CN109647228A - The polychloroethylene blended ultrafiltration membrane of lignin-and preparation method - Google Patents
The polychloroethylene blended ultrafiltration membrane of lignin-and preparation method Download PDFInfo
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- CN109647228A CN109647228A CN201811597902.2A CN201811597902A CN109647228A CN 109647228 A CN109647228 A CN 109647228A CN 201811597902 A CN201811597902 A CN 201811597902A CN 109647228 A CN109647228 A CN 109647228A
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- lignin
- polyvinyl chloride
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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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
-
- 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
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- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of polychloroethylene blended ultrafiltration membrane of lignin-and preparation method, include the following steps: that dry lignin 1) is taken to be added in solvent, interval is ultrasonically treated；2) dry polyvinyl chloride is added in the solution obtained to step 1), stirs, dissolves polyvinyl chloride；Perforating agent is added in the solution obtained to step 2), interval ultrasound continues to stir；Standing and defoaming obtains casting film sol solutions；4) membrane equipment is used, casting film sol solutions are painted into plate or are drawn into doughnut, is placed, is placed in water immersion, obtains the polychloroethylene blended ultrafiltration membrane of lignin-.The invention has the advantages that the present invention passes through enhancing mass and heat transfer means during preparing casting film sol solutions, lignin and polyvinyl chloride is enable to mix.Lignin is easy to get, at low cost, and includes a large amount of hydrophilic radical, can improve the hydrophily and anti-fouling performance of Pvc Ultrafiltration Membrane；Membrane flux is big, and processing pure water flux is big, and the flux for handling oily waste water is big.
Description
Technical field
The polychloroethylene blended ultrafiltration membrane of lignin-and preparation method are used the present invention relates to a kind of, belongs to the preparation of blend film
Technology.
Background technique
Ultrafiltration is a kind of novel isolation technics, using film as medium, passes through the screening in aperture under the driving of pressure
Effect achievees the purpose that separation.Since ultrafiltration is energy saving without phase transformation in operation, the driving effect of pressure is relied solely on
It realizes separation and is widely used in every field.In the practical application of ultrafiltration membrane the problem of inevitably fouling membrane.
Fouling membrane is the meetings such as micella, suspended particulate substance and microorganism when ultrafiltration membrane realizes material concentration, separation process, in material
The interaction such as physics, chemistry is spontaneously generated with film surface, causes the absorption of film surface pollutant and the blocking of fenestra road, so that
The feed liquid flux and separating property of ultrafiltration membrane are affected.Pollution of Ultrafiltration Membrane phenomenon mainly due to pollutant and film surface it
Between interaction caused by, including hydrophobic effect, electrostatic interaction etc..The preparation main target of antipollution ultrafiltration membrane is exactly
Weaken the adherency of these active force contaminant restrainings.
Film properties and film material of main part itself close relation, choosing suitable film material of main part is the premise for preparing ultrafiltration membrane
And key.Preparing the common high molecular material of ultrafiltration membrane has polyacrylonitrile, polysulfones, Kynoar etc..Wherein, polyvinyl chloride
(PVC) there is good acid-proof alkaline, resistant to chemical etching, anti-flammability and weatherability, the advantages that especially its is cheap,
Therefore in the ultrafiltration membrane field in China, there are biggish markets.But pvc material is hydrophobic material, as previously mentioned, will cause
Pollutant influences its performance because of the precipitation adsorption of hydrophobic forces, limits its use.It is main for the method for modifying of PVC material
There is blending and modifying, modification by copolymerization and surface are modified etc..Currently, numerous studies are dedicated to for amphiphilic macromolecular additive being added
Into PVC, due to its amphiphilic nature, can either ensure that has certain compatibility with film material of main part, and can pass through tune
Various parameters enable the function segment of amphiphilic macromolecular additive to move to film surface in restraining membrane process, utmostly
Improve the performance of film.But the preparation process of amphiphilic macromolecular is tediously long, and synthesis step is complicated, with high costs, limits it further
Application.
Summary of the invention
The purpose of the present invention is overcoming the deficiencies of the prior art and provide a kind of hydrophilic, anti-pollution, flux is biggish wooden
Element-polychloroethylene blended ultrafiltration membrane.
A second object of the present invention is to provide a kind of preparation sides of polychloroethylene blended ultrafiltration membrane of lignin-at low cost
Method.
