CN108014652B - Based on MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane - Google Patents
Based on MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane Download PDFInfo
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- CN108014652B CN108014652B CN201711476031.4A CN201711476031A CN108014652B CN 108014652 B CN108014652 B CN 108014652B CN 201711476031 A CN201711476031 A CN 201711476031A CN 108014652 B CN108014652 B CN 108014652B
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D69/08—Hollow fibre membranes
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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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Abstract
The invention discloses one kind to be based on metal organic framework compound MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane and preparation method, belongs to technical field of membrane separation.By 17.0 ~ 35.0%(w/w) cellulose acetate, 5.0 ~ 20.0%(w/w) polyethylene glycol-400 or polyvinylpyrrolidone, 0.05 ~ 2.0%(w/w) surfactant, 0.1 ~ 2.5%(w/w) MIL-101 (Cr)/GO and 40.5 ~ 77.85%(w/w) mixed solvent of N-Methyl pyrrolidone and acetone composition is added in dissolving tank in a certain order, dissolution is sufficiently stirred 5 ~ 16 hours at a temperature of 25 ~ 90 DEG C, and standing and defoaming obtains the blending doughnut forward osmosis membrane casting solution based on MIL-101 (Cr)/GO;Doughnut forward osmosis membrane is prepared using dry-wet spinning technique, and can be obtained after 10 ~ 60mins of heat treatment based on MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane in 30 ~ 90 DEG C of deionized waters.Forward osmosis membrane prepared by the present invention does driving liquid using 1M NaCl, deionized water does material liquid, and in the testing time of 1h, pure water flux reaches 27.0L/m2H or more, reversed flux salt are less than 0.5g/m2·h。
Description
Technical field
The present invention relates to a kind of polymeric hollow fiber forward osmosis membranes and preparation method thereof, more particularly to one kind based on gold
Belong to the acetyl cellulose blend doughnut forward osmosis membrane and preparation method of organic backbone compound MIL-101 (Cr)/GO.
Background technique
Positive infiltration (forward osmosis, FO) is a kind of membrane separation technique driven by film two sides osmotic pressure, tool
Have the advantages of low energy consumption, the high water rate of recovery, be just paid more and more attention, relevant theoretical and application study achieve it is biggish into
Exhibition, and it is successfully applied to the fields such as sea water desalination, wastewater treatment, food medicine, the energy.Currently, forward osmosis membrane commercialization degree
It is not high to be mainly a lack of forward osmosis membrane of good performance and suitable driving liquid, and forward osmosis membrane is the pass of entire positive process of osmosis
Where key.High performance forward osmosis membrane and the structure of its material properties and film are closely related, it is seen that the membrane material of function admirable and
Forward osmosis membrane preparation method is particularly important.Common forward osmosis membrane preparation method has interfacial polymerization, double selection tunic the preparation methods
With three kinds of nanofiltration membrane modifying.Concentration polarization is more serious in the positive osmosis composite membrane of interfacial polymerization preparation;Double selection tunics are effective
Interior concentration polarization is reduced, but preparation process is complex;Nanofiltration membrane Modified Membrane to the rejection and water flux of monovalent salt compared with
It is low;Therefore, it is necessary to develop new forward osmosis membrane preparation process to improve the feasibility of the separating property and industrialization of forward osmosis membrane.
The sixties in last century, foreign countries start the research of positive infiltration technology, using commercialization reverse osmosis membrane or nanofiltration membrane into
The application study that row is just permeating, as a result proves that existing reverse osmosis membrane or nanofiltration 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 show by selecting suitable membrane material, film-forming process, can be excellent with processability
Forward osmosis membrane.The research of the positive infiltration technology in China is started late, at present the domestic research to positive 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 has studied influence of the various factors to forward osmosis membrane performance, but not yet prepares the positive infiltration of commercially viable function admirable
Permeable membrane;The preparation and application study of forward osmosis membrane still shoulder heavy responsibilities.The studying enlightenments of early period 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, ZL201410769752.4 and 2017100954795,2017100954780,
2017100954846, which are respectively adopted nano-titanium dioxide, graphene, functionalized carbon nano-tube and acetyl cellulose blend preparation, puts down
Board-like forward osmosis membrane, the separating property and permeance property of prepared forward osmosis membrane have obtained raising by a relatively large margin;But pass through choosing
Select suitable auxiliary material, still can separating property to prepared forward osmosis membrane and permeance property further improved, it is full
Foot is commercially produced and application demand.
