CN108097059A - A kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide - Google Patents
A kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide Download PDFInfo
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- CN108097059A CN108097059A CN201810036612.4A CN201810036612A CN108097059A CN 108097059 A CN108097059 A CN 108097059A CN 201810036612 A CN201810036612 A CN 201810036612A CN 108097059 A CN108097059 A CN 108097059A
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- molybdenum disulfide
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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
- B01D69/10—Supported membranes; Membrane supports
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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
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/26—Electrical properties
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
A kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide, belongs to material modification field.The method is as follows：Configure molybdenum disulfide and m-phenylene diamine (MPD) mixed solution；Mixed solution is poured over polyether sulfone membrane surface, keeps 10min；Polyether sulfone basement membrane is taken out, is dried up with nitrogen；1,3,5 pyromellitic trimethylsilyl chloride hexane solution is poured into polyether sulfone membrane surface, makes the two fully reaction 1min；Polyether sulfone basement membrane is taken out, is dried up with nitrogen, removes redundant solution；Film obtained is placed in the baking oven of 60oC, reacts 15min.It is an advantage of the invention that：Individual layer nano molybdenum disulfide has the bidimensional layer structure similar with graphene, only there are one nanometer thickness, has been covered with nano-pore, when carrying out sea water desalination and salt retains, substantial amounts of seawater can be leaked, leaves salinity and other compositions, achievees the purpose that desalinize seawater and salt retains.The method is simple for process, and it is convenient to prepare.
Description
Technical field
The invention belongs to material modification fields, and in particular to it is anti-that a kind of utilization molybdenum disulfide establishes aquaporin reinforced polyamide
Permeate the method for modifying of membrane flux.
Background technology
Reverse osmosis technology is a kind of technology new at this stage, it can be directed to the monovalence of small molecule, divalent salt particle into
Row retention, can be used for the fields such as brackish water desalination, Domestic water purifying, has very wide application prospect, is referred to as " 21 century
Water-purifying technique ".In all reverse osmosis membranes, polyamide reverse osmose membrane has preferable mechanical strength, and higher water leads to
Amount and the performance of salt retention, are most widely used, occupy the staple market of reverse osmosis membrane at present.Although polyamide reverse osmose membrane
Water flux and salt cutoff performance it is higher, but still the requirement of industrial treatment cannot be met, thus at this stage many researchers poly-
Some electrodeless nanometer constituent elements with pore structure are introduced in imido functional layer to improve the pore structure of reverse osmosis membrane, are utilized
The hole of inorganic nano constituent element establishes water flux structure in the functional layer of polyimides, increases water flux or salt retention so as to reach
Purpose, but the achievement obtained still cannot meet the requirement of industrial treatment.
The content of the invention
The purpose of the invention is to overcome reverse osmosis membrane in the prior art, existing water leads in use
Amount and salt retention need to further improve, it is impossible to which the problem of meeting practical application provides and a kind of established water using molybdenum disulfide and led to
The method of modifying of road reinforced polyamide reverse osmosis membrane water flux.
To achieve the above object, the technical solution that the present invention takes is as follows：
A kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide, the method are specific
Step is as follows：
Step 1：Configuration quality fraction is 0.005% ~ 0.2% molybdenum disulfide and 1 ~ 3% m-phenylene diamine (MPD) mixed solution；
Step 2：Mixed solution made from step 1 is poured over polyether sulfone membrane surface, keeps 10min；
Step 3：The mixed solution of polyether sulfone membrane surface in removal step two carries out 5min drying processing with nitrogen；
Step 4：By 1,3, the 5- pyromellitic trimethylsilyl chloride hexane solutions that mass fraction is 0.1% be poured into that step 3 obtains it is poly-
Ether sulfone membrane surface makes 1,3,5- pyromellitic trimethylsilyl chloride hexane solutions and polyether sulfone basement membrane fully react 1min；
Step 5：The 1 of polyether sulfone membrane surface in removal step four, 3,5- pyromellitic trimethylsilyl chloride hexane solutions, is blown with nitrogen
2min so that film surface is dried, and removes redundant solution；
Step 6：Film obtained in step 5 is placed in the baking oven of 60oC, reacts 15min, obtains molybdenum disulfide modification
Reverse osmosis membrane.
