CN110385047A - A method of high-flux reverse osmosis membrane is prepared with graphene oxide chloride product - Google Patents
A method of high-flux reverse osmosis membrane is prepared with graphene oxide chloride product Download PDFInfo
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- CN110385047A CN110385047A CN201811648698.2A CN201811648698A CN110385047A CN 110385047 A CN110385047 A CN 110385047A CN 201811648698 A CN201811648698 A CN 201811648698A CN 110385047 A CN110385047 A CN 110385047A
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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
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/025—Reverse osmosis; Hyperfiltration
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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
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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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Abstract
A method of high-flux reverse osmosis membrane is prepared with graphene oxide chloride product.It is related to preparing the method for reverse osmosis membrane.Provide a kind of preparation method of reverse osmosis membrane with high pass flow characteristic.The principle of the present invention carries out chloride processing by the graphene oxide to appropriate piece diameter, then graphene oxide chloride product is added in oil-phase solution, a certain proportion of mixed solution is formed with aromatic polyfunctional's acyl chlorides, it is reacted with this, in interfacial polymerization process, many sites on reverse osmosis membrane surface can be uniform-distribution with graphene oxide, realize that the purpose of raising reverse osmosis membrane performance, the present invention provide a kind of method for preparing high-flux reverse osmosis membrane with graphene oxide chloride product with this.
Description
Technical field
The present invention relates to the methods for preparing reverse osmosis membrane, more particularly to one kind to prepare height with graphene oxide chloride product
The method of flux RO membrane.
Background technique
Reverse osmosis membrane is widely used in water treatment field, and present commercial film is largely polyamide composite film.Such as often
Polyamide reverse osmose membrane, technical principle are cannot to penetrate under the action of being higher than solution osmotic pressure according to other substances
Semi-permeable membrane and these substances and water are separated.
The membrane aperture of reverse osmosis membrane is very small, thus can be effectively removed in water dissolved salts, colloid, microorganism,
Organic matter etc. has many advantages, such as good water quality, low, the pollution-free, simple process of energy consumption, easy to operate.
Existing reverse osmosis membrane is usually prepared by interfacial polymerization method, and desalination layer material is usually polyamide.
Graphene is the planar materials with single layer atomic structure of discovered in recent years, in general, the carbon-to-carbon of graphene
Chemical bond is highly stable, has the carbon atom of missing in unmanned discovery graphene so far, therefore chemical property is sufficiently stable, but its
Edge is rich in dangling bond, defect, and especially the actually edge of graphene and basal plane is not completely reduced there is also certain amount
Oxygen-containing functional group (for the material of graphite oxide approach preparation), therefore there is the energy chemically reacted with other organic molecules
Power.For example, the surface and edge of graphene oxide (graphene oxide) are rich in hydroxyl, carboxyl and epoxy group etc.
The oxygen-containing functional group of high reaction activity, can using graphene oxide as precursor using its surface reactive group abundant into
Then row surface chemical modification is restored again and prepares different Graphene derivatives.However, the prior art be usually pass through by
Graphene is added in polyamide reverse osmose membrane preparation process, because of the size of graphene and polyamide reverse osmose membrane desalination layer
Thickness is in an order of magnitude, so extremely be easy to causeing defect, so that the salt rejection rate of reverse osmosis membrane be made to decline to a great extent, this is greatly limited
Application of the graphene on reverse osmosis membrane is made.
106268379 A of Chinese invention patent application CN discloses a kind of polyamide that chloride graphene oxide is modified
Supporting course is immersed in the aqueous phase solution containing multifunctional aromatic amine compound, then soaks by the preparation method of reverse osmosis membrane
Bubble is in the oil-phase solution of polyfunctional group acyl chlorides；Then containing graphene and thionyl chloride changing in Isopars are immersed in
Property agent solution, wherein the graphene is single-layer graphene or single-layer graphene oxide；The chloride oxidation is obtained after drying
The modified polyamide reverse osmose membrane of graphene.
The above method impregnates graphene oxide chloride on aramid layer surface and produces after the completion of interfacial polymerization process
The solution (being uniformly coated on chloride graphene oxide modifying agent on the reverse osmosis membrane that step (2) obtains) of object；Interfacial polymerization
In the process, the concentration of free aminated compounds is 10-20 times of acyl chlorides, and graphene oxide chloride product is coated on without place
On the reverse osmosis membrane of reason, these chloride products preferentially can be combined by excessive unreacted free aminated compounds, cause
Have high-throughput effect with the film that this method produces to have a greatly reduced quality.
