CN107899431A - The preparation method of the positive osmosis composite membrane of zirconium metal-organic framework materials modified polyamide - Google Patents
The preparation method of the positive osmosis composite membrane of zirconium metal-organic framework materials modified polyamide Download PDFInfo
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- CN107899431A CN107899431A CN201711259016.4A CN201711259016A CN107899431A CN 107899431 A CN107899431 A CN 107899431A CN 201711259016 A CN201711259016 A CN 201711259016A CN 107899431 A CN107899431 A CN 107899431A
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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
- B01D61/002—Forward osmosis or direct osmosis
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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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
- B01D71/56—Polyamides, e.g. polyester-amides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/46—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2323/00—Details relating to membrane preparation
- B01D2323/50—Control of the membrane preparation process
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Abstract
The present invention discloses a kind of preparation method of the positive osmosis composite membrane of zirconium metal-organic framework materials modified polyamide, comprises the following steps：（1）Zirconium chloride, deionized water, propionic acid, fumaric acid are mixed, filtered, is washed, centrifugation, obtains zirconium metal-organic framework materials；（2）By N, N dimethylacetylamides, polyethylene glycol 400 and deionized water mixing, add polysulfones, obtain polysulfones casting solution；（3）Polysulfones casting solution microwave is heated, knifing, soaks in water, obtains polysulfones basement membrane；（4）M-phenylenediamine solution and sodium dodecyl sulfate solution are mixed, obtain aqueous phase solution；Pyromellitic trimethylsilyl chloride, zirconium metal-organic framework materials are added in n-hexane, ultrasonic disperse, obtains organic phase solution；（5）The single side of polysulfones basement membrane is immersed in aqueous phase solution, then the two sides of polysulfones basement membrane is all immersed in organic phase solution；（6）Film is dried.Forward osmosis membrane good hydrophilic property, the separating property being prepared are good.
Description
Technical field
The invention belongs to technical field of membrane, and in particular to a kind of zirconium-metal-organic framework materials modified polyamide just permeates
The preparation method of composite membrane.
Background technology
With water resources shortage and the getting worse of lack of energy problem, more pure water are obtained with lower energy consumption
Isolation technics is by as main water process pattern.Forward osmosis membrane (FO), as a kind of emerging membrane separation technique, several recently
Nian Li, has caused the interest of more and more researchers.Positive process of osmosis is by drawing between liquid and material liquid
Pure water in osmotic pressure official post material liquid, which enters, to be drawn in liquid, rather than the external liquid used in reverse osmosis or nanofiltration process
Pressure, is compared to reverse osmosis (RO) technology of high drive, and FO has the advantages that energy consumption is low, fouling membrane is small, Water Sproading rate is high.Mesh
Before, that most forward osmosis membrane uses is all polyamide composite film (TFC), and this composite membrane is in plate membrane and hollow-fibre membrane
In have and widely apply.Composite membrane is made of porous support layer and active layer two parts, and active layer is generally by interface
It polymerize the polyamide formed.Due to the sandwich construction of composite membrane, make it have cellulose acetate film without flexibility, active layer
It can be modified respectively with the chemical property of supporting layer.Now, since composite membrane is anisotropic membrane, it is remote that it tests water flux
Less than predicted value, the water flux for improving positive osmosis composite membrane is the essential condition for expanding its application range.
In the method for numerous positive osmosis composite membrane performances of improvement, addition nano particle forms polyamide nano composite membrane
(TFN) it is that operation sequence is simple and water flux improves the big method of degree.According to nano particle in composite membrane point of addition
Difference, the principle of its raising water flux is also different, is broadly divided into two parts:（1）It is added in basement membrane, effectively reduces interior dense
Poor polarization phenomena;（2）It is added in surface-active layer, improves the hydrophily of film surface.In recent years, the nano particle master used
Have:Titanium dioxide, silica, graphene oxide etc..Studies have found that add graphene oxide into positive osmosis composite membrane
Aramid layer in, water flux can be made to increase to original 1.5-2 times.