The present invention is compared with the advantageous effect of the prior art：
Individual layer nano molybdenum disulfide has the bidimensional layer structure similar with graphene, only there are one nanometer thickness, has been covered with nanometer
Hole when carrying out sea water desalination and salt retains, can leak substantial amounts of seawater, leave salinity and other compositions, reach desalination sea
Water and the purpose of salt retention.Further, since the charge between molybdenum atom and sulphur atom is redistributed, edge atom has
Charge, this charged edge is permeated for hydrone and selectively ion screening plays crucial effect.Molybdenum disulfide
This unique atom composition structure the water penetration of molybdenum disulfide film is allowed to greatly promote.Moreover, since it has and graphite
The identical layer structure of alkene when molybdenum disulfide is introduced into polyamide functional layer, can be built using layer structure in functional layer
Vertical aquaporin improves osmotic efficiency of the water in functional layer.Therefore, the atomic structure of molybdenum disulfide uniqueness, two-dimensional layered structure, receive
After polyamide functional layer is introduced into, it is anti-can synchronously to improve polyamide for metre hole structure and good hydrone conduction
The water flux of infiltration and salt cutoff performance.The method is simple for process, and it is convenient to prepare.Water flux improves 14.8 ~ 73.1%, retention
Rate improves 0.07 ~ 1.6%.
Description of the drawings
Fig. 1 is the water flux of different reverse osmosis membranes and rejection figure.
Specific embodiment
Technical scheme is described further with reference to the accompanying drawings and examples, but is not limited thereto, it is all
It is technical solution of the present invention to be modified or equivalent substitution, without departing from the scope of technical solution of the present invention, should all contains
It covers among protection scope of the present invention.
Graphene surface is rich in substantial amounts of active group, and has two-dimensional layered structure, and many researchers are introduced into instead
Permeable membrane functional layer, with the monoatomic layer two dimensional surface and nano-pore structure of graphene uniqueness, using its bidimensional interlayer spacings and
Surface defect establishes aquaporin structure, enhances water flux and the retention of reverse osmosis membrane.Molybdenum disulfide has and ten split-phase of graphene
As two-dimensional structure, only there are one nanometer thickness, be covered with nano-pore, substantial amounts of seawater can be leaked, leave salinity and other into
Point, achieve the purpose that desalinize seawater.In addition, molybdenum disulfide unique atom composition structure allow molybdenum disulfide film water penetration significantly
It is promoted.The present invention introduces individual layer nano molybdenum disulfide, the charged edge knot of molybdenum disulfide in polyamide reverse osmose membrane functional layer
Structure is conducive to capture water and retains salt particle, while it has the layer structure similar with graphene oxide, can be reverse osmosis
Film functional layer establishes aquaporin, so as to achieve the purpose that the synchronous increase water flux of reverse osmosis membrane and salt cutoff performance.
Individual layer nanometer thickness has been covered with nano-pore by the present invention, has the nano molybdenum disulfide film that unique atom forms structure
PA membrane functional layer is introduced into, utilizes the atomic structure of molybdenum disulfide uniqueness, two-dimensional layered structure, nano-pore structure and good
Hydrone conduction, improve the water flux of polyamide reverse osmosis and salt cutoff performance.Moreover, since molybdenum disulfide has
There is the layer structure identical with graphene oxide, after molybdenum disulfide is added in aramid layer, water can be established in aramid layer
Passage improves water flux and salt retention efficiency.Therefore, after molybdenum disulfide being introduced PA membrane, water flux can synchronously be improved
And salt-stopping rate.
