CN109603577A - A method of it prepares to reserve and draws solute double activated layer forward osmosis membrane - Google Patents
A method of it prepares to reserve and draws solute double activated layer forward osmosis membrane Download PDFInfo
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- CN109603577A CN109603577A CN201811592379.4A CN201811592379A CN109603577A CN 109603577 A CN109603577 A CN 109603577A CN 201811592379 A CN201811592379 A CN 201811592379A CN 109603577 A CN109603577 A CN 109603577A
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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
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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
- B01D69/02—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
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
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Abstract
The invention belongs to UF membrane fields, are related to a kind of method for preparing and reserving and drawing solute double activated layer forward osmosis membrane.The present invention is supporting layer using perforated membrane, active layer is prepared on supporting layer two sides using interfacial polymerization method, and it is reserved in supporting layer and a certain amount of draws solute, the reserved solute double activated layer forward osmosis membrane that draw is with the more conventional higher flux of double activated layer forward osmosis membrane, more single active layer forward osmosis membrane has superior antifouling property under AL-DS mode, and has the advantages that preparation process is simple, is easy to be mass produced.
Description
Technical field
The invention belongs to UF membrane fields, are related to a kind of method for preparing double activated layer forward osmosis membrane.
Background technique
Nowadays, water quality deterioration and shortage of water resources drastically influence the development of society.Membrane separation technique as 21 century most
Promising water treatment technology, it is easy to operate because being not necessarily to add chemical reagent in its separation process, it is extensive in having obtained in recent years
It pays close attention to and promotes energetically in ground.The core of membrane separation technique is permeable membrane, according to membrane aperture size can be divided into microfiltration membranes (MF),
Ultrafiltration membrane (UF), nanofiltration membrane (NF), reverse osmosis membrane (RO) and forward osmosis membrane (FO), and forward osmosis membrane has point during the separation process
From high-efficient, fouling membrane tend to it is low, can low pressure even without pressure under the conditions of run the advantages that, shown in water treatment field good
Good separating property.Traditional forward osmosis membrane is anisotropic membrane, is made of loose supporting layer and fine and close active layer, certain
In degree, active layer determines film to the rejection of ion, and supporting layer determines water flux.During processing according to activity
The direction of layer can be divided into both operational modes of AL-FS and AL-DS, wherein claim when active layer is directly contacted with water inlet stoste
For AL-FS mode, active layer directly with draw when liquid contacts referred to as AL-DS mode.However, the direction of film is logical to fouling membrane, water
Amount and rejection have large effect.Under AL-FS mode, because the flux that interior concentration polarization problem can lead to water is lower, shadow
Treatment effeciency is rung；In AL-DS mode, although the flux problems of water are improved, due to the solute in processing water sample
Fenestra or even fouling can be blocked into supporting layer, the antifouling property of film is low.
To solve the above problems, it is proposed that the concept of the double activated tunic of innovation, this membrane material is in supporting layer
Two sides form fine and close active layer, and the active layer of feed side can protect supporting layer and avoid pollution.Such film design can be real
The now effect similar with AL-DS mode, the i.e. minimum puzzlement without having fouling membrane of interior concentration polarization.But double activated layer is due to right
It is lower than single active layer to will lead to water flux for the retention of solute.Therefore, it is badly in need of developing a kind of double activated layer of high-throughput, high anti-pollution
Forward osmosis membrane.
Summary of the invention
The purpose of the present invention is, provide a kind of to prepare high-throughput, high anti-pollution in view of the deficiencies of the prior art and the market demand
The reserved method for drawing solute double activated layer forward osmosis membrane of dye.
The present invention is directed to interior concentration polarization and membrane pollution problem, proposes and draws solute in supporting layer reserved part, is protecting
Shield supporting layer is while be contaminated, and is reserved in drawing solute and can effectively slow down interior concentration difference in supporting layer in supporting layer
Polarization problem, to improve the flux of water.
Technical solution of the present invention:
A kind of double activated layer forward osmosis membrane, with supporting layer and positioned at the densification activity of supporting layer upper and lower surfaces
Layer；Using perforated membrane as supporting layer, contains in the perforated membrane and draw solute.
It is described to draw percent 10-80% that content of the solute in perforated membrane is added concentration.
The perforated membrane is organic polymer films.It may be either the business organic film directly bought, it can also be logical for laboratory
Cross inversion of phases or Electrospun preparation.
The active layer property can be regulated and controled by the concentration of reactant in interfacial polymerization process with the reaction time.
The material of the perforated membrane be nylon, polyethers sough, polyacrylonitrile, Kynoar, Triafol T or acetic acid
The organic miillpore filter of cellulose.
The pore diameter range of the perforated membrane are as follows: 50-1000nm, porosity ranges are 20~98%.
The perforated membrane is plate membrane, tubular type, capillary type or hollow-fibre membrane.
The solute that draws is organic matter, inorganic salts or synthetic material；The organic matter is glucose, fructose, sucrose, second
Alcohol, sodium formate, sodium acetate, magnesium acetate or sodium propionate；The inorganic salts sulfate, nitrate, chloride or carbonate；
The synthetic material can for polyacrylic acid magnetic nano-particle, unit price or divalent dimethyl machine imidazolium compounds,
Poly- sodium propionate, high-molecular gel, acyl group-TAEA (three acyl group tren derivatives).
