CN107837690A - Flat mixed-matrix forward osmosis membrane and preparation method based on metal organic framework ZIF 8 - Google Patents
Flat mixed-matrix forward osmosis membrane and preparation method based on metal organic framework ZIF 8 Download PDFInfo
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- CN107837690A CN107837690A CN201711334168.6A CN201711334168A CN107837690A CN 107837690 A CN107837690 A CN 107837690A CN 201711334168 A CN201711334168 A CN 201711334168A CN 107837690 A CN107837690 A CN 107837690A
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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
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
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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
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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
- B01D69/06—Flat membranes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/445—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by forward osmosis
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Abstract
The invention discloses a kind of flat mixed-matrix forward osmosis membrane and preparation method based on metal organic framework ZIF 8, belong to technical field of membrane separation.By 0.1%~2.0%（w/w）ZIF 8 be dispersed in 64.0%~89.9% by ultrasound（w/w）In the mixed solvent, then with 8.0%~20.0%（w/w）Cellulose acetate together, be added in a certain order in three neck round bottom flask, stirring be completely dissolved cellulose acetate after, add 2.0%~14.0%（w/w）Polyvinylpyrrolidone or polyethylene glycol 400 2~16h of stirring and dissolving is to being completely dissolved at a temperature of 25~90 DEG C, 3~16h of standing and defoaming, prepare forward osmosis membrane casting solution；5~60mins is heat-treated using phase inversion striking film forming on backing material and in 30~90 DEG C of deionized waters, that is, the flat mixed-matrix forward osmosis membrane based on ZIF 8 is made.The made forward osmosis membrane of the present invention is by the use of 1M NaCl as driving liquid, deionized water as material liquid, and in 1h testing time, its pure water flux reaches 27.0L/m2More than h, reverse flux salt are less than 1.0g/m2•h。
Description
Technical field
The present invention relates to flat forward osmosis membrane of a kind of macromolecule and preparation method thereof, and metal is based on more particularly to one kind
Organic backbone ZIF-8 flat mixed-matrix forward osmosis membrane and preparation method.
Background technology
The scarcity of water resource and the water pollution of getting worse turn into the bottleneck for restricting social progress and economic development, new water
Source is developed and effluent sewage recycling also turns into global question of common concern.Because seawater resources are extremely abundant on the earth,
And substantial amounts of effluent sewage is produced, desalinization and sewage recycling turn into the strategic choice for solving water resources crisis.Many
Desalinization and sewage recycling technology in, membrane separation technique is one of best selection.Asked as to solve this key
Topic and be born low energy consumption, the positive infiltration technology of high Water Sproading rate is into desalinization and the research emphasis in sewage recycling field
And focus, to solving the problems, such as that shortage of water resources has important strategic importance.
Positive infiltration (forward osmosis, FO) is a kind of membrane separation technique driven by film both sides osmotic pressure, just
It is increasingly subject to pay attention to, related theory and application study achieve larger progress, and are successfully applied to desalinization, at waste water
The field such as reason, food medicine, the energy.At present, common forward osmosis membrane mainly has cellulose acetate film, polybenzimidazole membrane, gathered
Acid amides composite membrane etc., degree of commercialization is not high to be mainly a lack of forward osmosis membrane of good performance and suitable driving liquid, and just oozes
Permeable membrane is the key point of whole positive process of osmosis.The close phase of structure of high performance forward osmosis membrane and its material character and film
Close, it is seen that the membrane material and forward osmosis membrane preparation method of function admirable are particularly important.Common forward osmosis membrane preparation method bounded
Face polymerization, double selection tunics prepare three kinds of method and nanofiltration membrane modifying.Concentration difference in positive osmosis composite membrane prepared by interfacial polymerization
Polarize more serious；Double selection tunics effectively reduce interior concentration polarization, but preparation technology is complex；NF membrane Modified Membrane is to list
The rejection and water flux of valency salt are relatively low；Therefore, it is necessary to develop new forward osmosis membrane preparation technology to improve forward osmosis membrane
Separating property and the feasibility of industrialization.