Specific embodiment one：What present embodiment was recorded is that a kind of utilization molybdenum disulfide establishes aquaporin reinforced polyamide
The method of modifying of reverse osmosis membrane water flux, the method are as follows：
Step 1：Configuration quality fraction is 0.005% ~ 0.2% molybdenum disulfide and 1 ~ 3% m-phenylene diamine (MPD) mixed solution；
Step 2：Mixed solution made from step 1 is poured over polyether sulfone membrane surface, keeps 10min；
Step 3：The mixed solution of polyether sulfone membrane surface in removal step two carries out 5min drying processing with nitrogen；
Step 4：By 1,3, the 5- pyromellitic trimethylsilyl chloride hexane solutions that mass fraction is 0.1% be poured into that step 3 obtains it is poly-
Ether sulfone membrane surface makes 1,3,5- pyromellitic trimethylsilyl chloride hexane solutions and polyether sulfone basement membrane fully react 1min；
Step 5：The 1 of polyether sulfone membrane surface in removal step four, 3,5- pyromellitic trimethylsilyl chloride hexane solutions, is blown with nitrogen
2min so that film surface is dried, and removes redundant solution；
Step 6：Film obtained in step 5 is placed in the baking oven of 60oC, reacts 15min, obtains molybdenum disulfide modification
Reverse osmosis membrane.
Specific embodiment two：A kind of utilization molybdenum disulfide described in specific embodiment one establishes aquaporin enhancing polyamides
The method of modifying of amine reverse osmosis membrane water flux, in step 1, the mass fraction of the molybdenum disulfide is 0.005% ~ 0.05%.
Specific embodiment three：A kind of utilization molybdenum disulfide described in specific embodiment one establishes aquaporin enhancing polyamides
The method of modifying of amine reverse osmosis membrane water flux, in step 1, the mass fraction of the m-phenylene diamine (MPD) is 2%.
Embodiment 1：
A kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide, the method are specific
Step is as follows：
Step 1：Configuration quality fraction is 0.005% molybdenum disulfide and 2% m-phenylene diamine (MPD) mixed solution；
Step 2：Mixed solution made from step 1 is poured over polyether sulfone membrane surface, keeps 10min；
Step 3：The mixed solution of polyether sulfone membrane surface in removal step two carries out 5min drying processing with nitrogen；
Step 4：By 1,3, the 5- pyromellitic trimethylsilyl chloride hexane solutions that mass fraction is 0.1% be poured into that step 3 obtains it is poly-
Ether sulfone membrane surface makes 1,3,5- pyromellitic trimethylsilyl chloride hexane solutions and polyether sulfone basement membrane fully react 1min；
Step 5：The 1 of polyether sulfone membrane surface in removal step four, 3,5- pyromellitic trimethylsilyl chloride hexane solutions, is blown with nitrogen
2min so that film surface is dried, and removes redundant solution；
Step 6：Film obtained in step 5 is placed in the baking oven of 60oC, reacts 15min, obtains molybdenum disulfide modification
Reverse osmosis membrane.
Step 7：Using the sodium chloride solution of 2000ppm as separating liquid, to modified reverse osmosis membrane in 15.5bar
Pressure under carry out flux and retention test.Before testing, precompressed causes the flux of sodium chloride and retention to stablize for one hour, so
The filtered fluid is taken to carry out the test of water flux and salt rejection rate, the water flux measured and salt retention afterwards as shown in Figure 1, unmodified membrane
Water flux is 1.08 Lm-2·h-1·bar-1, retention efficiency is 97.2%, and after molybdenum disulfide is added in, modified membrane flux
For 1.24 Lm-2·h-1·bar-1, retention efficiency is 97.9%.Adding in after molybdenum disulfide establishes fenestra passage, water flux and
Salt retention has a degree of increase, and the performance of modified caudacoria is promoted.