Technical solution of the present invention is summarized as follows:
A kind of preparation method of the polychloroethylene blended ultrafiltration membrane of lignin-, includes the following steps:
1) dry lignin is taken to be added in solvent, under conditions of 80~260W, 30~80 DEG C, interval is ultrasonically treated altogether
0.5~5h；
2) dry polyvinyl chloride is added in the solution obtained to step 1), stirs, dissolves polyvinyl chloride；It is described wooden
The plain mass ratio with the polyvinyl chloride is 1:2~20；The quality sum and solvent of the lignin and the polyvinyl chloride
Mass ratio is 1:5~8；
3) perforating agent is added in the solution obtained to step 2), in 90~150W, 40~80 DEG C of interval ultrasound 0.5~
4h continues 10~15h of stirring；10~72h of standing and defoaming obtains casting film sol solutions；The lignin and the polyvinyl chloride
The mass ratio of quality sum and perforating agent is 1:0.1~0.8；
4) membrane equipment is used, the casting film sol solutions are painted into plate or are drawn into doughnut, places 5~100s,
It is placed in 20~80 DEG C of water, impregnates 24-48 hours, obtain the polychloroethylene blended ultrafiltration membrane of lignin-.
The dry condition of lignin selects choosing: in 50~100 DEG C of at a temperature of dry 2~12h.
Solvent is preferred: tetrahydrofuran, dimethylformamide, n-methyl-2-pyrrolidone, acetone, N, N- dimethylacetamide
Amine or dimethyl sulfoxide.
Preferably, step 1) interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min.
Preferably, the degree of polymerization 800 of polyvinyl chloride.
The drying condition of polyvinyl chloride is preferred: in 40~100 DEG C of at a temperature of dry 2~12h.
Perforating agent is preferably polyethylene glycol 200, cetomacrogol 1000, polyvinylpyrrolidone, lithium chloride or polyethylene glycol
2000。
Preferably, step 3) interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min.
A kind of polychloroethylene blended ultrafiltration membrane of lignin-of above method preparation.
The invention has the advantages that
1. the present invention, by enhancing mass and heat transfer means, makes lignin and polychlorostyrene second during preparing casting film sol solutions
Alkene can mix.
2. lignin is easy to get, at low cost, and includes a large amount of hydrophilic radical, Pvc Ultrafiltration Membrane can be effectively improved
Hydrophily and anti-fouling performance；
3. membrane flux is big, the processing pure water flux at 0.1MPa reaches 387.56L/ (m2H), oily waste water is handled
Flux reaches 186.55L/ (m2·h)。
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) cross-section diagram of polyvinyl chloride (PVC) ultrafiltration membrane made from embodiment 1.
Fig. 2 is the SEM cross-section diagram of the polychloroethylene blended ultrafiltration membrane of lignin-prepared by embodiment 2.
Fig. 3 is the SEM exterior view of the polychloroethylene blended ultrafiltration membrane of lignin-prepared by embodiment 2.
Fig. 4 is the surface partial size statistical chart of the polychloroethylene blended ultrafiltration membrane of lignin-prepared by embodiment 2.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
Embodiment 1 (control):
The preparation of polyvinyl chloride (PVC) ultrafiltration membrane:
Taking the degree of polymerization is that 800 polyvinyl chloride (PVC) powder is put into vacuum oven, is continuously done under conditions of 80 DEG C
Dry 14h.The tetrahydrofuran (THF) of polyvinyl chloride and 50mL after taking 13g dry is added in three-necked flask, in 85 DEG C of temperature
Under, the ultrasonic agitation 40min of 170r/min is heated to reflux and is completely dissolved polyvinyl chloride powder, adds the polyethylene glycol of 2mL
1000 (PEG1000) continue to stir and reflux 12h, standing and defoaming 30h are painted the colloidal sol prepared flat using membrane equipment
Plate is placed 40s, is placed in 60 DEG C of water, impregnates 36 hours, obtains polyvinyl chloride (PVC) ultrafiltration membrane.
After tested, polyvinyl chloride (PVC) ultrafiltration membrane thickness be 0.124mm, porosity 78.0%, average pore size 16.7nm,
101.73 ° of water contact angle, the processing pure water flux 105.60L/ (m at 0.1MPa2H), the flux of oily waste water is handled
50.06L/(m2H), oily rejection is 55.06%.
