CN106823826A - A kind of continuous preparation method of the compound forward osmosis membrane of high flux - Google Patents
A kind of continuous preparation method of the compound forward osmosis membrane of high flux Download PDFInfo
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- CN106823826A CN106823826A CN201710081934.6A CN201710081934A CN106823826A CN 106823826 A CN106823826 A CN 106823826A CN 201710081934 A CN201710081934 A CN 201710081934A CN 106823826 A CN106823826 A CN 106823826A
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- forward osmosis
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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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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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
- B01D61/002—Forward osmosis or direct osmosis
-
- 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
-
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
-
- 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
-
- 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
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
-
- 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
Abstract
A kind of continuous preparation method of the compound forward osmosis membrane of high flux, belongs to technical field of polymer separation membrane.The method specifically includes following steps：Backing material is under draw through the gap bilateral scraper, high concentration casting solution and low concentration casting solution are continuously coated using bilateral scraper in backing material both sides respectively, gained compound is by after air section, solidified forming in immersion coagulating bath obtains compound forward osmosis membrane support basement membrane；Interfacial polymerization is carried out in the high concentration casting solution coating side surface of the support basement membrane, the surface separation layer with cross-linked structure is formed, so as to compound forward osmosis membrane is obtained.The method can effectively improve the porosity of support basement membrane, form loose, porous, open bottom surface structure, so that the internal concentration polarization phenomenon in weakening supporting layer, improves the permeation flux of forward osmosis membrane.Additionally, the method process is simple, operation is easy, is suitable to industrialization.
Description
Technical field
The invention belongs to technical field of polymer separation membrane, and in particular to a kind of continuous system of the compound forward osmosis membrane of high flux
Preparation Method.
Background technology
Positive infiltration (FO) technology is, using naturally osmotic pressure, to make hydrone from pellicle side (material liquid side) to more
Opposite side (the drawing liquid side) infiltration of hyperosmosis, the method that then will be drawn liquid regeneration cycle and obtain fresh water.Therefore, just ooze
It is at ambient pressure the spontaneous membrane separating process for realizing Water transport of driving force with film both sides permeable pressure head to be thoroughly.With counter-infiltration (RO) phase
Than positive process of osmosis has low pressure even without press operation, low energy consumption, excellent desalting performance, low fouling membrane, high-recovery, zero-emission
The many advantages such as put.Positive infiltration technology is applied to the aspects such as desalinization, the processing of liquid food and drug products, is most latent
The Water warfare and desalting technology of power.Similar to reverse osmosis membrane, forward osmosis membrane is typically also made up of dense layer surface and porous support layer,
But the permeation flux of forward osmosis membrane is often limited by the concentration polarization effect occurred inside porous support layer.By ripe reverse osmosis
Permeable membrane is used for positive process of osmosis, tests and finds positive infiltration aquifer yield far below expection.Therefore, different from reverse osmosis membrane, positive infiltration
While possessing selective penetrated property, its support Rotating fields is needed to be optimized and showed with slowing down internal concentration polarization therein film
As.The supporting layer of high performance forward osmosis membrane should possess thinner thickness, porosity higher and lower empty tortuosity.
The preparation process of the supporting layer of forward osmosis membrane is usually that polymeric casting film liquid is compounded in into low-density backing material (such as
Fabric, non-woven fabrics, screen cloth of low-density etc.) surface, through coagulating bath solidified forming after, obtain composite support basement membrane.Patent
CN103182252B discloses exemplary complex forward osmosis membrane and preparation method thereof, and casting solution is coated in into low-density nonwoven fabric layer
On, inversion of phases obtains porous support layer in coagulation bath；Then on porous support layer, polynary amine aqueous solution has with polynary acyl chlorides
Machine solution reaction forms ultra-thin separating layer, so as to obtain including low-density nonwoven fabric layer, porous support layer and ultra-thin separating layer
Compound forward osmosis membrane with three-decker.This method prepares the subject matter that compound forward osmosis membrane is present：Casting solution pole
Easily penetrate into and even pass through low-density supporting layer, ultimately form thicker polymeric layer, be unfavorable for the raising of forward osmosis membrane flux.Specially
Sharp CN106215715A discloses a kind of preparation method of the compound forward osmosis membrane of high flux, is film forming substrate with porous material, will
Screen cloth is fixed in the film forming substrate of porous material, and polysulfones casting solution is coated on screen cloth, and phase turns in being then immersed in coagulation bath
Change obtains porous basement membrane；Interface polymerization reaction generation active separating layer is carried out in porous membrane surface.The porous knot of film forming substrate
Structure causes to be more likely formed the finger-like pore structure and open bottom surface structure for running through in basement membrane, so that interior in reducing positive process of osmosis
Concentration polarization phenomenon, improves the water flux of compound forward osmosis membrane.The method prepares compound forward osmosis membrane, and casting solution can still ooze
Screen cloth is crossed, is separated because the casting solution of screen cloth both sides is almost contacted with water simultaneously, easily form double cortexes.