The last century 60's, foreign countries are started the research of positive infiltration technology, entered using existing reverse osmosis membrane or NF membrane
The application study that row is just permeating, as a result proves that existing reverse osmosis membrane or NF membrane are difficult to use in positive process of osmosis, but simultaneously
Performance and membrane material, the membrane structure for demonstrating forward osmosis membrane are closely related；Then, all multimembrane scientific workers have started positive infiltration
The basic research of film preparation.Result of study shows, can be excellent with processability by selecting suitable membrane material, film-forming process
Forward osmosis membrane.The research of the positive infiltration technology in China is started late, and the current country aligns the research of infiltration technology, either film system
Standby or membrane process research, still in the exploratory stage.Some film researchers explore the preparation of cellulose family forward osmosis membrane
Condition, influence of the various factors to forward osmosis membrane performance is have studied, but not yet prepare just oozing for commercially viable function admirable
Permeable membrane；The preparation and application study of forward osmosis membrane still shoulder heavy responsibilities.The studying enlightenments of early stage we, changed using blending technology
Property membrane material, be expected to improve water flux, salt-stopping rate, mechanical performance and the anti-fouling performance of forward osmosis membrane, and be easily achieved production
Industry.Patent of invention ZL201410770001.4,201510245514.8 and ZL201410769752.4,201510245504.4
Nano titanium oxide and graphene is respectively adopted and prepares flat and doughnut forward osmosis membrane with acetyl cellulose blend, it is made
The separating property and permeance property of standby forward osmosis membrane have obtained raising by a relatively large margin；Patent of invention 2017100954795,
2017100954780th, 2017100954846 more excellent performance is prepared for using functionalized carbon nano-tube and acetyl cellulose blend
Forward osmosis membrane；But by selecting suitable material, the separating property and permeance property of prepared forward osmosis membrane can still be carried out
Further to improve, satisfaction is commercially produced and application demand.
It is new that metal organic framework (Metal-Organic Frameworks, MOFs) is that a kind of latest developments are got up
Material, also known as metal organic complex polymer, it is to pass through coordination group by the organic ligand and metal ion of oxygen-containing, nitrogen etc.
Fill the porous material of the infinite network structure formed.Compared to traditional inorganic porous material, MOFs materials possess zeolite, activity
The unrivaled premium properties of the inorganic porous materials such as charcoal, CNT, its Micropore volume are higher by several than above-mentioned porous material
Times, and have the characteristics that duct is variable, steady chemical structure.These excellent characteristics cause MOFs materials in gas storage, water
Body pollution thing adsorbing separation, gas catalysis etc. have huge application prospect.Metal organic framework is as a kind of new
Organic-inorganic hybrid material, the organic ligand in its structure are favorably improved the affinity between MOFs particles and polymer substrate,
It is preferable mixed substrate membrane containing nano-grade molecular sieve dispersed phase.Therefore, suitable MOFs materials and acetyl cellulose blend are such as prepared into mixed-matrix
Forward osmosis membrane, it is expected to while high water flux, salt-stopping rate is obtained, also make forward osmosis membrane product that there is stain resistance, this is just
The research and development and application of permeable membrane material provide new thinking.
How while hydrophilic nmature is obtained, make forward osmosis membrane that there is resistance tocrocking again and keep the stabilization of water flux
Property, this is the problem that film scientific worker is thinking and studied always in recent years.The present invention is improving mixed-matrix just using ZIF-8
The research of the structure and permeance property, separating property of permeable membrane, both at home and abroad there is not yet document report.
The content of the invention
It is an object of the invention to provide a kind of flat mixed-matrix forward osmosis membrane based on metal organic framework ZIF-8,
It is a further object to provide the preparation method of the mixed-matrix forward osmosis membrane.
To achieve the above object, the technical scheme taken of the present invention is：
A kind of flat mixed-matrix forward osmosis membrane based on ZIF-8, is by the material composition of following mass percent：Polymerization
Thing membrane material 8.0%~20.0%（w/w）, pore-foaming agent 2.0%~14.0%（w/w）, ZIF-8 0.1%~2.0%（w/w）, solvent
64.0%~89.9%（w/w）；
Described polymeric film material is one or both of cellulose diacetate and Triafol T, content is 8.0%~
20.0%（w/w）；
Described metal organic framework ZIF-8 is self-control metal-organic framework materials, typical three-dimensional 12 face body structures, and content is
0.1%~2.0%（w/w）；
Described pore-foaming agent is one kind of polyvinylpyrrolidone and PEG-4000, and content is 2.0%~14.0%（w/w）；
The solvent is the mixed solvent of 1-METHYLPYRROLIDONE and acetone, and its volume ratio is 1-METHYLPYRROLIDONE:Acetone=
1:0.1~7.0, content is 64.0%~89.9%（w/w）.