Summary of the invention
The present invention is in view of the above problems, provide a kind of preparation method of reverse osmosis membrane with high pass flow characteristic.
The technical scheme is that method includes the following steps:
1) preparation contains the modifying agent of 0.1g/L graphene oxide and 0.1-lg/L thionyl chloride in Isopars
Thionyl chloride revolving after mixing, is eliminated in -0.1Mpa to -0.03Mpa, 50 DEG C -80 DEG C, obtains graphene oxide acyl by solution
Chlorizate；
2) it takes multifunctional aromatic amine compound to be dissolved in the water, obtains the water of 0.5%-10% by weight percentage
Supporting layer is immersed in the aqueous phase solution by phase solution, and the extra aqueous phase solution of support layer surface is removed after taking-up；
3) miscella that the product of step 2) is immersed in polyfunctional group acyl chlorides and graphene oxide chloride product is mixed
In liquid, the mixed solution is the polyfunctional group acyl chlorides and by weight percentage of 0.1%-2% by weight percentage
The solution of the graphene oxide chloride product of 0.001-0.01% in organic solvent removes the oily phase of excess surface after taking-up
Solution, oil-phase solution obtain reverse osmosis membrane after volatilizing；
4) reverse osmosis membrane that step 3) obtains is dried at 60 DEG C-l00 DEG C 80-600s, obtains the chloride oxidation
The modified polyamide reverse osmose membrane of graphene.
The multifunctional aromatic amine of step 2) is selected from m-phenylene diamine (MPD), p-phenylenediamine or o-phenylenediamine.
The supporting layer of step 2) is polysulfone ultrafiltration membrane.
The mixed solution of step 3) includes the chloride product of polyfunctional group acyl chlorides and graphene oxide；Polyfunctional group acyl chlorides
Selected from one of pyromellitic trimethylsilyl chloride, paraphthaloyl chloride, m-phthaloyl chloride or o-phthaloyl chloride or multiple compounds
Mixture.
The organic solvent of step 3) is selected from normal hexane, hexamethylene, mixing one of isoparaffin or normal heptane or a variety of
The mixture of organic solvent.
The average piece diameter of the graphene of step 1) is 300nm.Single-layer graphene oxide (Graphene Oxide) is often referred to
A kind of two-dimentional carbon material constituted by one layer with the periodically closelypacked carbon atom of benzene ring structure.They are under scanning electron microscope mirror
In the form of sheets, usually show the size of the material by " average piece diameter ".
The Isopars of step 1) are selected from Isopar E or Isopar G；
Application of the reverse osmosis membrane that preparation method described in any claim obtains in water process.
Reverse osmosis membrane of the invention is taken off in pressure 150psi, with 2000ppm sodium-chloride water solution to measure it for feed liquid
Salt rate is greater than 99.6%, and measuring its water flux is 50-75LMH.
The principle of the present invention carries out chloride processing by the graphene oxide to appropriate piece diameter, then by graphene oxide
Chloride product is added in oil-phase solution, forms a certain proportion of mixed solution with aromatic polyfunctional's acyl chlorides, anti-with this
It answers, in interfacial polymerization process, many sites on reverse osmosis membrane surface can be uniform-distribution with graphene oxide, be mentioned with this to realize
The purpose of high reverse osmosis membrane performance, the present invention, which provides, a kind of prepares high-flux reverse osmosis membrane with graphene oxide chloride product
Method.
Detailed description of the invention
Fig. 1 is the preparation process schematic diagram of graphene oxide chloride product,
Specific embodiment
The present invention is as shown in Figure 1；Following embodiment for explaining technical solution of the present invention without limitation.This field skill
Art personnel can use for reference the content of present invention, and the links such as appropriate feed change, parameter realize that corresponding other purposes, correlation change
All without departing from the contents of the present invention, all similar substitutions and modifications are apparent to those skilled in the art
, it should all be deemed to be included within the scope of the present invention.In the present invention, unless otherwise specified, term " part " is attached most importance to
Part is measured, " % " or " percentage " is weight percentage.