In order to effectively reduce the gross thickness of forward osmosis membrane, weaken the internal concentration polarization phenomenon in supporting layer, raising is just oozed
The permeation flux of permeable membrane, preparation method disclosed in patent CN105617885A is：By the way of two-sided casting film, first loose
Backing material surface apply coated with full-bodied first casting solution and through coagulating bath solidified forming, then in gained compound support
Opposite side apply coated with low viscous second casting solution and through coagulating bath solidified forming, due to the presence of first polymer layer, have
Effect prevents the seepage of the second casting solution；After second polymer layer surface carries out interfacial polymerization, by first polymer layer from again
Stripping in structure is closed, relatively thin the second polymer layer has been obtained.The preparation method operation is various, and process is complicated, and the first polymerization
The stripping of nitride layer, recovery increased production cost, be unfavorable for industrialization.
The content of the invention
Regarding to the issue above, problem to be solved by this invention is to provide a kind of continuous system of the compound forward osmosis membrane of high flux
Preparation Method.Not only process is simple for the method, and operation is easy, and can effectively improve the porosity of support basement membrane, formed it is loose,
Porous, open bottom surface structure, so that the internal concentration polarization phenomenon in weakening supporting layer, the infiltration for improving forward osmosis membrane is led to
Amount.
A kind of continuous preparation method of the compound forward osmosis membrane of high flux, the method specifically includes following steps：
1) preparation of basement membrane is supported：Backing material under draw through the gap bilateral scraper, using bilateral
Scraper continuously coats casting solution, side coating high concentration casting solution, opposite side coating low concentration casting simultaneously in backing material both sides
Film liquid, gained compound is by after air section, solidified forming in immersion coagulating bath obtains compound forward osmosis membrane support basement membrane；
2) it is combined the preparation of forward osmosis membrane：Interface is carried out in the high concentration casting solution coating side surface of the support basement membrane to gather
Close, form the surface separation layer with cross-linked structure.
Further preferred, the backing material is non-woven fabrics, fabric or the screen cloth of low-density；The material of the non-woven fabrics
Including but not limited to polyester, nylon, polyethylene or polypropylene；The material of the fabric or screen cloth includes but is not limited to polyester, Buddhist nun
Dragon, polyethylene, polypropylene, stainless steel, glass fibre or carbon fiber；The thickness of the backing material is 30-150 μm, porosity
It is 50-95%.
Further, the device of above-mentioned coating casting solution is that backing material both sides are respectively the movable of parallel support material
Baffle plate (3), while be inclined scraper (4) below movable baffle plate (3), in the same side of backing material, movable baffle plate (3)
There is a space between scraper (4), pore size can be adjusted as needed.Bilateral scraper coordinates movable baffle controls casting solution
Coating thickness；Gap between the bilateral scraper is 50-200 μm；The movable baffle plate can upper and lower, inside and outside movement, use
With the release order or release amount of two kinds of casting solutions of control, so as to adjust two kinds of relative coating thickness of casting solution.
Further preferred, the high concentration casting solution and low concentration casting solution are by film forming polymer, solvent, additive
Composition, in its middle and high concentration casting solution film forming polymer, solvent, the mass fraction of additive be respectively 5-20%, 55-95%,
0-25%, film forming polymer, solvent, the mass fraction of additive are respectively 0-5%, 65-100%, 0- in low concentration casting solution
30%, it is 5% when film forming polymer is different with film forming polymer mass fraction in low concentration casting solution in high concentration casting solution.