A kind of preparation method of the flat mixed-matrix forward osmosis membrane based on metal organic framework ZIF-8, including it is following
Step：
（1）A certain amount of ZIF-8 is added in the mixed solvent, is allowed to fully dispersed wherein using ultrasound, is disperseed
After the completion of be added in three neck round bottom flask, and add a certain amount of polymeric film material, stir；
（2）A certain amount of pore-foaming agent is added in three neck round bottom flask, stirring and dissolving 2~16 hours at a temperature of 25~90 DEG C
To being completely dissolved, the initial casting solution of the flat mixed-matrix forward osmosis membrane based on ZIF-8 is configured to；Then, will obtain
Casting solution is static at a temperature of stirring and dissolving to be placed 3~16 hours, removes bubble remaining in casting solution；
（3）Supporting layer is laid on the glass plate cleaned and dried, then poured into a certain amount of casting solution on glass plate, used
Flat Membrane scraper striking film forming；After the nascent state film formed is evaporated into 1~30 second at room temperature, 15~60 DEG C of constant temperature is immersed
Solidification forming in coagulating bath water tank, film shaping automatically disengages glass plate, after taking the film out in deionized water at normal temperature immersion 12~
48 hours, then it is heat-treated 5~60 minutes in 30~90 DEG C of deionized water, that is, obtains the flat mixing based on ZIF-8
Matrix forward osmosis membrane.
Described supporting layer is one kind of polyester screen, non-woven fabrics, cotton yarn filter cloth, filter paper and nylon cloth, and its aperture is 60
~280 mesh；
Evaporation time under described nascent state film normal temperature, refer to that prepared flat forward osmosis membrane is completed after sky in knifing
Residence time in gas, evaporation time are 1~30 second；
Described heat treatment temperature and time, refer to the deionization water temperature being heat-treated to prepared flat forward osmosis membrane
Degree and processing time, heat treatment temperature are 30~90 DEG C, and heat treatment time is 5~60 minutes；
Described coagulating bath is deionized water.
The invention provides a kind of flat mixed-matrix forward osmosis membrane based on metal organic framework ZIF-8 and preparation side
Method, ZIF-8 is incorporated into polymer and prepares mixed-matrix forward osmosis membrane, and assign mixed-matrix forward osmosis membrane good infiltration
Performance, separating property and antifouling property, this is the innovation of the present invention.Test result shows, prepared forward osmosis membrane
Pure water flux and reverse flux salt have very big improvement.
The present invention compares with prior art, has following beneficial effect：
（1）ZIF-8 provided by the present invention solves the problem of caving in of conventional metals organic backbone, prepared by its blending and modifying
Blending forward osmosis membrane phase of the flat mixed-matrix forward osmosis membrane with traditional Cellulose acetate forward osmotic membrane, based on CNT
Than its pure water flux and reverse flux salt are obviously improved.
（2）The method that ZIF-8 blending and modifyings provided by the present invention prepare flat mixed-matrix forward osmosis membrane, it is used
Equipment is simple, easily-controllable, and film preparation technique is simple, assign while film forming prepared by the good permeance property of forward osmosis membrane, separation
Performance and antifouling property, it is easy to accomplish industrialization.