A method of high-flux reverse osmosis membrane being prepared with graphene oxide chloride product, this method includes following step
It is rapid:
1) preparation contains the modifying agent of 0.1g/L graphene oxide and 0.1-lg/L thionyl chloride in Isopars
Thionyl chloride revolving after mixing, is eliminated in -0.1Mpa to -0.03Mpa, 50 DEG C -80 DEG C, obtains graphene oxide acyl by solution
Chlorizate；
2) it takes multifunctional aromatic amine compound to be dissolved in the water, obtains the water of 0.5%-10% by weight percentage
Supporting layer is immersed in the aqueous phase solution by phase solution, and the extra aqueous phase solution of support layer surface is removed after taking-up；
3) miscella that the product of step 2) is immersed in polyfunctional group acyl chlorides and graphene oxide chloride product is mixed
In liquid, the mixed solution is the polyfunctional group acyl chlorides and by weight percentage of 0.1%-2% by weight percentage
The solution of the graphene oxide chloride product of 0.001-0.01% in organic solvent removes the oily phase of excess surface after taking-up
Solution, oil-phase solution obtain reverse osmosis membrane after volatilizing；
4) reverse osmosis membrane that step 3) obtains is dried at 60 DEG C-l00 DEG C 80-600s, obtains the chloride oxidation
The modified polyamide reverse osmose membrane of graphene.
The multifunctional aromatic amine of step 2) is selected from m-phenylene diamine (MPD), p-phenylenediamine or o-phenylenediamine.
The supporting layer of step 2) is polysulfone ultrafiltration membrane.
The mixed solution of step 3) includes the chloride product of polyfunctional group acyl chlorides and graphene oxide；Polyfunctional group acyl chlorides
Selected from one of pyromellitic trimethylsilyl chloride, paraphthaloyl chloride, m-phthaloyl chloride or o-phthaloyl chloride or multiple compounds
Mixture.
The organic solvent of step 3) is selected from normal hexane, hexamethylene, mixing one of isoparaffin or normal heptane or a variety of
The mixture of organic solvent.
The average piece diameter of the graphene of step 1) is 300nm.
The Isopars of step 1) are selected from Isopar E or Isopar G；
Embodiment l
Aqueous phase solution: 0.5 weight % m-phenylene diamine (MPD) aqueous solution
Oil-phase solution: the normal hexane solution of 0.1 weight % pyromellitic trimethylsilyl chloride
Prepare modifying agent: the Isopar E of the graphene oxide+0.5g/L thionyl chloride of configuration 0.05g/L piece diameter 50nm is molten
Liquid is boiled off in -0.l MPa, 70 DEG C of backspins except thionyl chloride obtains the chloride product of graphene oxide after mixing.
Polysulfone ultrafiltration membrane is impregnated into 20s in aqueous phase solution, removes redundant solution after taking-up；It is impregnated in oil-phase solution again
20s removes redundant solution after taking-up；120s is impregnated in modifying agent again, then dries 240s at 60 DEG C, obtains chloride oxygen
The modified polyamide reverse osmose membrane l of graphite alkene.
Embodiment 2
Aqueous phase solution: 1.0 weight % m-phenylene diamine (MPD) aqueous solutions
Oil-phase solution: the normal hexane solution of 0.5 weight % pyromellitic trimethylsilyl chloride
Prepare modifying agent: the Isopar E of the graphene oxide+0.5g/L thionyl chloride of configuration 0.l g/L piece diameter 50nm is molten
Liquid is boiled off in -0.l MPa, 70 DEG C of backspins except thionyl chloride obtains the chloride product of graphene oxide after mixing.
Polysulfone ultrafiltration membrane is impregnated into 20s in aqueous phase solution, removes redundant solution after taking-up；It is impregnated in oil-phase solution again
20s removes redundant solution after taking-up；120s is impregnated in modifying agent again, then dries 240s at 60 DEG C, obtains chloride oxygen
The modified polyamide reverse osmose membrane 2 of graphite alkene.
