| CN115055208A (en) * | 2022-06-24 | 2022-09-16 | 安庆市长三角未来产业研究院 | Preparation method of two-phase flow catalytic membrane, two-phase flow catalytic membrane and application thereof |
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