Metal organic framework (Metal-Organic Frameworks, MOFs) is a kind of with infinite network structure
Porous material;Compared to traditional inorganic porous material, it is inorganic porous that MOFs material possesses zeolite, active carbon, carbon nanotube etc.
The unrivaled excellent performance of material, Micropore volume are higher by several times than above-mentioned porous material, and have duct variable, chemical
The features such as stable structure;These excellent characteristics urge MOFs material in gas storage, water pollutant adsorbing separation, gas
Change etc. has huge application prospect.Meanwhile as a kind of novel organic-inorganic hybrid material, metal organic framework knot
Organic ligand in structure helps to improve the affinity between MOFs particle and polymer substrate, is ideal mixed substrate membrane containing nano-grade molecular sieve dispersion
Phase.Therefore, the MOFs material for being suitable for and acetyl cellulose blend are such as prepared into forward osmosis membrane, is expected to obtaining high water flux, cutting
While salt rate, also make forward osmosis membrane product that there is stain resistance and high mechanical strength, the research of this permeable membrane material that is positive
Exploitation and application provide new thinking.
Currently, most of forward osmosis membrane component is plate membrane pattern, the pattern membrane module small, membrane module with specific surface area
The problems such as packed density is low affects the application efficiency of film.Patent of invention 201510245514.8,201510245504.4 is distinguished
Doughnut forward osmosis membrane, prepared forward osmosis membrane are prepared for using nano-titanium dioxide and graphene and acetyl cellulose blend
Separating property and permeance property obtained raising by a relatively large margin, but its self-supporting ability is it is still necessary to further increase, to meet
The needs of industrial applications;ZL201210137147.6,201510639448.2,201710039263.7,201580044166
.6 the compound forward osmosis membrane of doughnut has been invented, has improved the performance of forward osmosis membrane, but preparation process is complex;The present invention adopts
The structure for improving doughnut forward osmosis membrane with MIL-101 (Cr)/GO blending method simplifies film-forming process, improves forward osmosis membrane
Mechanical performance and permeance property, separating property research, both at home and abroad there is not yet document report.
Summary of the invention
The invention discloses one kind to be based on metal organic framework compound MIL-101 (Cr)/GO acetyl cellulose blend
Doughnut forward osmosis membrane, it is a further object to provide the preparation methods of the blending doughnut forward osmosis membrane.
To achieve the above object, the technical scheme adopted by the invention is as follows:
One kind is just seeped based on metal organic framework compound MIL-101 (Cr)/GO acetyl cellulose blend doughnut
Permeable membrane is by the material composition of following mass percent: 17.0 ~ 35.0%(w/w of polymeric film material), pore-foaming agent 5.0 ~
20.0%(w/w), 0.05 ~ 2.0%(w/w of surfactant), MIL-101 (Cr)/0.1 ~ 2.5%(w/w of GO), mixed solvent 40.5
~ 77.85%(w/w).
The polymeric film material is one or both of cellulose diacetate and Triafol T, and content is
17.0 ~ 35.0%(w/w);
MIL-101 (the Cr)/GO is self-control metal organic framework compound, is blocky-shaped particle structure, and content is
0.1 ~ 2.5%(w/w).
The pore-foaming agent is one kind of polyvinylpyrrolidone and polyethylene glycol-400, and content is 5.0% ~ 20.0%(w/
W).
The surfactant is Tween-80, and content is 0.05% ~ 2.0%(w/w).
The mixed solvent is the mixed solvent that N-Methyl pyrrolidone and acetone form, volume ratio be 1:0.2 ~
10.0(v/v), content is 40.5 ~ 77.85%(w/w).