Further preferred, the film forming polymer includes but is not limited to polysulfones, polyether sulfone, PEI, polypropylene
Nitrile, one kind of cellulose acetate or two of which and two or more mixtures, preferably polyacrylonitrile；The solvent include but not
It is limited to N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, 1-METHYLPYRROLIDONE, one kind of dimethyl sulfoxide (DMSO) or wherein two
Plant and two or more mixtures；The additive includes but is not limited to water, methyl alcohol, ethanol, ethylene glycol, glycerine, poly- second two
One kind or two of which and two or more mixtures in alcohol, polyvinylpyrrolidone, lithium chloride, lithium bromide, zinc chloride.
Further preferred, the coagulation bath composition is the mixture of water and the solvent, the wherein mass fraction of solvent
It is 0-50%, the temperature of the coagulating bath is 0-60 DEG C.
It is further preferred, in the interfacial polymerization process, successively using aqueous phase solution and organic phase solution, the water phase
Reaction monomers are polyamine, including but not limited to m-phenylene diamine (MPD), p-phenylenediamine, equal benzene triamine or piperazine, its quality point in solution
Number is 0.2-5%, and the solvent of the organic phase solution includes but is not limited to pentane, n-hexane, hexamethylene or petroleum ether, is reacted
Monomer is polynary acyl chlorides, including but not limited to pyromellitic trimethylsilyl chloride, and its mass fraction is 0.02-0.5%.
The present invention can obtain following Advantageous Effects：As a result of the backing material of low-density, casting solution easily oozes
Backing material is crossed, and bilateral scraper can effectively control the gross thickness of the compound forward osmosis membrane for ultimately forming, movable baffle plate energy
Enough control two kinds of relative coating thickness of casting solution.High concentration casting solution and low concentration casting solution are coated in backing material simultaneously
Both sides, can form the support basement membrane with different bilateral structures, and high concentration casting solution forms smooth flawless surface texture,
It is suitable as the matrix of interfacial polymerization；Low concentration casting solution forms loose porous open surface structure, can slow down positive infiltration
During internal concentration polarization phenomenon, improve forward osmosis membrane permeation flux and efficiency, especially in high concentration side, additive is adopted
Film can be further improved when using macromolecular material polyvinylpyrrolidone, polyethylene glycol etc. with inorganic salts, and low concentration side
Performance.
Brief description of the drawings
Fig. 1 is a kind of continuous preparation device schematic flow sheet of the compound forward osmosis membrane of high flux of the present invention.Wherein,
1- backing material let off roll, 2- backing materials, the movable baffle plates of 3-, 4- bilateral scrapers, 5- high concentration casting solutions, 6- low concentration casting films
Liquid, 7- coagulating baths, 8- support basement membranes, 9- interfacial polymerizations mechanism, 10- is combined forward osmosis membrane, the compound forward osmosis membrane wind-up rolls of 11-.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.These embodiments be merely to illustrate the present invention without
For limiting the scope of the present invention.The experiment condition of unreceipted design parameter in the following example, generally according to normal condition or
Production suggestion condition.To those of ordinary skill in the art, on the premise of the technology of the present invention principle is not departed from, may be used also
To make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Embodiment 1
Mass fraction is respectively into 13%, 80%, 7% polysulfones, 1-METHYLPYRROLIDONE, Macrogol 600 to be configured to
High concentration casting solution, mass fraction is respectively 2%, 88%, 10% polysulfones, 1-METHYLPYRROLIDONE, polyvinylpyrrolidine
Ketone K30 is configured to low concentration casting solution；The polyester non-woven fabric that thickness is 80 μm, porosity is 75% is under draw from gap
To be passed through in the middle of 100 μm of bilateral scraper, the high concentration casting solution and low concentration casting solution that will be prepared using bilateral scraper are distinguished
Non-woven fabrics both sides are coated in, compound is by after of short duration air section, solidified forming in the pure water bath of 25 DEG C of immersion is combined
Forward osmosis membrane supports basement membrane；Interfacial polymerization is carried out successively in the high concentration casting solution coating side surface of the support basement membrane, first
Aqueous phase solution used is the m-phenylene diamine (MPD) aqueous solution that mass concentration is 3%, and then organic phase solution used is for mass concentration
The hexane solution of 0.15% pyromellitic trimethylsilyl chloride, water phase and organic phase reaction form the surface with cross-linked structure and separate
Layer, so as to compound forward osmosis membrane is obtained.
Comparative example 1
Compound forward osmosis membrane is prepared using with the similar mode of above-described embodiment 1, difference is, in support basement membrane
Preparation process in, only film side coat high concentration casting solution, remaining the step of it is identical with embodiment 1.