Metal-organic framework materials (MOF) are the hot spots of investigation of materials in recent years.Metal-organic framework materials are that height is tied
Brilliant porous material, it by metal ion or metal cluster be node that it, which is, is matched somebody with somebody with the three-dimensional structure of rigid organic ligand composition
Position compound.Since the aperture of MOF can be compared to other nanometers by controlling the length of connector molecule to be adjusted
Material, it is widely applied with many chemical properties, such as absorb, be catalyzed etc..
Zirconium-metal-organic framework materials（Zr-MOF）It is initially to be synthesized by solvent of n,N-Dimethylformamide, but obtains
Product there is hydrophobicity, and whole building-up process, when industrialized production, can cause ring due to the use of substantial amounts of organic solvent
Pollute in border.
The content of the invention
The defects of for the prior art, the present invention provide a kind of zirconium-metal-organic framework materials modified polyamide and just permeate
The preparation method of composite membrane, the forward osmosis membrane separating property being prepared are good.
The preparation method of zirconium-positive osmosis composite membrane of metal-organic framework materials modified polyamide, comprises the following steps：
（1）By zirconium chloride, deionized water, propionic acid, fumaric acid proportionally 0.12g:10mL:2.68g:0.18g is mixed,
It is subsequently placed at 120 DEG C and reacts 24-30h, cooled to room temperature, filtering, washs 3 times, so respectively with deionized water and methanol
After centrifuge, sediment is placed into 24h at normal temperatures, obtains zirconium-metal-organic framework materials；
（2）It is 74 in mass ratio by n,N-dimethylacetamide, polyethylene glycol 400 and deionized water:8:0.5 mixing, stirring,
Then polysulfones is added, 24h is stirred at 65 DEG C, cooling 24h is then stood, obtains polysulfones casting solution；
（3）Polysulfones casting solution microwave is heated into 10min, then carries out knifing on a glass, the thickness of film is 65 ± 5 μm, quiet
30s is put, stands 5-10min into the water, film is taken off from glass plate, then soaks 24h in deionized water, obtains polysulfones
Basement membrane；
（4）M-phenylenediamine solution and sodium dodecyl sulfate solution are mixed, obtain aqueous phase solution；By pyromellitic trimethylsilyl chloride, zirconium-
Metal-organic framework materials are added in n-hexane, and ultrasonic disperse 20min, obtains organic phase solution；
（5）The single side of polysulfones basement membrane is immersed in 2-5min in aqueous phase solution, is drained after taking-up, then again by the two of polysulfones basement membrane
Face is all immersed in 1-3min in organic phase solution, is drained after taking-up；
（6）By step（5）Obtained film dries 5-10min at 80 DEG C, that is, obtains positive osmosis composite membrane.
Preferably, step（2）Middle n,N-dimethylacetamide, the mass ratio of polysulfones are 40:13.
Preferably, it is characterised in that：Step（3）The power of middle microwave heating is 200W.
Preferably, it is characterised in that：Step（4）The mass concentration of middle m-phenylenediamine solution is 2%.
Preferably, it is characterised in that：Step（4）The mass concentration of middle sodium dodecyl sulfate solution is 0.15%.
Preferably, it is characterised in that：Step（4）Middle m-phenylenediamine solution, the volume ratio of sodium dodecyl sulfate solution are
1:1。
Preferably, step（4）The condition of middle ultrasonic disperse is：Ultrasonic power 200-500W, supersonic frequency 30Hz.
Advantages of the present invention：
Method provided by the invention is easy to operate, pollution-free, the forward osmosis membrane water flux being prepared is big, good hydrophilic property, separation
Performance is good.