Embodiment 2
A kind of preparation method of the polychloroethylene blended ultrafiltration membrane of lignin-, includes the following steps:
1) dry lignin is taken to be added in tetrahydrofuran, under conditions of 150W, 50 DEG C, interval is ultrasonically treated total 3h；
Wherein: the dry condition of lignin is the at a temperature of dry 8h at 80 DEG C；
Interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min；
2) dry 800 polyvinyl chloride of the degree of polymerization is added in the solution obtained to step 1), stirs, keeps polyvinyl chloride molten
Solution；The mass ratio of the lignin and the polyvinyl chloride is 1:10；The quality sum and solvent of lignin and polyvinyl chloride
Mass ratio is 1:6；
Wherein: the drying condition of polyvinyl chloride is the at a temperature of dry 8h at 80 DEG C；
3) cetomacrogol 1000 is added in the solution obtained to step 2), continues to stir in 120W, 60 DEG C of interval ultrasound 2h
Mix 12h；Standing and defoaming 48h obtains casting film sol solutions；The quality sum and polyethylene glycol of the lignin and the polyvinyl chloride
1000 mass ratio is 1:0.5；
Interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min；
4) membrane equipment is used, the casting film sol solutions are painted into plate, 50s is placed, is placed in 60 DEG C of water, impregnate 36
Hour, obtain the polychloroethylene blended ultrafiltration membrane of lignin-.
The polychloroethylene blended ultrafiltration membrane thickness of the lignin-being prepared after tested is 0.121mm, and porosity is
89.2%, average pore size 22.8nm, handle pure water flux 387.56L/ (m at 0.1MPa by 45.62 ° of water contact angle2H), locate
Manage the flux 186.55L/ (m of oily waste water2H), oily rejection is 99.12%.
Embodiment 3
A kind of preparation method of the polychloroethylene blended ultrafiltration membrane of lignin-, includes the following steps:
1) dry lignin is taken to be added in dimethylformamide, under conditions of 80W, 80 DEG C, interval is ultrasonically treated altogether
5h；
Wherein: the dry condition of lignin is the at a temperature of dry 12h at 50 DEG C；
Interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min；
2) dry 800 polyvinyl chloride of the degree of polymerization is added in the solution obtained to step 1), stirs, keeps polyvinyl chloride molten
Solution；The mass ratio of the lignin and the polyvinyl chloride is 1:2；The quality sum of the lignin and the polyvinyl chloride with
The mass ratio of dimethylformamide is 1:5；
Wherein: the drying condition of polyvinyl chloride is the at a temperature of dry 12h at 40 DEG C；
3) polyethylene glycol 200 is added in the solution obtained to step 2), continues to stir in 90W, 80 DEG C of interval ultrasound 4h
10h；Standing and defoaming 10h obtains casting film sol solutions；The quality sum and polyethylene glycol of the lignin and the polyvinyl chloride
200 mass ratio is 1:0.1；
Interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min；
4) membrane equipment is used, the casting film sol solutions are painted into plate, 5s is placed, is placed in 20 DEG C of water, impregnate 48
Hour, obtain the polychloroethylene blended ultrafiltration membrane of lignin-.
The polychloroethylene blended ultrafiltration membrane thickness of the lignin-being prepared after tested is 0.132mm, and porosity is
80.1%, average pore size 19.7mm, handle pure water flux 260.51L/ (m at 0.1MPa by 54.10 ° of water contact angle2H), locate
Manage the flux 88.66L/ (m of oily waste water2H), oily rejection is 86.95%.
It is demonstrated experimentally that substituting the dimethyl methyl in the present embodiment with acetone, n,N-dimethylacetamide or dimethyl sulfoxide
Amide, other same the present embodiment, the property of the polychloroethylene blended ultrafiltration membrane of the lignin-of preparation and the lignin-of the present embodiment
Polychloroethylene blended ultrafiltration membrane is similar.
It is demonstrated experimentally that the polyethylene glycol 200 in the present embodiment is substituted with lithium chloride or polyethylene glycol 2000, it is other with this reality
Apply example, the polychloroethylene blended ultrafiltration of lignin-of the property and the present embodiment of the polychloroethylene blended ultrafiltration membrane of the lignin-of preparation
Film is similar.