Embodiment 2
Mass fraction is respectively into 16%, 74%, 10% polyether sulfone, DMAC N,N' dimethyl acetamide, Macrogol 600 to match somebody with somebody
High concentration casting solution is made, mass fraction is respectively 4%, 88%, 8% polyether sulfone, DMA, poly- second two
Alcohol 2000 is configured to low concentration casting solution；The nylon screen that thickness is 50 μm, porosity is 60% is under draw from gap
To be passed through in the middle of 80 μm of bilateral scraper, the high concentration casting solution and low concentration casting solution of preparation are applied respectively using bilateral scraper
Non-woven fabrics both sides are overlayed on, compound is by after of short duration air section, solidified forming in the pure water bath of 30 DEG C of immersion obtains being combined just
Permeable membrane supports basement membrane；Interfacial polymerization is carried out in the high concentration casting solution coating side surface of the support basement membrane, water used first
Phase solution is the m-phenylene diamine (MPD) aqueous solution that mass concentration is 2%, then organic phase solution used for mass concentration be 0.05%
The hexane solution of pyromellitic trimethylsilyl chloride, water phase and organic phase reaction form the surface separation layer with cross-linked structure, so as to make
Forward osmosis membrane must be combined.
Comparative example 2
Compound forward osmosis membrane is prepared using with the similar mode of above-described embodiment 2, difference is, in support basement membrane
Preparation process in, only film side coat high concentration casting solution, remaining the step of it is identical with embodiment 2.
Embodiment 3
Mass fraction is respectively into 15%, 80%, 5% polyacrylonitrile, N,N-dimethylformamide, lithium chloride to be configured to
High concentration casting solution, mass fraction is respectively 3%, 85%, 12% polyacrylonitrile, DMF, poly- second two
Alcohol 6000 is configured to low concentration casting solution；The polypropylene mesh that thickness is 100 μm, porosity is 80% under draw from
Gap is that 120 μm of bilateral scraper centre passes through, the high concentration casting solution and low concentration casting solution point that will be prepared using bilateral scraper
Non-woven fabrics both sides are not coated in, and compound is by after of short duration air section, solidified forming in the pure water bath of 23 DEG C of immersion is answered
Close forward osmosis membrane support basement membrane；Interfacial polymerization is carried out in the high concentration casting solution coating side surface of the support basement membrane, first institute
It is the m-phenylene diamine (MPD) aqueous solution that mass concentration is 2% with aqueous phase solution, then organic phase solution used is that mass concentration is 0.1%
Pyromellitic trimethylsilyl chloride hexane solution, water phase and organic phase reaction form the surface separation layer with cross-linked structure so that
Compound forward osmosis membrane is obtained.
Comparative example 3
Compound forward osmosis membrane is prepared using with the similar mode of above-described embodiment 3, difference is, in support basement membrane
Preparation process in, only film side coat high concentration casting solution, remaining the step of it is identical with embodiment 3.
Film properties test：As liquid is drawn, with pure water as material liquid, test is obtained just oozes sodium-chloride water solution with 1mol/L
Pure water flux (the L/m of permeable membrane2H) with back-mixing flux salt (g/m2h).In test, the surface separation layer of film towards material liquid, effectively
Membrane area is 40cm2, material liquid is 100mL/min with the cycle rate for drawing liquid, and test temperature is 25 DEG C.Following table 1 is arranged
The test result of the made compound forward osmosis membranes of embodiment 1-3 and comparative example 1-3 is gone out.
Table 1
According to the performance comparison of table 1, can learn：The pure water flux that forward osmosis membrane is combined obtained in comparative example is significantly lower than
The pure water flux of forward osmosis membrane is combined obtained in correspondence embodiment, but its back-mixing flux salt is more or less the same.Therefore, system of the invention
Preparation Method uses high concentration casting solution and low concentration casting solution, while the casting film on backing material, makes finally obtained being combined just
While certain separating property is kept, permeation flux effectively improves permeable membrane.