Embodiment
Embodiment 1
The preparation method of zirconium-positive osmosis composite membrane of metal-organic framework materials modified polyamide, comprises the following steps：
（1）By zirconium chloride, deionized water, propionic acid, fumaric acid proportionally 0.12g:10mL:2.68g:0.18g is mixed,
It is subsequently placed at 120 DEG C and reacts 24h, cooled to room temperature, filtering, washs 3 times, Ran Houli respectively with deionized water and methanol
The heart, 24h is placed by sediment at normal temperatures, obtains zirconium-metal-organic framework materials；
（2）It is 74 in mass ratio by n,N-dimethylacetamide, polyethylene glycol 400 and deionized water:8:0.5 mixing, stirring,
Then polysulfones is added, 24h is stirred at 65 DEG C, cooling 24h is then stood, obtains polysulfones casting solution；Wherein, N, N- dimethyl second
Acid amides, the mass ratio of polysulfones are 40:13；
（3）By polysulfones casting solution, microwave heats 10min under power 200W, then carries out knifing, the thickness of film on a glass
For 60 μm, 30s is stood, 5min is stood into the water, film is taken off from glass plate, then soaks 24h in deionized water, obtains
To polysulfones basement membrane；
（4）It is 0.15% sodium dodecyl sulfate solution according to body by m-phenylenediamine solution and mass concentration that mass concentration is 2%
Product ratio 1:1 mixing, obtains aqueous phase solution；Pyromellitic trimethylsilyl chloride, zirconium-metal-organic framework materials are added in n-hexane,
Ultrasonic disperse 20min under conditions of ultrasonic power 200W, supersonic frequency 30Hz, obtains organic phase solution；
（5）The single side of polysulfones basement membrane is immersed in 2min in aqueous phase solution, is drained after taking-up, then again by the two sides of polysulfones basement membrane
1min in organic phase solution is all immersed in, is drained after taking-up；
（6）By step（5）Obtained film dries 5min at 80 DEG C, that is, obtains positive osmosis composite membrane.
Embodiment 2
The preparation method of zirconium-positive osmosis composite membrane of metal-organic framework materials modified polyamide, comprises the following steps：
（1）By zirconium chloride, deionized water, propionic acid, fumaric acid proportionally 0.12g:10mL:2.68g:0.18g is mixed,
It is subsequently placed at 120 DEG C and reacts 30h, cooled to room temperature, filtering, washs 3 times, Ran Houli respectively with deionized water and methanol
The heart, 24h is placed by sediment at normal temperatures, obtains zirconium-metal-organic framework materials；
（2）It is 74 in mass ratio by n,N-dimethylacetamide, polyethylene glycol 400 and deionized water:8:0.5 mixing, stirring,
Then polysulfones is added, 24h is stirred at 65 DEG C, cooling 24h is then stood, obtains polysulfones casting solution；Wherein, N, N- dimethyl second
Acid amides, the mass ratio of polysulfones are 40:13；
（3）By polysulfones casting solution, microwave heats 10min under power 200W, then carries out knifing, the thickness of film on a glass
For 70 μm, 30s is stood, 10min is stood into the water, film is taken off from glass plate, then soaks 24h in deionized water,
Obtain polysulfones basement membrane；
（4）It is 0.15% sodium dodecyl sulfate solution according to body by m-phenylenediamine solution and mass concentration that mass concentration is 2%
Product ratio 1:1 mixing, obtains aqueous phase solution；Pyromellitic trimethylsilyl chloride, zirconium-metal-organic framework materials are added in n-hexane,
Ultrasonic disperse 20min under conditions of ultrasonic power 500W, supersonic frequency 30Hz, obtains organic phase solution；
（5）The single side of polysulfones basement membrane is immersed in 5min in aqueous phase solution, is drained after taking-up, then again by the two sides of polysulfones basement membrane
3min in organic phase solution is all immersed in, is drained after taking-up；
（6）By step（5）Obtained film dries 10min at 80 DEG C, that is, obtains positive osmosis composite membrane.
