CN109092068A - A kind of ultrafiltration membrane preparation method - Google Patents
A kind of ultrafiltration membrane preparation method Download PDFInfo
- Publication number
- CN109092068A CN109092068A CN201811171442.7A CN201811171442A CN109092068A CN 109092068 A CN109092068 A CN 109092068A CN 201811171442 A CN201811171442 A CN 201811171442A CN 109092068 A CN109092068 A CN 109092068A
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- ultrafiltration membrane
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- membrane preparation
- forming plates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- 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
- B01D67/0006—Organic membrane manufacture by chemical reactions
-
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention proposes a kind of ultrafiltration membrane preparation methods, graft modification is carried out to polyether sulfone as modified material using methacrylic acid, especially by polyether sulfone, N, dinethylformamide and the stirring of metering system acid dissolution, and the mode of logical irradiation carries out graft modification, modified poly (ether-sulfone) ultrafiltration membrane is obtained, which there is good contamination resistance and hydrophily to be improved.
Description
Technical field
The present invention relates to separation membrane technical field more particularly to a kind of ultrafiltration membrane preparation methods.
Background technique
Membrane separation technique is a kind of current new separation technology, with easy to operate, efficient and low-energy-efficiency protrusion
Advantage is widely used in water resource utilization, the depollution of environment, food production and biological medicine preparation field.
Ultrafiltration Membrane be using ultrafiltration membrane as filter medium, under pressure, feed liquid contact membranes table to be processed
When face, only water and the small-molecule substance smaller than membrane aperture is allowed to pass through.However due to ultrafiltration membrane material or the shadow of its structure
It rings, ultrafiltration membrane in the long-term use process, is all inevitably contaminated, and pollution problem will lead to the flux of ultrafiltration membrane
With separating property sharp fall, increase use cost.
It at present using polysulfones as ultrafiltration membrane material, is avoided pollution by addition antibacterial agent, common antibacterial agent includes gold
Belong to and metal nanoparticle, quaternary ammonium salt, the bacteriostatic agent containing metal or Jinsha lake nanoparticle are easy stream in use
It loses, anti-microbial property declines and causes damages to environment.Failure, antibiotic property are easy after antibacterial agent long-time use containing quaternary ammonium salt
It can reduce.
Summary of the invention
In view of this, the invention proposes it is a kind of can long-term antipollution, good hydrophilic property ultrafiltration membrane preparation method.
The technical scheme of the present invention is realized as follows: the present invention provides a kind of ultrafiltration membrane preparation method, including it is as follows
Preparation step:
Step 1: polyether sulfone, n,N-Dimethylformamide, methacrylic acid are uniformly mixed by following mass percents,
Obtain homogeneous mixed solution；
Polyether sulfone 10%
N,N-Dimethylformamide 88%~89%
Methacrylic acid 1%~2%
Step 2: homogeneous mixed solution obtained in step 1 is placed in irradiation devices, nitrogen is passed through into irradiation devices
Gas is irradiated 15~20 hours with the radiation parameter that dose of radiation is 1~30Kgy/h, obtains grafting crude product；
It is stood Step 3: the grafting crude product in step 2 is placed in deionized water, filters, obtain after standing 12~36 hours
To much filtrate, much filtrate is dried at a temperature of 50~80 DEG C obtains dry much filtrate, and the dry much filtrate is grafting finished product；
Step 3: by quality ratio, much filtrate: solvent: additive=(5-25): (30-85): the ratio of (2-30) will be dried
Example feeds intake, and stirs under the conditions of 50~80 DEG C to being uniformly dissolved, obtains casting solution；
Step 4: the casting solution in step 3 is applied on film-forming plates, and film-forming plates are immersed in coagulation bath, are impregnated
Time is 5~10min, and immersion finishes to obtain graft modification of polyethersulfone ultrafiltration membrane.
On the basis of above technical scheme, it is preferred that in step 1, the uniformly mixed step includes:
Dry polyether sulfone solid powder is put into n,N-Dimethylformamide solvent, 50~70 DEG C is heated to, stirs
Dissolution is mixed, dissolution, which is finished, is cooled to 20~30 DEG C for solution, methacrylic acid monomer is put into solution to cooling down, stirring and dissolving,
Obtain homogeneous mixed solution.
On the basis of above technical scheme, it is preferred that in step 3, the solvent is n,N-Dimethylformamide, N-
One of methyl pyrrolidone or n,N-dimethylacetamide or a variety of mixtures.
On the basis of above technical scheme, it is preferred that in step 3, the additive be methanol, ethyl alcohol, ethylene glycol,
One of polyethylene glycol-400, polyvinyl alcohol -200, diethylene glycol (DEG), triethylene glycol or three polyglycereol or a variety of mixtures.
Still more preferably, in step 4, the coagulation bath is deionized water or tap water.
On the basis of above technical scheme, it is preferred that the step 4 further includes carrying out to the film-forming plates that immersion finishes
Concussion operation, ultrafiltration membrane fall off from film-forming plates by concussion operation.