Embodiment：
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1：
By 0.7%（w/w）ZIF-8 be added to 54.3%（w/w）1-METHYLPYRROLIDONE and 25.0%（w/w）Acetone composition mixes
In bonding solvent, it is allowed to fully dispersed wherein using ultrasound, is added to after the completion of scattered in three neck round bottom flask, and adds
Enter 12.0%（w/w）Cellulose acetate, stir.By 8.0%（w/w）PEG-4000 pore-foaming agent be added to three mouthfuls of circles
In the flask of bottom, stirring and dissolving is configured to the flat mixed-matrix based on ZIF-8 in 8 hours to being completely dissolved at a temperature of 60 DEG C
The initial casting solution of forward osmosis membrane；Then, static placement 9 hours, removing casting at a temperature of stirring and dissolving by obtained casting solution
Remaining bubble in film liquid.The polyester screen of 180 mesh is laid on the glass plate cleaned and dried, then by a certain amount of casting
Film liquid is poured on glass plate, with Flat Membrane scraper striking film forming；After the nascent state film formed is evaporated into 10 seconds at room temperature, leaching
Enter solidification forming in 25 DEG C of constant temperature coagulating bath water tank, film shaping automatically disengages glass plate, in normal temperature deionization after taking the film out
Soaked in water 24 hours, be then heat-treated 15 minutes in 65 DEG C of deionized water, that is, obtain the flat mixing based on ZIF-8
Matrix forward osmosis membrane.It is prepared in 1h testing time as material liquid by the use of 1MNaCl as driving liquid, deionized water
The pure water flux of forward osmosis membrane reaches 27.0L/m2More than h, reverse flux salt are less than 1.0g/m2•h。
Embodiment 2：
The content of ZIF-8,1-METHYLPYRROLIDONE is adjusted to 0.1% respectively（w/w）With 54.9%（w/w）, remaining is the same as implementation
Example 1.Then the performance of the obtained flat mixed-matrix forward osmosis membrane based on ZIF-8 is：By the use of 1MNaCl as driving liquid,
Deionized water is as material liquid, and in 1h testing time, the pure water flux of prepared forward osmosis membrane reaches 23.5L/m2H with
On, reverse flux salt is less than 2.0g/m2•h。
Embodiment 3：
The content of ZIF-8,1-METHYLPYRROLIDONE is adjusted to 2.0% respectively（w/w）With 53.0%（w/w）, remaining is the same as implementation
Example 1.Then the performance of the obtained flat mixed-matrix forward osmosis membrane based on ZIF-8 is：By the use of 1MNaCl as driving liquid,
Deionized water is as material liquid, and in 1h testing time, the pure water flux of prepared forward osmosis membrane reaches 29.0L/m2H with
On, reverse flux salt is less than 2.5g/m2•h。
Embodiment 4：
PEG-4000 in pore-foaming agent is replaced by polyvinylpyrrolidone, remaining is the same as embodiment 1.It is then obtained
The performance of flat mixed-matrix forward osmosis membrane based on ZIF-8 is：By the use of 1MNaCl as driving liquid, deionized water is as former
Feed liquid, in 1h testing time, the pure water flux of prepared forward osmosis membrane reaches 24.0L/m2More than h, reverse flux salt are small
In 1.0g/m2•h。
Embodiment 5：
Coagulation bath temperature is adjusted to 60 DEG C by 25 DEG C, remaining is the same as embodiment 1.It is then obtained based on the flat of ZIF-8
The performance of mixed-matrix forward osmosis membrane is：By the use of 1MNaCl as driving liquid, deionized water is as material liquid, in 1h test
Between in, the pure water flux of prepared forward osmosis membrane reaches 31.0L/m2More than h, reverse flux salt are less than 2.0g/m2•h。
Embodiment 6：
Heat treatment temperature is adjusted to 90 DEG C by 65 DEG C, remaining is the same as embodiment 1.It is then obtained based on the flat of ZIF-8
The performance of mixed-matrix forward osmosis membrane is：By the use of 1MNaCl as driving liquid, deionized water is as material liquid, in 1h test
Between in, the pure water flux of prepared forward osmosis membrane reaches 25.0L/m2More than h, reverse flux salt are less than 1.5g/m2•h。
Embodiment 7：
Heat treatment time was adjusted to 60 minutes by 15 minutes, remaining is the same as embodiment 1.The then obtained height based on ZIF-8
The performance of the flat forward osmosis membrane of performance is：By the use of 1MNaCl as driving liquid, deionized water is as material liquid, in 1h test
In time, the pure water flux of prepared forward osmosis membrane reaches 26.0L/m2More than h, reverse flux salt are less than 1.0g/m2•h。
Comparative example 1：
By 55.0%（w/w）1-METHYLPYRROLIDONE and 25.0%（w/w）The mixed solvent of acetone composition is added to three mouthfuls of round bottoms and burnt
In bottle, 13.0% is then added（w/w）Cellulose acetate, stir.By 7.0%（w/w）PEG-4000 pore-foaming agent
It is added in three neck round bottom flask, stirring and dissolving is configured to flat acetate fiber in 8 hours to being completely dissolved at a temperature of 65 DEG C
The initial casting solution of plain mixed-matrix forward osmosis membrane；Then, by obtained casting solution, static placement 9 is small at a temperature of stirring and dissolving
When, remove bubble remaining in casting solution.The polyester screen of 180 mesh is laid on the glass plate cleaned and dried, then will
A certain amount of casting solution is poured on glass plate, with Flat Membrane scraper striking film forming；The nascent state film formed is steamed at room temperature
Hair immerses solidification forming in 25 DEG C of constant temperature coagulating bath water tank after 10 seconds, and film shaping automatically disengages glass plate, after taking the film out
Soaked in deionized water at normal temperature 24 hours, be then heat-treated 15 minutes in 65 DEG C of deionized water, that is, obtain flat acetic acid
Cellulose mixed-matrix forward osmosis membrane.By the use of 1MNaCl as driving liquid, deionized water is as material liquid, in 1h testing time
In, the pure water flux of prepared forward osmosis membrane reaches 33.0L/m2More than h, reverse flux salt are less than 4.0g/m2•h。
Claims (10)
1. a kind of flat mixed-matrix forward osmosis membrane based on metal organic framework ZIF-8, it is characterised in that in its casting solution
Containing metal organic framework ZIF-8, and influence the structure and performance of forward osmosis membrane；Casting solution by following mass percent material
Composition：Polymeric film material 8.0%~20.0%（w/w）, pore-foaming agent 2.0%~14.0%（w/w）, ZIF-8 0.1%~2.0%（w/
w）, solvent 64.0%~89.9%（w/w）.