Embodiment 2：
A kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide, the method are specific
Step is as follows：
Step 1：Configuration quality fraction is 0.01% molybdenum disulfide and 2% m-phenylene diamine (MPD) mixed solution；
Step 2：Mixed solution made from step 1 is poured over polyether sulfone membrane surface, keeps 10min；
Step 3：The mixed solution of polyether sulfone membrane surface in removal step two carries out 5min drying processing with nitrogen；
Step 4：By 1,3, the 5- pyromellitic trimethylsilyl chloride hexane solutions that mass fraction is 0.1% be poured into that step 3 obtains it is poly-
Ether sulfone membrane surface makes 1,3,5- pyromellitic trimethylsilyl chloride hexane solutions and polyether sulfone basement membrane fully react 1min；
Step 5：The 1 of polyether sulfone membrane surface in removal step four, 3,5- pyromellitic trimethylsilyl chloride hexane solutions, is blown with nitrogen
2min so that film surface is dried, and removes redundant solution；
Step 6：Film obtained in step 5 is placed in the baking oven of 60oC, reacts 15min, obtains molybdenum disulfide modification
Reverse osmosis membrane.
Step 7：Using the sodium chloride solution of 2000ppm as separating liquid, to modified reverse osmosis membrane in 15.5bar
Pressure under carry out flux and retention test.Before testing, precompressed causes the flux of sodium chloride and retention to stablize for one hour, so
The filtered fluid is taken to carry out the test of water flux and salt rejection rate, the water flux measured and salt retention afterwards as shown in Figure 1, unmodified membrane
Water flux is 1.08 Lm-2·h-1·bar-1, retention efficiency is 97.2%, and after molybdenum disulfide is added in, the water of Modified Membrane leads to
It measures as 1.48 Lm-2·h-1·bar-1, retention efficiency is 98.8%.Compared with unmodified membrane, it is found that adding in two sulphur
After change molybdenum establishes fenestra passage, water flux and salt retention have a degree of increase, and the performance of modified caudacoria is promoted.
Embodiment 3：
A kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide, the method are specific
Step is as follows：
Step 1：Configuration quality fraction is 0.02% molybdenum disulfide and 2% m-phenylene diamine (MPD) mixed solution；
Step 2：Mixed solution made from step 1 is poured over polyether sulfone membrane surface, keeps 10min；
Step 3：The mixed solution of polyether sulfone membrane surface in removal step two carries out 5min drying processing with nitrogen；
Step 4：By 1,3, the 5- pyromellitic trimethylsilyl chloride hexane solutions that mass fraction is 0.1% be poured into that step 3 obtains it is poly-
Ether sulfone membrane surface makes 1,3,5- pyromellitic trimethylsilyl chloride hexane solutions and polyether sulfone basement membrane fully react 1min；
Step 5：The 1 of polyether sulfone membrane surface in removal step four, 3,5- pyromellitic trimethylsilyl chloride hexane solutions, is blown with nitrogen
2min so that film surface is dried, and removes redundant solution；
Step 6：Film obtained in step 5 is placed in the baking oven of 60oC, reacts 15min, obtains molybdenum disulfide modification
Reverse osmosis membrane.
Step 7：Using the sodium chloride solution of 2000ppm as separating liquid, to modified reverse osmosis membrane in 15.5bar
Pressure under carry out flux and retention test.Before testing, precompressed causes the flux of sodium chloride and retention to stablize for one hour, so
The filtered fluid is taken to carry out the test of water flux and salt rejection rate, the water flux measured and salt retention afterwards as shown in Figure 1, unmodified membrane
Water flux is 1.08 Lm-2·h-1·bar-1, retention efficiency is 97.2%, and after molybdenum disulfide is added in, the water of Modified Membrane leads to
It measures as 1.87 Lm-2·h-1·bar-1, retention efficiency is 98.6%.It can be found that establish fenestra passage adding in molybdenum disulfide
Afterwards, water flux and salt retention have a degree of increase, and the performance of modified caudacoria is promoted.