A kind of ultrafiltration membrane preparation method of the invention has the advantages that compared with the existing technology
A kind of ultrafiltration membrane preparation method of the invention is modified polyether sulfone strand by the way of irradiation grafting, warp
It crosses the resistant to pollution performance of modified poly (ether-sulfone) ultrafiltration membrane to greatly promote, while also being obtained by modified ultrafiltration membrane hydrophily
It improves, and the modified monomer that the present invention selects has certain sensibility to temperature and pH value after polymerisation, makes the present invention
The ultrafiltration membrane that preparation method prepares can work well under different temperatures and different pH environment.
Specific embodiment
Below in conjunction with embodiment of the present invention, the technical solution in embodiment of the present invention is carried out clearly and completely
Description, it is clear that described embodiment is only some embodiments of the invention, rather than whole embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all
Other embodiments shall fall within the protection scope of the present invention.
Embodiment 1
100g polyether sulfone is put into 880gN, in dinethylformamide solvent, is heated to 50 DEG C, stirring and dissolving, dissolution
It finishes, water cooling puts into 20g methacrylic acid monomer into solution after cooling to 20 DEG C, and stirring and dissolving is mixed molten
Homogeneous mixed solution is placed in irradiation devices and summarized by liquid, keeps nitrogen atmosphere in irradiation devices, is irradiated 15 hours with 1Kgy/h,
Grafting crude product is obtained, grafting crude product is placed in deionized water 12 hours, is filtered, much filtrate is dried at 50 °C, weighed
Much filtrate 5g after drying, is added to 30gN, in dinethylformamide solvent, adds 2g methanol, while being warming up to 50 DEG C
Stirring and dissolving obtains casting solution, and casting solution is applied on film-forming plates with 200um scraper, and film-forming plates are impregnated just in water-bath
In, 5min is impregnated, concussion impregnates the film-forming plates finished, obtains graft modification of polyethersulfone ultrafiltration membrane.
Embodiment 2
100g polyether sulfone is put into 882gN, in dinethylformamide solvent, is heated to 55 DEG C, stirring and dissolving, dissolution
It finishes, water cooling puts into 18g methacrylic acid monomer into solution after cooling to 22 DEG C, and stirring and dissolving is mixed molten
Homogeneous mixed solution is placed in irradiation devices and summarized by liquid, keeps nitrogen atmosphere in irradiation devices, is irradiated 16 hours with 5Kgy/h,
Grafting crude product is obtained, grafting crude product is placed in deionized water 18 hours, is filtered, much filtrate is dried at a temperature of 55 DEG C, weighed
Much filtrate 10g after drying, is added in 40g N-Methyl pyrrolidone, adds 10g ethyl alcohol, while being warming up to 55 DEG C of stirrings
Dissolution, obtains casting solution, casting solution is applied on film-forming plates with 200um scraper, and film-forming plates are impregnated leaching just in a water bath
6min is steeped, concussion impregnates the film-forming plates finished, obtains graft modification of polyethersulfone ultrafiltration membrane.
Embodiment 3
100g polyether sulfone is put into 884gN, in dinethylformamide solvent, is heated to 60 DEG C, stirring and dissolving, dissolution
It finishes, water cooling puts into 16g methacrylic acid monomer into solution after cooling to 24 DEG C, and stirring and dissolving is mixed molten
Homogeneous mixed solution is placed in irradiation devices and summarized by liquid, keeps nitrogen atmosphere in irradiation devices, is irradiated 17 hours with 10Kgy/h,
Grafting crude product is obtained, grafting crude product is placed in deionized water 24 hours, is filtered, much filtrate is dried at a temperature of 60 DEG C, weighed
Much filtrate 15g after drying, is added to 50gN, in N- dimethylacetamide solvent, adds 15g ethylene glycol, is warming up to simultaneously
65 DEG C of stirring and dissolvings, obtain casting solution, and casting solution is applied on film-forming plates with 200um scraper, and film-forming plates are impregnated
In water-bath, 7min is impregnated, concussion impregnates the film-forming plates finished, obtains graft modification of polyethersulfone ultrafiltration membrane.
Embodiment 4
100g polyether sulfone is put into 886gN, in dinethylformamide solvent, is heated to 65 DEG C, stirring and dissolving, dissolution
It finishes, water cooling puts into 14g methacrylic acid monomer into solution after cooling to 26 DEG C, and stirring and dissolving is mixed molten
Homogeneous mixed solution is placed in irradiation devices and summarized by liquid, keeps nitrogen atmosphere in irradiation devices, is irradiated 18 hours with 20Kgy/h,
Grafting crude product is obtained, grafting crude product is placed in deionized water 30 hours, is filtered, much filtrate is dried at a temperature of 70C, weighs baking
Much filtrate 20g after dry, is added to 65gN, in dinethylformamide solvent, adds 25g diethylene glycol (DEG), while being warming up to 75
DEG C stirring and dissolving, obtains casting solution, casting solution is applied on film-forming plates with 200um scraper, and film-forming plates are impregnated just in water
In bath, 8min is impregnated, concussion impregnates the film-forming plates finished, obtains graft modification of polyethersulfone ultrafiltration membrane.
