CN110449043A - A kind of preparation method of the high-performance reverse osmosis membrane based on building Multi-network - Google Patents
A kind of preparation method of the high-performance reverse osmosis membrane based on building Multi-network Download PDFInfo
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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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
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Abstract
The invention belongs to reverse osmosis composite membrane technical field, a kind of high performance reverse osmosis membrane preparation method based on building Multi-network.The present invention first coats the aqueous solution containing dopamine and one or more water soluble polymers on polysulfones counterdie, so that dopamine autohemagglutination forms a film, water soluble polymer, which is mixed, forms three-dimensional net structure in poly bar amine film, after drying in the shade, it is coated with the aqueous phase solution containing polyamine, after drying in the shade, it is coated with the oil-phase solution that polynary acyl chlorides is dissolved in Isopar G (a kind of Isopars), then it will be post-processed at a certain temperature by the film of coating, finally obtained reverse osmosis membrane.It is an advantage of the invention that preparing reverse osmosis membrane by interfacial polymerization had not only maintained good rejection, but also water flux is greatly improved, reproducibility is preferable, and preparation cost is cheap.
Description
Technical field
The invention belongs to reverse osmosis composite membrane technical field, a kind of high performance reverse osmosis based on building Multi-network
Permeable membrane preparation method.
Background technique
The core of reverse osmosis technology is high performance reverse osmosis composite membrane, the function as seperation film technical foundation and core
Membrane material is always the emphasis of beauty, the development of Deng developed country membrane technology, the especially research to high-performance reverse osmosis composite membrane
The even more most important thing.Reverse osmosis membrane typically now is all the PA membrane obtained by interfacial polymerization.Polyamide reverse osmosis is multiple
Film is closed since its excellent separating property has become the mainstream applications film of current reverse osmosis membrane sea water desalination.Polyamide reverse osmosis
Saturating composite membrane is formed by 3 layers: ultra-thin polyamide active layer；Poroid polysulfones (PSf) supporting layer；Non-woven fabrics mechanical support layer.
Fine and close surface-active layer provides excellent separating property, and polysulfone supporting layer provides good platform, mechanics for surface-active layer
Supporting layer provides good mechanical support.Relative to other reverse osmosis membranes, polyamide reverse osmosis composite film has apparent advantage,
But the problem of still facing 3 aspects: relationship, film surface pollution and the chlorine limited mutually between flux and salt ion rejection
Oxidation etc..There is the relationship (Trade-to check and balance between the flux and salt ion rejection of polyamide reverse osmosis composite film
Off): under the premise of operating pressure is constant, the flux of film can be realized by reducing the degree of cross linking and the thickness of aramid layer,
But the raising of membrane flux can reduce salt ion rejection.Improve flux and the salt ion retention of film simultaneously by the modification to film
Rate is the bottleneck problem that current polyamide reverse osmosis composite film faces, this is also an importance for reducing its energy consumption.
The present invention not only increases the water flux of composite membrane, also increases by separating the extremely hydrophilic network structure of layer building in function
Various salt ions in a network by resistance, increase the rejection of composite membrane.With the network of traditional polyamide separating layer
Structure is different, before network structure of the invention is implemented in water phase coating, just constructs one layer of three-dimensional before polysulfones counterdie coats water phase
Network structure, this deep layer for not only contributing to water phase are impregnated with so that generate polyamide separating layer it is finer and close with it is complete, and
And due to the network structure of building and its hydrophilic, the water flux lost since aramid layer is too fine and close is compensated for.Dopamine
(DOPA) research hotspot that current material surface modifying is had become from poly- complex technique of bionic adhesion, but utilize this technology
Network structure is constructed, and the research for further preparing reverse osmosis membrane is less.
The present invention is utilized from poly- complex technique, and under alkaline environment, DOPA and water-soluble macromolecule mixed solution can be in solids
Surface auto polymerization, DOPA form strength and are attached to the PDOPA layer of counterdie, and long chain macromolecule is mixed at PDOPA layers, are formed
Three-dimensional net structure.Then polyamide reverse osmose membrane is prepared again and improves retention and the flux of reverse osmosis membrane, has obtained high property
It can reverse osmosis composite membrane.