Embodiment 3
The preparation method of zirconium-positive osmosis composite membrane of metal-organic framework materials modified polyamide, comprises the following steps：
（1）By zirconium chloride, deionized water, propionic acid, fumaric acid proportionally 0.12g:10mL:2.68g:0.18g is mixed,
It is subsequently placed at 120 DEG C and reacts 28h, cooled to room temperature, filtering, washs 3 times, Ran Houli respectively with deionized water and methanol
The heart, 24h is placed by sediment at normal temperatures, obtains zirconium-metal-organic framework materials；
（2）It is 74 in mass ratio by n,N-dimethylacetamide, polyethylene glycol 400 and deionized water:8:0.5 mixing, stirring,
Then polysulfones is added, 24h is stirred at 65 DEG C, cooling 24h is then stood, obtains polysulfones casting solution；Wherein, N, N- dimethyl second
Acid amides, the mass ratio of polysulfones are 40:13；
（3）By polysulfones casting solution, microwave heats 10min under power 200W, then carries out knifing, the thickness of film on a glass
For 70 μm, 30s is stood, 7min is stood into the water, film is taken off from glass plate, then soaks 24h in deionized water, obtains
To polysulfones basement membrane；
（4）It is 0.15% sodium dodecyl sulfate solution according to body by m-phenylenediamine solution and mass concentration that mass concentration is 2%
Product ratio 1:1 mixing, obtains aqueous phase solution；Pyromellitic trimethylsilyl chloride, zirconium-metal-organic framework materials are added in n-hexane,
Ultrasonic disperse 20min under conditions of ultrasonic power 400W, supersonic frequency 30Hz, obtains organic phase solution；
（5）The single side of polysulfones basement membrane is immersed in 4min in aqueous phase solution, is drained after taking-up, then again by the two sides of polysulfones basement membrane
2min in organic phase solution is all immersed in, is drained after taking-up；
（6）By step（5）Obtained film dries 8min at 80 DEG C, that is, obtains positive osmosis composite membrane.
Claims (7)
1. the preparation method of zirconium-positive osmosis composite membrane of metal-organic framework materials modified polyamide, it is characterised in that：Including following
Step：
（1）By zirconium chloride, deionized water, propionic acid, fumaric acid proportionally 0.12g:10mL:2.68g:0.18g is mixed,
It is subsequently placed at 120 DEG C and reacts 24-30h, cooled to room temperature, filtering, washs 3 times, so respectively with deionized water and methanol
After centrifuge, sediment is placed into 24h at normal temperatures, obtains zirconium-metal-organic framework materials；
（2）It is 74 in mass ratio by n,N-dimethylacetamide, polyethylene glycol 400 and deionized water:8:0.5 mixing, stirring,
Then polysulfones is added, 24h is stirred at 65 DEG C, cooling 24h is then stood, obtains polysulfones casting solution；
（3）Polysulfones casting solution microwave is heated into 10min, then carries out knifing on a glass, the thickness of film is 65 ± 5 μm, quiet
30s is put, stands 5-10min into the water, film is taken off from glass plate, then soaks 24h in deionized water, obtains polysulfones
Basement membrane；
（4）M-phenylenediamine solution and sodium dodecyl sulfate solution are mixed, obtain aqueous phase solution；By pyromellitic trimethylsilyl chloride, zirconium-
Metal-organic framework materials are added in n-hexane, and ultrasonic disperse 20min, obtains organic phase solution；
（5）The single side of polysulfones basement membrane is immersed in 2-5min in aqueous phase solution, is drained after taking-up, then again by the two of polysulfones basement membrane
Face is all immersed in 1-3min in organic phase solution, is drained after taking-up；
（6）By step（5）Obtained film dries 5-10min at 80 DEG C, that is, obtains positive osmosis composite membrane.
2. the preparation method of zirconium according to claim 1-positive osmosis composite membrane of metal-organic framework materials modified polyamide,
It is characterized in that：Step（2）Middle n,N-dimethylacetamide, the mass ratio of polysulfones are 40:13.
3. the preparation method of zirconium according to claim 1-positive osmosis composite membrane of metal-organic framework materials modified polyamide,
It is characterized in that：Step（3）The power of middle microwave heating is 200W.
4. the preparation method of zirconium according to claim 1-positive osmosis composite membrane of metal-organic framework materials modified polyamide,
It is characterized in that：Step（4）The mass concentration of middle m-phenylenediamine solution is 2%.
5. the preparation method of zirconium according to claim 4-positive osmosis composite membrane of metal-organic framework materials modified polyamide,
It is characterized in that：Step（4）The mass concentration of middle sodium dodecyl sulfate solution is 0.15%.
6. the preparation method of zirconium according to claim 5-positive osmosis composite membrane of metal-organic framework materials modified polyamide,
It is characterized in that：Step（4）Middle m-phenylenediamine solution, the volume ratio of sodium dodecyl sulfate solution are 1:1.