Embodiment 5
100g polyether sulfone is put into 890gN, in dinethylformamide solvent, is heated to 70 DEG C, stirring and dissolving, dissolution
It finishes, water cooling puts into 10g methacrylic acid monomer into solution after cooling to 30 DEG C, and stirring and dissolving is mixed molten
Homogeneous mixed solution is placed in irradiation devices and summarized by liquid, keeps nitrogen atmosphere in irradiation devices, is irradiated 20 hours with 30Kgy/h,
Grafting crude product is obtained, grafting crude product is placed in deionized water 36 hours, is filtered, much filtrate is dried at a temperature of 80 DEG C, weighed
Much filtrate 25g after drying, is added in 85g N-Methyl pyrrolidone, adds tri- polyglycereol of 35g, while being warming up to 80 DEG C
Stirring and dissolving obtains casting solution, and casting solution is applied on film-forming plates with 200um scraper, and film-forming plates are impregnated just in water-bath
In, 10min is impregnated, concussion impregnates the film-forming plates finished, obtains graft modification of polyethersulfone ultrafiltration membrane.
It is 35.3cm that the graft modification of polyethersulfone ultrafiltration membrane prepared in above embodiments, which is cut into effective area,2Original
Piece filters evaluation system by film and carries out test evaluation, the film table of system is set as 2kg/h, film surface pressure to water flow velocity
Penetrating fluid is then changed to by the BSA grafting solution of concentration 500ppm, identical to ultrafiltration membrane precompressed 20min for 0.5bar
It is tested under flow velocity and pressure condition.
The foregoing is merely better embodiments of the invention, are not intended to limit the invention, all of the invention
Within spirit and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of ultrafiltration membrane preparation method, including following preparation step:
Step 1: polyether sulfone, n,N-Dimethylformamide, methacrylic acid are uniformly mixed by following mass percents, obtain
Homogeneous mixed solution；
Polyether sulfone 10%
N,N-Dimethylformamide 88%~89%
Methacrylic acid 1%~2%
Step 2: homogeneous mixed solution obtained in step 1 is placed in irradiation devices, nitrogen is passed through into irradiation devices, with
The radiation parameter that dose of radiation is 1~30Kgy/h irradiates 15~20 hours, obtains grafting crude product；
It is stood Step 3: the grafting crude product in step 2 is placed in deionized water, filters, filtered after standing 12~36 hours
Object out, much filtrate is dried at a temperature of 50~80 DEG C obtains dry much filtrate, and the dry much filtrate is grafting finished product；
Step 3: by quality ratio, by dry much filtrate: solvent: additive=(5-25): (30-85): the ratio of (2-30) is thrown
Material, stirs to being uniformly dissolved under the conditions of 50~80 DEG C, obtains casting solution；
It is immersed in coagulation bath on film-forming plates, and by film-forming plates Step 4: scratching the casting solution in step 3, soaking time
For 5~10min, immersion finishes to obtain graft modification of polyethersulfone ultrafiltration membrane.
2. a kind of ultrafiltration membrane preparation method as described in claim 1, which is characterized in that described uniformly mixed in step 1
Step includes:
Dry polyether sulfone solid powder is put into n,N-Dimethylformamide solvent, is heated to 50~70 DEG C, is stirred molten
Solution, dissolution, which is finished, is cooled to 20~30 DEG C for solution, puts into methacrylic acid monomer into cooling solution, stirring and dissolving obtains
Homogeneous mixed solution.
3. a kind of ultrafiltration membrane preparation method as described in claim 1, which is characterized in that in step 3, the solvent is N, N-
One of dimethylformamide, N-Methyl pyrrolidone or n,N-dimethylacetamide or a variety of mixtures.
4. a kind of ultrafiltration membrane preparation method as described in claim 1, which is characterized in that in step 3, the additive is first
One of alcohol, ethyl alcohol, ethylene glycol, polyethylene glycol-400, polyvinyl alcohol -200, diethylene glycol (DEG), triethylene glycol or three polyglycereol are more
The mixture of kind.
5. a kind of ultrafiltration membrane preparation method as described in claim 1, which is characterized in that in step 4, the coagulation bath is to go
Ionized water or tap water.
6. a kind of ultrafiltration membrane preparation method as described in claim 1, which is characterized in that the step 4 further includes to having impregnated
Complete film-forming plates carry out concussion operation, and ultrafiltration membrane falls off from film-forming plates by concussion operation.
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Cited By (2)
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| CN110548422A (en) * | 2019-08-27 | 2019-12-10 | 武汉艾科滤膜技术有限公司 | Organic solvent-resistant ultrafiltration membrane and preparation method and application thereof |
| CN111729516A (en) * | 2020-06-10 | 2020-10-02 | 清华大学 | Hydrophilic modified ultrafiltration membrane and preparation method thereof |
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| CN111729516A (en) * | 2020-06-10 | 2020-10-02 | 清华大学 | Hydrophilic modified ultrafiltration membrane and preparation method thereof |
| CN111729516B (en) * | 2020-06-10 | 2021-08-20 | 清华大学 | Hydrophilic modified ultrafiltration membrane and preparation method thereof |
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Application publication date: 20181228 |