One kind is just seeped based on metal organic framework compound MIL-101 (Cr)/GO acetyl cellulose blend doughnut
The preparation method of permeable membrane, comprising the following steps:
(1) selecting cellulose diacetate or Triafol T is membrane material, and Tween-80 is surfactant, polyethylene
Pyrrolidones or polyethylene glycol-400 are pore-foaming agent, and metal organic framework compound MIL-101 (Cr)/GO is as additive, N-
The mixed solvent of methyl pyrrolidone and acetone composition is added separately in dissolving tank, stirs at a temperature of 25 ~ 90 DEG C as solvent
Dissolution 5 ~ 16 hours is mixed to full and uniform, prepares casting solution;Then, it puts obtained casting solution is static at a temperature of stirring and dissolving
It sets 3 ~ 16 hours, removes bubble remaining in casting solution, it is hollow to obtain the acetyl cellulose blend based on MIL-101 (Cr)/GO
Fiber forward osmosis membrane casting solution;
(2) keeping forward osmosis membrane casting solution temperature is 25 ~ 90 DEG C, and the pressure for adjusting metering pump is 0.05 ~ 0.5MPa, will be cast
Film liquid, which is squeezed into the annular space of spinning nozzle by metering pump, forms as-spun fibre, and as-spun fibre leaves spray head by 0 ~ 15cm's
It behind the air gap, is pulled into the coagulating basin equipped with 15 ~ 60 DEG C of deionized waters through winding-roller, carries out 0.5 ~ 5mins solidification
Doughnut forward osmosis membrane is blended in forming, spinning;
(3) it impregnates, rinse 12 ~ 48 hours in deionized water at normal temperature after taking out the doughnut forward osmosis membrane of forming,
Change a water within every 4 ~ 8 hours;Then 10 ~ 60mins is heat-treated in 30 ~ 90 DEG C of deionized water to get organic to metal is based on
Skeleton compound MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane.
The air gap refers to spinning nozzle annular space the distance between to the coagulating bath water surface, the air gap is 0 ~
15cm;
The coagulating bath is deionized water, and coagulation bath temperature is 15 ~ 60 DEG C, and setting time is 0.5 ~ 5mins;
The heat treatment temperature and time refers to and is heat-treated to prepared blending doughnut forward osmosis membrane
Deionized water temperature and processing time, heat treatment temperature are 30 ~ 90 DEG C, and heat treatment time is 5 ~ 60 mins.
The present invention provides one kind to be based on metal organic framework compound MIL-101 (Cr)/GO acetyl cellulose blend
Doughnut forward osmosis membrane, by the metal organic framework compound MIL-101 with huge surface area, porosity and adsorptivity
(Cr)/GO is introduced into preparation in polymer and doughnut forward osmosis membrane is blended, and effectively improves the knot of doughnut forward osmosis membrane
Structure and performance, improve prepared mechanical performance, permeance property and the separating property that doughnut forward osmosis membrane is blended, this is this
The innovation of invention.Test result shows the pure water flux of prepared forward osmosis membrane, reversed flux salt, mechanical performance and resistance to
Pollutant performance has very big improvement.
The present invention is compared with prior art, has following beneficial effect:
(1) MIL-101 (Cr)/GO provided by the present invention solves the problems, such as the collapsing of conventional metals organic backbone, is total to
The pure water flux of doughnut forward osmosis membrane and reversed flux salt prepared by mixed modification are obviously improved.
(2) side of doughnut forward osmosis membrane is blended in MIL-101 (Cr) provided by the present invention/GO blending and modifying preparation
Method, equipment used is simple, easily-controllable, film preparation simple process, assigns while film forming prepared forward osmosis membrane good infiltration
Performance, separating property, mechanical performance and antifouling property, it is easy to accomplish industrialization.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1:
By the cellulose acetate of 28.0%(w/w), 12.0%(w/w) polyethylene glycol-400,0.2%(w/w) surface-active
Agent, 0.8%(w/w) MIL-101 (Cr)/GO and 59.0%(w/w) mixed solvent that forms with acetone of N-Methyl pyrrolidone presses
It is added in dissolving tank according to certain sequence, dissolution 12 hours is sufficiently stirred at a temperature of 70 DEG C, and standing and defoaming is based on
MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane casting solution;Then, it is spinned and is blended using wet-dry change
Doughnut forward osmosis membrane, and the solidification forming into 25 DEG C of coagulating baths is pulled by winding-roller;By the doughnut of forming
Forward osmosis membrane is impregnated in deionized water at normal temperature after taking out, is rinsed 24 hours, is then heat-treated in 65 DEG C of deionized water
15mins is based on the acetyl cellulose blend doughnut forward osmosis membrane of metal organic framework MIL-101 (Cr)/GO to get arriving.