Summary of the invention
The present invention is intended to provide a kind of high performance reverse osmosis membrane preparation method based on building Multi-network.Originally it grinds
Study carefully and first coat dopamine and water-soluble macromolecule mixed solution in counterdie before water phase coats, therefore constructs three dimensional network on counterdie
Network.The preparation process of this high performance reverse osmosis membrane must first coating contains dopamine and one or more on polysulfones counterdie
The aqueous phase solution of water soluble polymer, so that dopamine autohemagglutination forms a film, water soluble polymer is mixed to be formed in poly bar amine film
Three-dimensional net structure is coated with the aqueous phase solution containing polyamine, is coated with polynary acyl chlorides and is dissolved in Isopar L (a kind of isomery
Alkane solvent) in oil-phase solution, reverse osmosis membrane is prepared by interfacial polymerization.It is excellent by being carried out to coating liquid each component and type
Change selection, post-processing temperature is regulated and controled, high-performance reverse osmosis membrane has been prepared.
The present invention is achieved through the following technical solutions:
A kind of high performance reverse osmosis membrane preparation method based on building Multi-network, it is characterized in that: first in polysulfones
The aqueous solution containing dopamine and one or more water soluble polymers is coated on counterdie, so that dopamine autohemagglutination forms a film, it is water-soluble
Property macromolecule mix and form three-dimensional net structure in poly bar amine film, after drying in the shade, be coated with the aqueous phase solution containing polyamine,
After drying in the shade, it is coated with the oil-phase solution that polynary acyl chlorides is dissolved in Isopar G (a kind of Isopars), it then will be by applying
The film covered is post-processed at a certain temperature, finally obtained reverse osmosis membrane.
Preferably, the aqueous solution of dopamine and water soluble polymer contains dopamine in above-mentioned preparation method, and contain
Polyvinyl alcohol (PVA), polyethyleneimine (PEI), one of polyethylene glycol (PEG) or a variety of.
Preferably, the macromolecule contained in aqueous phase solution in above-mentioned preparation method has m-phenylene diamine (MPD) (MPD), piperazine
(PIP), one of polyethyleneimine or a variety of, and the high molecule mass percentage in water phase is 0.1-5.0%.As more preferably
Selection, the macromolecule of aqueous phase solution is m-phenylene diamine (MPD) (MPD), and m-phenylene diamine (MPD) (MPD) mass percent is 0.1-3%.
Preferably, the macromolecule contained in oil-phase solution in above-mentioned preparation method has pyromellitic trimethylsilyl chloride (TMC), oneself two
Acyl chlorides (APC), one or more, and the solute polymer mass percent in oily phase of hexamethylene diisocyanate (HDI)
For 0.1-4.0%.As more preferably selecting, the macromolecule in oil-phase solution is pyromellitic trimethylsilyl chloride (TMC), and TMC mass percentage
Than for 0.1-3.5%.
Preferably, the post-processing temperature of composite membrane is 100 DEG C -150 DEG C in above-mentioned preparation method.As more preferably selecting,
The post-processing temperature of reverse osmosis membrane is 110 DEG C -130 DEG C.
In the present invention, polysulfones counterdie can be the counterdie that any producer provides, the type of the performance difference of counterdie, counterdie
Result of the invention is had no and is directly affected, therefore can choose business polysulfones counterdie or self-control, this is also of the invention general
Logical applicable, progress commercial applications provide possibility.
In the present invention, the raw material of this reverse osmosis membrane preparation is easy to get, and water phase each component is all highly soluble in water, in life
Any one production technology for changing production line is completely dispensed in producing line production process, thus also for it is of the invention it is generally suitable,
It carries out commercial applications and provides possibility.
The post-processing temperature of reverse osmosis membrane can be controlled by baking oven, and especially at 110 DEG C -130 DEG C, performance is more excellent
More.