Embodiment 3
Aqueous phase solution: 5.0 weight % m-phenylene diamine (MPD) aqueous solutions
Oil-phase solution: the normal hexane solution of 1.0 weight % pyromellitic trimethylsilyl chlorides
Prepare modifying agent: the Isopar E of the graphene oxide+0.5g/L thionyl chloride of configuration 0.l5g/L piece diameter 50nm is molten
Liquid is boiled off in -0.l MPa, 70 DEG C of backspins except thionyl chloride obtains the chloride product of graphene oxide after mixing.
Polysulfone ultrafiltration membrane is impregnated into 20s in aqueous phase solution, removes redundant solution after taking-up；It is impregnated in oil-phase solution again
20s removes redundant solution after taking-up；120s is impregnated in modifying agent again, then dries 240s at 60 DEG C, obtains chloride oxygen
The modified polyamide reverse osmose membrane 3 of graphite alkene.
Embodiment 4
Aqueous phase solution: 10.0 weight % m-phenylene diamine (MPD) aqueous solutions
Oil-phase solution: the normal hexane solution of 2.0 weight % pyromellitic trimethylsilyl chlorides
Prepare modifying agent: the Isopar E of the graphene oxide+0.5g/L thionyl chloride of configuration 0.2g/L piece diameter 50nm is molten
Liquid is boiled off in -0.l MPa, 70 DEG C of backspins except thionyl chloride obtains the chloride product of graphene oxide after mixing.
Polysulfone ultrafiltration membrane is impregnated into 20s in aqueous phase solution, removes redundant solution after taking-up；It is impregnated in oil-phase solution again
20s removes redundant solution after taking-up；120s is impregnated in modifying agent again, then dries 240s at 60 DEG C, obtains chloride oxygen
The modified polyamide reverse osmose membrane 4 of graphite alkene.
Comparative example
Aqueous phase solution: 5.0 weight % m-phenylene diamine (MPD) aqueous solutions
Oil-phase solution: the normal hexane solution of 1.0 weight % pyromellitic trimethylsilyl chlorides
Polysulfone ultrafiltration membrane is impregnated into 20s in aqueous phase solution, removes redundant solution after taking-up；It is impregnated in oil-phase solution again
20s removes redundant solution after taking-up；Then 240s is dried at 60 DEG C, obtains conventional polyamide reverse osmosis membrane.
Performance test:
Water flux and salt rejection rate measurement are carried out respectively to above 5 parts of reverse osmosis membranes, in pressure 150psi, with 2000ppm chlorine
Changing sodium water solution is to measure its salt rejection rate and water flux for feed liquid.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example | |
| Flux (LMH) | 60.5 | 74.8 | 65.2 | 51.3 | 37.4 |
| Salt rejection rate (%) | 98.2 | 97.5 | 98.5 | 99.3 | 99.5 |
As can be seen that this is mainly by aqueous phase solution and oil-phase solution although the water flux of each embodiment differs greatly
Composition influence.The water flux for the 50-75LMH that the reverse osmosis membrane of embodiment 1-4 has is considered to have good water
Flux and salt rejection rate.
As it can be seen that chloride graphene oxide is successfully grafted to poly- by the present invention by selection single-layer graphene oxide material
Sulfone ultrafiltration membrane surface, it can be ensured that reverse osmosis membrane keeps outstanding salt rejection rate while obtaining high-throughput.
Claims (7)
1. a kind of method for preparing high-flux reverse osmosis membrane with graphene oxide chloride product, which is characterized in that this method packet
Include following steps:
1) preparation is molten containing the modifying agent of 0.1g/L graphene oxide and 0.1-lg/L thionyl chloride in Isopars
Thionyl chloride revolving after mixing, is eliminated in -0.1 Mpa to -0.03Mpa, 50 °C -80 °C, obtains graphene oxide acyl by liquid
Chlorizate；
2) multifunctional aromatic amine compound is taken to be dissolved in the water, obtain by weight percentage 0.5% -10% water phase it is molten
Supporting layer is immersed in the aqueous phase solution by liquid, and the extra aqueous phase solution of support layer surface is removed after taking-up；
3) product of step 2) is immersed in the mixing oil-phase solution of polyfunctional group acyl chlorides and graphene oxide chloride product
In, the mixed solution is by weight percentage 0.1% -2% polyfunctional group acyl chlorides and 0.001- by weight percentage
The solution of 0.01% graphene oxide chloride product in organic solvent removes the oil-phase solution of excess surface, oil after taking-up
Phase solution obtains reverse osmosis membrane after volatilizing；
4) reverse osmosis membrane that step 3) obtains is dried under 60 °C-l00 °C 80-600s, obtains the chloride oxidation stone
The modified polyamide reverse osmose membrane of black alkene.