Driving liquid is done using 1M NaCl, deionized water does material liquid, prepared based on MIL-101 in the testing time of 1h
(Cr) pure water flux of/GO acetyl cellulose blend doughnut forward osmosis membrane reaches 27.0L/m2H or more, reversed salt
Flux is less than 0.5g/m2·h。
Embodiment 2:
The ratio of metal-organic framework materials MIL-101 (Cr)/GO, mixed solvent is adjusted to 0.1%(w/w), 59.7%
(w/w), remaining is the same as embodiment 1.It is then prepared based on MIL-101 (Cr)/GO acetyl cellulose blend doughnut
The performance of forward osmosis membrane are as follows: using 1M NaCl as driving liquid, deionized water as material liquid, in the testing time of 1h
In, pure water flux reaches 21.0L/m2H or more, reversed flux salt are less than 1.0g/m2•h。
Embodiment 3:
The ratio of metal-organic framework materials MIL-101 (Cr)/GO, mixed solvent is adjusted to 2.5%(w/w), 57.3%
(w/w), remaining is the same as embodiment 1.It is then prepared based on MIL-101 (Cr)/GO acetyl cellulose blend doughnut
The performance of forward osmosis membrane are as follows: using 1M NaCl as driving liquid, deionized water as material liquid, in the testing time of 1h
In, pure water flux reaches 25.5L/m2H or more, the reversed small 0.5g/m2 h of flux salt.
Embodiment 4:
Polyethylene glycol-400 in pore-foaming agent is changed to polyvinylpyrrolidone, remaining is the same as embodiment 1.It is then prepared
The performance based on MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane are as follows: using 1M NaCl make
It is driving liquid, deionized water as material liquid, in the testing time of 1h, pure water flux reaches 23.5L/m2H or more,
Reversed flux salt is less than 0.5g/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 prepared based on MIL-101
(Cr) performance of/GO acetyl cellulose blend doughnut forward osmosis membrane are as follows: using 1M NaCl as driving liquid, go from
Sub- water is as material liquid, and in the testing time of 1h, pure water flux reaches 29.0L/m2H or more, reversed flux salt are small
In 1.0g/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 prepared based on MIL-101
(Cr) performance of/GO acetyl cellulose blend doughnut forward osmosis membrane are as follows: using 1M NaCl as driving liquid, go from
Sub- water is as material liquid, and in the testing time of 1h, pure water flux reaches 23.5L/m2H or more, reversed flux salt are small
In 0.5g/m2•h。
Embodiment 7:
Heat treatment time is adjusted to 60mins by 15mins, remaining is the same as embodiment 1.It is then prepared based on MIL-
The performance of the acetyl cellulose blend doughnut forward osmosis membrane of 101 (Cr)/GO are as follows: using 1M NaCl as driving liquid,
Deionized water is as material liquid, and in the testing time of 1h, pure water flux reaches 25.0L/m2H or more, reversed salt are logical
Amount is less than 0.5g/m2•h。
Comparative example 1:
By the cellulose acetate of 27.0%(w/w), 12.0%(w/w) polyethylene glycol-400,0.2%(w/w) surface-active
Agent and 60.8%(w/w) N-Methyl pyrrolidone and acetone composition mixed solvent be added in dissolving tank in a certain order,
Dissolution 12 hours is sufficiently stirred at a temperature of 70 DEG C, and standing and defoaming obtains cellulose acetate doughnut forward osmosis membrane casting film
Liquid;Then, doughnut forward osmosis membrane is spinned using wet-dry change, and is pulled by winding-roller into 30 DEG C of coagulating baths and is solidified
Forming;It impregnates, rinse 24 hours in deionized water at normal temperature after the doughnut forward osmosis membrane of forming is taken out, then at 65 DEG C
Deionized water in heat treatment 20mins to get arrive cellulose acetate doughnut forward osmosis membrane.It is driven using 1M NaCl
Liquid, deionized water do material liquid, in the testing time of 1h, the pure water of prepared cellulose acetate doughnut forward osmosis membrane
Flux reaches 21.0L/m2H or more, reversed flux salt are less than 3.5g/m2·h。
Claims (5)
1. one kind is just permeated based on metal organic framework compound MIL-101 (Cr)/GO acetyl cellulose blend doughnut