2. the flat mixed-matrix forward osmosis membrane based on ZIF-8 according to claim 1, it is characterised in that：Described
Forward osmosis membrane is prepared using traditional phase inversion i.e. dry-wet method.
3. the flat mixed-matrix forward osmosis membrane based on ZIF-8 according to claim 1, it is characterised in that：Described
ZIF-8 is self-control metal organic framework, and for typical three-dimensional 12 face body structures, content is 0.1%~2.0%（w/w）.
4. the flat mixed-matrix forward osmosis membrane according to claim 1 based on ZIF-8, it is characterised in that：Described
Cellulose acetate is one or both of cellulose diacetate and Triafol T.
5. the flat mixed-matrix forward osmosis membrane according to claim 1 based on ZIF-8, it is characterised in that：Described
Pore-foaming agent is one kind of polyvinylpyrrolidone and PEG-4000, and content is 2.0%~14.0%（w/w）.
6. the flat mixed-matrix forward osmosis membrane according to claim 1 based on ZIF-8, it is characterised in that：It is described molten
Agent is the mixed solvent of 1-METHYLPYRROLIDONE and acetone, and its volume ratio is 1-METHYLPYRROLIDONE：Acetone=1:0.1~7.0,
Content is 64.0%~89.9%（w/w）.
A kind of 7. preparation method of the flat mixed-matrix forward osmosis membrane based on metal organic framework ZIF-8, it is characterised in that
It includes：
（1）A certain amount of ZIF-8 is added in the mixed solvent, is allowed to fully dispersed wherein using ultrasound, is disperseed
After the completion of be added in three neck round bottom flask, and add a certain amount of polymeric film material, stir；
（2）A certain amount of pore-foaming agent is added in three neck round bottom flask, stirring and dissolving 2~16 hours at a temperature of 25~90 DEG C
To being completely dissolved, the initial casting solution of the flat mixed-matrix forward osmosis membrane based on ZIF-8 is configured to；Then, will obtain
Casting solution is static at a temperature of stirring and dissolving to be placed 3~16 hours, removes bubble remaining in casting solution；
（3）Supporting layer is laid on the glass plate cleaned and dried, then poured into a certain amount of casting solution on glass plate, used
Flat Membrane scraper striking film forming；After the nascent state film formed is evaporated into 1~30 second at room temperature, 15~60 DEG C of constant temperature is immersed
Solidification forming in coagulating bath water tank, film shaping automatically disengages glass plate, after taking the film out in deionized water at normal temperature immersion 12~
48 hours, then it is heat-treated 5~60 minutes in 30~90 DEG C of deionized water, that is, obtains the flat mixing based on ZIF-8
Matrix forward osmosis membrane.
8. the preparation method of the flat mixed-matrix forward osmosis membrane according to claim 7 based on ZIF-8, its feature exist
In：Described supporting layer is one kind of polyester screen, non-woven fabrics, cotton yarn filter cloth, filter paper and nylon cloth, and its aperture is 60~280
Mesh；Described coagulating bath is deionized water.
9. the preparation method of the flat mixed-matrix forward osmosis membrane according to claim 7 based on ZIF-8, its feature exist
In：Evaporation time under described nascent state film normal temperature is 1~30 second.
10. the preparation method of the flat mixed-matrix forward osmosis membrane according to claim 7 based on ZIF-8, its feature
It is：Described heat treatment temperature is 30~90 DEG C, and described heat treatment time is 5~60 minutes.
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