2. preparation method according to claim 1, which is characterized in that the multifunctional aromatic amine of step 2) is selected from isophthalic
Diamines, p-phenylenediamine or o-phenylenediamine.
3. preparation method according to claim 1, which is characterized in that the supporting layer of step 2) is polysulfone ultrafiltration membrane.
4. preparation method according to claim 1, which is characterized in that the mixed solution of step 3) includes polyfunctional group acyl
The chloride product of chlorine and graphene oxide；Polyfunctional group acyl chlorides is selected from pyromellitic trimethylsilyl chloride, paraphthaloyl chloride, isophthalic diformazan
The mixture of one of acyl chlorides or o-phthaloyl chloride or multiple compounds.
5. preparation method according to claim 1, which is characterized in that the organic solvent of step 3) is selected from normal hexane, hexamethylene
The mixture of alkane, mixing one of isoparaffin or normal heptane or a variety of organic solvents.
6. preparation method according to claim 1, which is characterized in that the average piece diameter of the graphene of step 1) is 300nm.
7. preparation method according to claim 1, which is characterized in that the Isopars of step 1) are selected from Isopar E
Or Isopar G.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110876897A (en) * | 2019-11-07 | 2020-03-13 | 恩泰环保科技（常州）有限公司 | High-flux anti-pollution nano hybrid reverse osmosis membrane and preparation method and application thereof |
| CN115245760A (en) * | 2022-01-07 | 2022-10-28 | 盐城工业职业技术学院 | Preparation method of emergency drinking nano-filtration purification membrane |
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| CN106076132A (en) * | 2016-06-27 | 2016-11-09 | 天津工业大学 | A kind of graphene oxide modified polyamide composite nanometer filtering film and preparation method thereof |
| CN106268379A (en) * | 2016-09-23 | 2017-01-04 | 北京碧水源膜科技有限公司 | The preparation method of the polyamide reverse osmose membrane that a kind of chloride graphene oxide is modified, described modified reverse osmosis membrane and application thereof |
| CN107297154A (en) * | 2017-06-05 | 2017-10-27 | 浙江工业大学 | A kind of carboxylated graphene oxide NF membrane and its preparation and application |
| US20180333685A1 (en) * | 2016-08-04 | 2018-11-22 | King Fahd University Of Petroleum And Minerals | Method for making a polygraphene membrane for water desalination |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106076132A (en) * | 2016-06-27 | 2016-11-09 | 天津工业大学 | A kind of graphene oxide modified polyamide composite nanometer filtering film and preparation method thereof |
| US20180333685A1 (en) * | 2016-08-04 | 2018-11-22 | King Fahd University Of Petroleum And Minerals | Method for making a polygraphene membrane for water desalination |
| CN106268379A (en) * | 2016-09-23 | 2017-01-04 | 北京碧水源膜科技有限公司 | The preparation method of the polyamide reverse osmose membrane that a kind of chloride graphene oxide is modified, described modified reverse osmosis membrane and application thereof |
| CN107297154A (en) * | 2017-06-05 | 2017-10-27 | 浙江工业大学 | A kind of carboxylated graphene oxide NF membrane and its preparation and application |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110876897A (en) * | 2019-11-07 | 2020-03-13 | 恩泰环保科技（常州）有限公司 | High-flux anti-pollution nano hybrid reverse osmosis membrane and preparation method and application thereof |
| CN110876897B (en) * | 2019-11-07 | 2022-05-03 | 恩泰环保科技（常州）有限公司 | High-flux anti-pollution nano hybrid reverse osmosis membrane and preparation method and application thereof |
| CN115245760A (en) * | 2022-01-07 | 2022-10-28 | 盐城工业职业技术学院 | Preparation method of emergency drinking nano-filtration purification membrane |
| CN115245760B (en) * | 2022-01-07 | 2023-03-10 | 盐城工业职业技术学院 | Preparation method of emergency drinking nano-filtration purification membrane |
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