Claims (9)
1. a kind of high flux is combined the continuous preparation method of forward osmosis membrane, it is characterised in that the method specifically includes following steps：
1) preparation of basement membrane is supported：Backing material under draw through the gap bilateral scraper, using bilateral scraper
Casting solution is continuously coated simultaneously in backing material both sides, and side coating high concentration casting solution, opposite side coats low concentration casting solution,
Gained compound is by after air section, solidified forming in immersion coagulating bath obtains compound forward osmosis membrane support basement membrane；
2) it is combined the preparation of forward osmosis membrane：Interfacial polymerization is carried out in the high concentration casting solution coating side surface of the support basement membrane,
Form the surface separation layer with cross-linked structure.
2. according to a kind of continuous preparation method of the compound forward osmosis membrane of high flux described in claim 1, it is characterised in that described
Backing material is non-woven fabrics, fabric or the screen cloth of low-density；The material of the non-woven fabrics is selected from polyester, nylon, polyethylene or poly-
Propylene；The material of the fabric or screen cloth is selected from polyester, nylon, polyethylene, polypropylene, stainless steel, glass fibre or carbon fiber；
The thickness of the backing material is 30-150 μm, and porosity is 50-95%.
3. according to a kind of continuous preparation method of the compound forward osmosis membrane of high flux described in claim 1, it is characterised in that coating
The device of casting solution is that backing material both sides are respectively the movable baffle plate (3) of parallel support material, while in movable baffle plate (3)
Below be inclined scraper (4), have a space between the same side of backing material, movable baffle plate (3) and scraper (4),
Pore size can be adjusted as needed；Bilateral scraper coordinates the coating thickness of movable baffle controls casting solution；The bilateral scraper
Between gap be 50-200 μm；The movable baffle plate can upper and lower, inside and outside movement, be used to control two kinds of releases of casting solution time
Sequence or release amount, so as to adjust two kinds of relative coating thickness of casting solution.
4. according to a kind of continuous preparation method of the compound forward osmosis membrane of high flux described in claim 1, it is characterised in that described
High concentration casting solution and low concentration casting solution are constituted by film forming polymer, solvent, additive, in its middle and high concentration casting solution into
Membrane polymer, solvent, the mass fraction of additive are respectively 5-20%, 55-95%, 0-25%, film forming in low concentration casting solution
Polymer, solvent, the mass fraction of additive are respectively 0-5%, 65-100%, 0-30%, and film forming is gathered in high concentration casting solution
It is 5% when compound is different with film forming polymer mass fraction in low concentration casting solution.
5. according to a kind of continuous preparation method of the compound forward osmosis membrane of high flux described in claim 1, it is characterised in that described
Film forming polymer is selected from polysulfones, polyether sulfone, PEI, polyacrylonitrile, one kind of cellulose acetate or two of which and two
Plant the mixture of the above；The solvent be selected from N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, 1-METHYLPYRROLIDONE,
One kind or two of which and two or more mixtures of dimethyl sulfoxide (DMSO)；The additive is selected from water, methyl alcohol, ethanol, second two
One kind or two of which and two in alcohol, glycerine, polyethylene glycol, polyvinylpyrrolidone, lithium chloride, lithium bromide, zinc chloride
Plant the mixture of the above.
6. according to a kind of continuous preparation method of the compound forward osmosis membrane of high flux described in claim 1, it is characterised in that described
Coagulation bath composition is the mixture of water and the solvent, and wherein the mass fraction of solvent is 0-50%, the temperature of the coagulating bath
It is 0-60 DEG C.
7. according to a kind of continuous preparation method of the compound forward osmosis membrane of high flux described in claim 1, it is characterised in that described
In interfacial polymerization process, successively using aqueous phase solution and organic phase solution, reaction monomers are polyamine in the aqueous phase solution, its
Mass fraction is 0.2-5%, and the organic phase solution reaction monomers are polynary acyl chlorides, and its mass fraction is 0.02-0.5%.
8. according to a kind of continuous preparation method of the compound forward osmosis membrane of high flux described in claim 7, it is characterised in that described
Reaction monomers are m-phenylene diamine (MPD), p-phenylenediamine, equal benzene triamine or piperazine in aqueous phase solution, and the solvent of organic phase solution is selected from positive penta
Alkane, n-hexane, hexamethylene or petroleum ether, the monomer of organic phase solution is pyromellitic trimethylsilyl chloride.
9. the compound forward osmosis membrane of high flux for being prepared according to claim 1-8 any one methods.
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| CN114870644A (en) * | 2022-06-17 | 2022-08-09 | 杭州福斯特应用材料股份有限公司 | Semipermeable membrane composite material and preparation method thereof |
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Application publication date: 20170613 |