Film, it is characterised in that: contain metal organic framework compound MIL-101 (Cr)/GO in its casting solution, and influence doughnut just
The structure and performance of permeable membrane;Based on MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane casting solution
The composition of formula are as follows: cellulose acetate 17 .0 ~ 35 .0%(w/w), pore-foaming agent 5 .0 ~ 20 .0%(w/w), surfactant 0
.05 ~ 2.0%(w/w), MIL-101 (Cr)/0.8 ~ 2.5%(w/w of GO), remaining is mixed solvent;
The pore-foaming agent is polyethylene glycol-400;
It is described to be based on metal organic framework compound MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane
Preparation method the following steps are included:
(1) preparation of the acetyl cellulose blend doughnut forward osmosis membrane casting solution based on MIL-101 (Cr)/GO:
Selecting cellulose diacetate or Triafol T is membrane material, and Tween-80 is surfactant, and polyethylene glycol-400 is
Pore-foaming agent, metal organic framework compound MIL-101 (Cr)/GO are formed as additive, N-Methyl pyrrolidone and acetone
Mixed solvent is added separately in dissolving tank as solvent, and stirring and dissolving 5 ~ 16 hours is to sufficiently at a temperature of 25 ~ 90 DEG C
It is even, prepare casting solution;Then, obtained casting solution is static at a temperature of stirring and dissolving to place 3 ~ 16 hours, remove casting solution
The bubble of middle remaining obtains the acetyl cellulose blend doughnut forward osmosis membrane casting solution based on MIL-101 (Cr)/GO;
(2) spinning of the acetyl cellulose blend doughnut forward osmosis membrane based on MIL-101 (Cr)/GO:
Keeping forward osmosis membrane casting solution temperature is 25 ~ 90 DEG C, and the pressure for adjusting metering pump is the .5MPa of 0 .05 ~ 0, by casting solution
It is squeezed into the annular space of spinning nozzle by metering pump and forms as-spun fibre, as-spun fibre leaves the air that spray head passes through 0 ~ 15cm
It behind gap, is pulled into the coagulating basin equipped with 15 ~ 60 DEG C of deionized waters through winding-roller, carries out 0 .5 ~ 5mins and be frozen into
Doughnut forward osmosis membrane is blended in shape, spinning;
(3) post-process: immersion, flushing 12~48 are small in deionized water at normal temperature after the doughnut forward osmosis membrane of forming is taken out
When, change a water within every 4~8 hours;Then 10 ~ 60mins is heat-treated in 30 ~ 90 DEG C of deionized water to get to based on metal
Organic backbone compound MIL-101 (Cr)/GO acetyl cellulose blend doughnut forward osmosis membrane.
2. total based on metal organic framework compound MIL-101 (Cr)/GO cellulose acetate described according to claim 1
Mixed doughnut forward osmosis membrane, it is characterised in that: the forward osmosis membrane is spinned using traditional phase inversion i.e. dry-wet process
's.
3. total based on metal organic framework compound MIL-101 (Cr)/GO cellulose acetate described according to claim 1
Mixed doughnut forward osmosis membrane, it is characterised in that: MIL-101 (the Cr)/GO is self-control metal organic framework compound,
For blocky-shaped particle structure, content is 0.8 ~ 2.5%(w/w).
4. according to claim 1 total based on metal organic framework compound MIL-101 (Cr)/GO cellulose acetate
Mixed doughnut forward osmosis membrane, it is characterised in that: the surfactant is Tween-80, and content is the .0%(w/ of 0 .05% ~ 2
W).
5. according to claim 1 total based on metal organic framework compound MIL-101 (Cr)/GO cellulose acetate
Mixed doughnut forward osmosis membrane, it is characterised in that: the solvent is the mixed solvent that N-Methyl pyrrolidone and acetone form,
Its volume ratio is 1:0.2 ~ 10.0(v/v), content is 40.5 ~ 77 .85%(w/w).
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Thin-Film Nanocomposite (TFN) Membranes Incorporated with Super-Hydrophilic Metal-Organic Framework (MOF) UiO-66: Toward Enhancement of Water Flux and Salt Rejection;Dangchen Ma et al.;《Applied Materials & Interfaces》;20170210;第9卷(第8期);第7523-7532页 * |
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