The utility model has the advantages that using this patent the method, first coating contains dopamine and one or more on polysulfones counterdie
The aqueous phase solution of water soluble polymer, so that dopamine autohemagglutination forms a film, water soluble polymer is mixed to be formed in poly bar amine film
Three-dimensional net structure is coated with the aqueous phase solution containing polyamine, is coated with polynary acyl chlorides and is dissolved in Isopar L (a kind of isomery
Alkane solvent) in oil-phase solution, reverse osmosis membrane is prepared by interfacial polymerization and had not only maintained good rejection, but also is greatly improved
Water flux, reproducibility is preferable, and preparation cost is cheap.
Specific embodiment
A specific embodiment of the invention is illustrated below:
Following embodiment provides a kind of high performance reverse osmosis membrane preparation method based on building Multi-network.
Following embodiments are merely provided as explanation rather than limiting the invention.
Polysulfones counterdie used in following embodiment is self-control counterdie.The film date of manufacture to experiment the date less than 30 days, the phase
Between be stored in 2% aqueous solution of sodium bisulfite.Before carrying out interfacial reaction and preparing composite membrane, for 24 hours in advance by polysulfones counterdie
It is soaked in pure water.
A kind of film properties of high performance reverse osmosis membrane based on building Multi-network are made in following embodiment
Evaluation: sodium chloride salt rejection rate and water flux.Test pressure when performance evaluation is 1.05MPa, and concentrated water flow is 1.0L/min, ring
Border temperature is 25 DEG C, and concentrated water pH value is 6.5~7.5, and concentrated water is sodium-chloride water solution, concentration 1000ppm.
In following embodiment, salt rejection rate is defined as concentrated water and produces the difference of the concentration of water divided by concentrated water concentration；Water flux definition
For water volume of the unit time through unit area composite separating film, unit L/m in above-mentioned test process2·h(LMH)。
Each of the above data point is averaged to obtain by 9 samples.
Comparative example
Counterdie is coated without dopamine and water soluble polymer mixed liquor, directly coats water phase, and oil is coated with after drying in the shade
Phase solution, is prepared for polyamide reverse osmose membrane.It is tested by experiment, prepared reverse osmosis membrane is to 1000ppm aqueous sodium chloride
The rejection of liquid is up to 99.5%, and water flux is up to 53LMH.Test pressure when performance evaluation is 1.05MPa, concentrated stream
Amount is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5~7.5, and concentrated water is sodium-chloride water solution, and concentration is
1000ppm。
Embodiment 1
The PVA aqueous solution of the DOPA of configuration quality score 0.5% and 0.5% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 65LMH, salt rejection rate
It is 99.7%.
Embodiment 2
The PVA aqueous solution of the DOPA of configuration quality score 0.7% and 0.5% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 69LMH, salt rejection rate
It is 99.7%.
Embodiment 3
The PVA aqueous solution of the DOPA of configuration quality score 0.5% and 0.8% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 66LMH, salt rejection rate
It is 99.7%.
Embodiment 4
The PEI aqueous solution of the DOPA of configuration quality score 0.5% and 0.5% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 70LMH, salt rejection rate
It is 99.7%.
Embodiment 5
The PVA aqueous solution of the DOPA of configuration quality score 0.5% and 1% is coated on polysulfones counterdie in advance.After drying in the shade,
The m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride that mass fraction 2% is added, 0.5% triethylamine,
It is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution, uniformly
Coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput sea based on new buffer system of method preparation
Moisture film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, concentrated water pH value is 6.5~
7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 75LMH, and salt rejection rate is
99.7%.
Embodiment 6
The PVA aqueous solution of the DOPA of configuration quality score 0.5% and 0.8% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 71LMH, salt rejection rate
It is 99.7%.
Embodiment 7
The PVA aqueous solution of the DOPA of configuration quality score 0.6% and 0.5% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 71LMH, salt rejection rate
It is 99.6%.
Embodiment 8
The PVA aqueous solution of the DOPA of configuration quality score 0.8% and 0.8% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 69LMH, salt rejection rate
It is 99.8%.