7. the preparation method of zirconium according to claim 1-positive osmosis composite membrane of metal-organic framework materials modified polyamide,
It is characterized in that：Step（4）The condition of middle ultrasonic disperse is：Ultrasonic power 200-500W, supersonic frequency 30Hz.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012181A (en) * | 2018-09-13 | 2018-12-18 | 青岛科技大学 | A kind of synthetic method and gained permeable membrane of the modified Cellulose acetate forward osmotic membrane of ZIF-8 |
| CN109126480A (en) * | 2018-09-04 | 2019-01-04 | 同济大学 | Modified forward osmosis membrane of a kind of metal organic frame nanometer sheet and its preparation method and application |
| CN110523282A (en) * | 2019-09-26 | 2019-12-03 | 东华大学 | A kind of compound forward osmosis membrane of UiO-66 and its preparation and application |
| CN112210081A (en) * | 2020-09-29 | 2021-01-12 | 西安建筑科技大学 | Sulfonated graphene oxide loaded metal organic framework modified forward osmosis nano composite membrane and preparation method thereof |
| CN113041864A (en) * | 2021-04-08 | 2021-06-29 | 大连理工大学 | Method for modifying ceramic-based TFN forward osmosis membrane by titanium dioxide intermediate layer and application of method |
| CN113877426A (en) * | 2021-10-12 | 2022-01-04 | 上海应用技术大学 | Super-hydrophobic polypropylene modified ultrafiltration membrane and preparation method and application thereof |
| CN115463557A (en) * | 2022-09-19 | 2022-12-13 | 北京理工大学 | Synthesis of MOF-808 and preparation and application of modified polyamide composite membrane thereof |
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- 2017-12-04 CN CN201711259016.4A patent/CN107899431A/en not_active Withdrawn
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| CN109126480A (en) * | 2018-09-04 | 2019-01-04 | 同济大学 | Modified forward osmosis membrane of a kind of metal organic frame nanometer sheet and its preparation method and application |
| CN109126480B (en) * | 2018-09-04 | 2021-06-01 | 同济大学 | Metal organic framework nanosheet modified forward osmosis membrane and preparation method and application thereof |
| CN109012181A (en) * | 2018-09-13 | 2018-12-18 | 青岛科技大学 | A kind of synthetic method and gained permeable membrane of the modified Cellulose acetate forward osmotic membrane of ZIF-8 |
| CN110523282A (en) * | 2019-09-26 | 2019-12-03 | 东华大学 | A kind of compound forward osmosis membrane of UiO-66 and its preparation and application |
| CN110523282B (en) * | 2019-09-26 | 2021-11-09 | 东华大学 | UiO-66 composite forward osmosis membrane and preparation and application thereof |
| CN112210081A (en) * | 2020-09-29 | 2021-01-12 | 西安建筑科技大学 | Sulfonated graphene oxide loaded metal organic framework modified forward osmosis nano composite membrane and preparation method thereof |
| CN112210081B (en) * | 2020-09-29 | 2022-06-21 | 西安建筑科技大学 | Sulfonated graphene oxide loaded metal organic framework modified forward osmosis nano composite membrane and preparation method thereof |
| CN113041864A (en) * | 2021-04-08 | 2021-06-29 | 大连理工大学 | Method for modifying ceramic-based TFN forward osmosis membrane by titanium dioxide intermediate layer and application of method |
| CN114471200A (en) * | 2021-04-08 | 2022-05-13 | 大连理工大学 | Method for improving preparation of Zr-based MOF film through intermediate modification layer and forward osmosis application of method |
| CN113877426A (en) * | 2021-10-12 | 2022-01-04 | 上海应用技术大学 | Super-hydrophobic polypropylene modified ultrafiltration membrane and preparation method and application thereof |
| CN115463557A (en) * | 2022-09-19 | 2022-12-13 | 北京理工大学 | Synthesis of MOF-808 and preparation and application of modified polyamide composite membrane thereof |
| CN115463557B (en) * | 2022-09-19 | 2023-09-29 | 北京理工大学 | Synthesis of MOF-808 and preparation and application of modified polyamide composite membrane |
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