Claims (3)
1. a kind of method of modifying that aquaporin reinforced polyamide reverse osmosis membrane water flux is established using molybdenum disulfide, feature are existed
In：The method is as follows：
Step 1：Configuration quality fraction is 0.005% ~ 0.2% molybdenum disulfide and the m-phenylene diamine (MPD) mixed solution of 1-3%；
Step 2：Mixed solution made from step 1 is poured over polyether sulfone membrane surface, keeps 10min；
Step 3：The mixed solution of polyether sulfone membrane surface in removal step two carries out 5min drying processing with nitrogen；
Step 4：By 1,3, the 5- pyromellitic trimethylsilyl chloride hexane solutions that mass fraction is 0.1% be poured into that step 3 obtains it is poly-
Ether sulfone membrane surface makes 1,3,5- pyromellitic trimethylsilyl chloride hexane solutions and polyether sulfone basement membrane fully react 1min；
Step 5：The 1 of polyether sulfone membrane surface in removal step four, 3,5- pyromellitic trimethylsilyl chloride hexane solutions, is blown with nitrogen
2min so that film surface is dried, and removes redundant solution；
Step 6：The film obtained in step 5 is placed in the baking oven of 60oC, reacts 15min, obtains the anti-of molybdenum disulfide modification
Permeable membrane.
2. a kind of aquaporin reinforced polyamide reverse osmosis membrane water flux is established according to claim 1 using molybdenum disulfide
Method of modifying, it is characterised in that：In step 1, the mass fraction of the molybdenum disulfide is 0.005% ~ 0.05%.
3. a kind of aquaporin reinforced polyamide reverse osmosis membrane water flux is established according to claim 1 using molybdenum disulfide
Method of modifying, it is characterised in that：In step 1, the mass fraction of the m-phenylene diamine (MPD) is 2%.
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| CN109943310A (en) * | 2019-04-02 | 2019-06-28 | 侯吉瑞 | A kind of modified MoS2Nano material and preparation method thereof |
| CN110141976A (en) * | 2019-04-28 | 2019-08-20 | 浙江大学 | Anti-chlorine, antibacterial molybdenum disulfide/crosslinked hyperbranched polyalcohol composite nano filter membrance with photothermal conversion effect and preparation method thereof |
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| CN109943310B (en) * | 2019-04-02 | 2022-05-24 | 侯吉瑞 | Modified MoS2Nano material and preparation method thereof |
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| CN110141976A (en) * | 2019-04-28 | 2019-08-20 | 浙江大学 | Anti-chlorine, antibacterial molybdenum disulfide/crosslinked hyperbranched polyalcohol composite nano filter membrance with photothermal conversion effect and preparation method thereof |
| CN111359458A (en) * | 2020-04-03 | 2020-07-03 | 江西省科学院能源研究所 | Molybdenum disulfide oxide modified flat nanofiltration membrane as well as preparation method and application thereof |
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| CN113797770A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | Dopamine-modified molybdenum oxide-molybdenum disulfide-doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
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| CN113522045A (en) * | 2021-08-24 | 2021-10-22 | 河北工业大学 | Preparation method and application of molybdenum disulfide nanodot hybrid nanofiltration membrane |
| CN114887495A (en) * | 2022-04-27 | 2022-08-12 | 南京中医药大学 | Preparation method and application of modified dialysis membrane with alkylated composite molybdenum disulfide as modifier and trichosanthes kirilowii pulp starch as coating thickener |
| CN114887495B (en) * | 2022-04-27 | 2024-05-07 | 南京中医药大学 | Preparation method and application of modified dialysis membrane with alkylated composite molybdenum disulfide as modifier and trichosanthes kirilowii Maxim pulp starch as coating thickener |
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| US12040517B2 (en) | 2023-05-09 | 2024-07-16 | Rahul S. Nana | Reverse electrodialysis or pressure-retarded osmosis cell and methods of use thereof |
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| CN117225210B (en) * | 2023-09-20 | 2024-04-19 | 山东大学 | Method for preparing novel nanofiltration membrane by aid of amphiphilic molybdenum disulfide nanosheets |
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