Embodiment 9
The PEG aqueous solution of the DOPA of configuration quality score 0.5% and 0.5% is coated on polysulfones counterdie in advance.It dries in the shade
Afterwards, the m-phenylene diamine (MPD) aqueous solution of configuration quality score 2% and the triethylamine hydrochloride of mass fraction 2% is added, 0.5% three second
Amine is uniformly mixed, is coated uniformly on diaphragm.After drying in the shade, it is reconfigured 0.2% pyromellitic trimethylsilyl chloride (TMC) oil-phase solution,
It is even to be coated on diaphragm, and 5min is heat-treated in 120 DEG C of baking ovens.Thus the high throughput based on new buffer system of method preparation
Seawater film is 1.05MPa in test pressure, and concentrated water flow is 1.0L/min, and environment temperature is 25 DEG C, and concentrated water pH value is 6.5
~7.5, concentrated water is sodium-chloride water solution, and concentration is under the experiment condition of 1000ppm, and measuring its water flux is 73LMH, salt rejection rate
It is 99.7%.
Claims (8)
1. a kind of preparation method of the high-performance reverse osmosis membrane based on building Multi-network, it is characterized in that: first at polysulfones bottom
The aqueous solution containing dopamine and one or more water soluble polymers is coated on film, after drying in the shade；Re-coating contains polyamine
Aqueous phase solution, then after drying in the shade；It is coated with the oil-phase solution that polynary acyl chlorides is dissolved in Isopar G, then by the film by coating
It is post-processed at a certain temperature, finally obtained reverse osmosis membrane.
2. a kind of preparation method according to claim 1, it is characterized in that: in the aqueous solution of the water soluble polymer
Water soluble polymer is one of polyvinyl alcohol, polyethyleneimine or polyethylene glycol or a variety of.
3. a kind of preparation method according to claim 1, it is characterized in that: the polyamine in the aqueous phase solution is isophthalic two
One of amine, piperazine or polyethyleneimine are a variety of；And the mass percent of the polyamine in aqueous phase solution is 0.1-
5.0%.
4. a kind of preparation method according to claim 3, it is characterized in that: as more preferably selecting, in the aqueous phase solution
Polyamine is m-phenylene diamine (MPD), and the mass percent of m-phenylene diamine (MPD) is 0.1-3%.
5. a kind of preparation method according to claim 1, it is characterized in that: polynary acyl chlorides is equal benzene three in the oil-phase solution
Formyl chloride, Adipoyl Chloride or hexamethylene diisocyanate it is one or more, and in oily phase polynary acyl chlorides mass percent
For 0.1-4.0%.
6. a kind of preparation method according to claim 5, it is characterized in that: the polynary acyl chlorides in the oil-phase solution is equal benzene
Three formyl chlorides, and the mass percent of pyromellitic trimethylsilyl chloride is 0.1-3.5%.
7. a kind of preparation method according to claim 1, it is characterized in that: the post-processing temperature of the composite membrane be 100 DEG C-
150℃。
8. a kind of preparation method according to claim 7, it is characterized in that: the post-processing temperature of the composite membrane be 110 DEG C-
130℃。
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| CN109499395A (en) * | 2018-11-16 | 2019-03-22 | 杭州华滤膜科技有限公司 | A kind of preparation method of the reverse osmosis seawater film of high throughput |
| CN109675440A (en) * | 2018-11-16 | 2019-04-26 | 杭州水处理技术研究开发中心有限公司 | A kind of preparation method of the reverse osmosis seawater film of high-performance |
| CN110302685A (en) * | 2019-06-13 | 2019-10-08 | 浙江特分环境技术有限公司 | A kind of high performance reverse osmosis membrane preparation method based on building Multi-network |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109499395A (en) * | 2018-11-16 | 2019-03-22 | 杭州华滤膜科技有限公司 | A kind of preparation method of the reverse osmosis seawater film of high throughput |
| CN109675440A (en) * | 2018-11-16 | 2019-04-26 | 杭州水处理技术研究开发中心有限公司 | A kind of preparation method of the reverse osmosis seawater film of high-performance |
| CN110302685A (en) * | 2019-06-13 | 2019-10-08 | 浙江特分环境技术有限公司 | A kind of high performance reverse osmosis membrane preparation method based on building Multi-network |
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Application publication date: 20191115 |