Embodiment 4
A kind of preparation method of the polychloroethylene blended ultrafiltration membrane of lignin-, includes the following steps:
1) dry lignin is taken to be added in n-methyl-2-pyrrolidone, under conditions of 260W, 30 DEG C, interval ultrasound
Handle total 0.5h；
Wherein: the dry condition of lignin is the at a temperature of dry 2h at 100 DEG C；
Interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min；
2) dry 800 polyvinyl chloride of the degree of polymerization is added in the solution obtained to step 1), stirs, keeps polyvinyl chloride molten
Solution；The mass ratio of the lignin and the polyvinyl chloride is 1:20；The quality sum of the lignin and the polyvinyl chloride
Mass ratio with n-methyl-2-pyrrolidone is 1:8；
Wherein: the drying condition of polyvinyl chloride is the at a temperature of dry 2h at 100 DEG C；
3) polyvinylpyrrolidone is added in the solution obtained to step 2), in 150W, 40 DEG C of interval ultrasound 0.5h, after
Continuous stirring 15h；Standing and defoaming 72h obtains casting film sol solutions；The quality sum and poly- second of the lignin and the polyvinyl chloride
The mass ratio of alkene pyrrolidone is 1:0.8；
Interval ultrasound, sets ultrasonic time as 5min, intermittent time 1min；
4) membrane equipment is used, the casting film sol solutions are drawn into doughnut, 100s is placed, is placed in 80 DEG C of water
In, it impregnates 24 hours, obtains the polychloroethylene blended ultrafiltration membrane of lignin-.
The polychloroethylene blended ultrafiltration membrane thickness of the lignin-being prepared after tested is 0.155mm, and porosity is
85.2%, average pore size 20.1nm, handle pure water flux 355.37L/ (m at 0.1MPa by 50.26 ° of water contact angle2H), locate
Manage the flux 132.45L/ (m of oily waste water2H), oily rejection is 91.06%.
Claims (9)
1. a kind of preparation method of the polychloroethylene blended ultrafiltration membrane of lignin-, it is characterized in that including the following steps:
1) dry lignin is taken to be added in solvent, under conditions of 80~260W, 30~80 DEG C, interval ultrasonic treatment totally 0.5
~5h；
2) dry polyvinyl chloride is added in the solution obtained to step 1), stirs, dissolves polyvinyl chloride；The lignin with
The mass ratio of the polyvinyl chloride is 1:2~20；The lignin and the quality sum of the polyvinyl chloride and the quality of solvent
Than for 1:5~8；
3) perforating agent is added in the solution obtained to step 2), in 90~150W, 40~80 DEG C of interval 0.5~4h of ultrasound, after
10~15h of continuous stirring；10~72h of standing and defoaming obtains casting film sol solutions；The quality of the lignin and the polyvinyl chloride it
With with the mass ratio of perforating agent be 1:0.1~0.8；
4) membrane equipment is used, the casting film sol solutions are painted into plate or are drawn into doughnut, 5~100s is placed, is placed in
In 20~80 DEG C of water, impregnates 24-48 hours, obtain the polychloroethylene blended ultrafiltration membrane of lignin-.
2. according to the method described in claim 1, it is characterized in that the condition of lignin drying is the temperature at 50~100 DEG C
2~12h of lower drying.
3. according to the method described in claim 1, it is characterized in that the solvent is tetrahydrofuran, dimethylformamide, N- methyl-
2-Pyrrolidone, acetone, DMAC N,N' dimethyl acetamide or dimethyl sulfoxide.
4. according to the method described in claim 1, it is characterized in that step 1) interval ultrasound, ultrasonic time is set as 5min,
Intermittent time 1min.
5. according to the method described in claim 1, it is characterized in that the degree of polymerization 800 of polyvinyl chloride.
6. according to the method described in claim 1, it is characterized in that the drying condition of the polyvinyl chloride is the temperature at 40~100 DEG C
The lower dry 2~12h of degree.
7. according to the method described in claim 1, it is characterized in that the perforating agent is polyethylene glycol 200, cetomacrogol 1000, gathers
Vinylpyrrolidone, lithium chloride or polyethylene glycol 2000.
8. according to the method described in claim 1, it is characterized in that step 3) interval ultrasound, ultrasonic time is set as 5min,
Intermittent time 1min.
9. the polychloroethylene blended ultrafiltration membrane of a kind of lignin-prepared by the method for one of claim 1-8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114618319A (en) * | 2022-03-15 | 2022-06-14 | 常州大学 | PVDF film with long-term antibacterial and anti-pollution performance and preparation method thereof |
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