The sulfate is potassium sulfate, sodium sulphate, magnesium sulfate or copper sulphate；The nitrate be potassium nitrate, sodium nitrate or
Calcium nitrate；The chloride is potassium chloride, sodium chloride, calcium chloride or ammonium chloride；The carbonate is sodium bicarbonate or bicarbonate
Potassium.
The above-mentioned preparation method for stating double activated layer forward osmosis membrane, the active layer generate polyamide by interfacial polymerization
Active layer.Polyamide active layer is usually occurred by polyamine and polynary acyl chlorides monomer in two mutual exclusive solvent interfaces
Polymerization reaction, so that shape forms one layer of ultra-thin fine and close aramid layer in support.
It the polyamide active layer and draws and has no specific corresponding relationship between solute, can correspond to and arbitrarily draw solute.
The amine monomers are triethylene tetramine, diethylenetriamine, ethylenediamine, p-phenylenediamine, m-phenylene diamine (MPD), 1,2- benzene two
Amine, 1,4- phenylenediamine, piperazine, polyethyleneimine, triethanolamine or methyl diethanolamine；The acyl chlorides monomer be between phenyl-diformyl
Chlorine, paraphthaloyl chloride, pyromellitic trimethylsilyl chloride, four formyl chloride of equal benzene or 5- isocyanates-different peptide acyl chlorides.
Preparation method the following steps are included:
Step A, the perforated membrane is rinsed with deionized water, and dry 1~60min is spare at 40-60 DEG C；
Step B, polyamine is dissolved in deionized water, forms the polynary amine aqueous solution of 1~7wt%；
Step C, solute will be drawn, the resulting polynary amine aqueous solution of step B is added, drawing solute concentration is 0~15wt%, system
Obtain mixed solution；
Step D, polynary acyl chlorides is dissolved in hexane solution, forms the polynary solution of acid chloride of 0.01~1wt%；
Step E, the perforated membrane after processing of step A is soaked in 1~30min in the resulting mixed solution of step C, makes to draw
Solute is taken to remain in supporting layer；The residual solution for blotting support layer surface after taking-up with filter paper, is placed in Suction filtration device；
Step F, a single side of perforated membrane is immersed in 10-120s in the resulting polynary solution of acid chloride of step D, is gathered
Amide active layer；
Step G, it repeats step F and polyamide active layer is prepared in the another side of perforated membrane；
Step H, film is put to 1~20min of processing in the baking oven for place into deionized water 80~100 DEG C.
The present invention has a characteristic that
1, it reserves and draws solute double activated layer forward osmosis membrane with high-throughput and resistance tocrocking；
2, being reserved between double activated layer the solute that draws (i.e. in supporting layer) can be improved the permeation flux of forward osmosis membrane；
3, the permeation flux of the forward osmosis membrane, which improves degree, to realize regulation by adjusting the reserved amount for drawing solute；
Detailed description of the invention
Fig. 1 is that the photo in kind for drawing solute double activated layer polypropylene nitrile tunica fibrosa is reserved in embodiment 1；
Fig. 2 is the stereoscan photograph of polyacrylonitrile fibre supporting layer in embodiment 1；
Fig. 3 is that the double activated layer forward osmosis membrane stereoscan photograph for drawing solute has been reserved in embodiment 1.
Fig. 4 is preventing membrane pollution results of property figure in embodiment 1；
Fig. 5 is preventing membrane pollution results of property figure in embodiment 2；
Fig. 6 is preventing membrane pollution results of property figure in embodiment 3.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.Test method described in following embodiments is unless otherwise specified conventional method；The examination
Agent and material commercially obtain unless otherwise specified.
The reserved double activated layer forward osmosis membrane for drawing solute, can be divided into active layer and supporting layer two parts.To have reserved portion
Dividing the perforated substrate for drawing solute is supporting layer, prepares active layer by interfacial polymerization.It reserves and draws in the supporting layer
The amount of solute, can be according to the permeable pressure head regulation driven between liquid and raw material water inlet in operational process.
It is reserved draw solute double activated layer forward osmosis membrane the preparation method is as follows:
It step A, is 50-1000nm by pore diameter range, porosity ranges are rushed in 20~98% supporting layer with deionized water
It washes, and dry 1~60min is spare at 40-60 DEG C；
Step B, polyamine is dissolved in deionized water, forms the polynary amine aqueous solution of 1~7wt%；
Step C, solute will be drawn, the resulting polynary amine aqueous solution of step B is added, drawing solute concentration is 0~15wt%, system
Obtain mixed solution；
Step D, polynary acyl chlorides is dissolved in hexane solution, forms the polynary solution of acid chloride of 0.01~1wt%；
Step E, by 1~30min in the resulting solution of supporting layer soaking step C, make to draw solute and remain in supporting layer；
Step F, the residual solution for blotting support layer surface after taking-up with filter paper, is placed in Suction filtration device, allows single-side support
Layer is immersed in 10-120s in the resulting solution of step D, obtains polyamide active layer, repeats the process in the another side of supporting layer
Also polyamide active layer is prepared；
Step G, it reserved will draw the taking-up of solute double activated layer forward osmosis membrane to put in deionized water, and place into 80~100
DEG C baking oven in handle 1~20min, increase crosslinking degree.
Embodiment 1
It (1) is 200nm by aperture, the polyacrylonitrile fibre supporting layer substrate that porosity is 90% is rinsed with deionized water,
And dry 10min is spare at 40 DEG C；
(2) m-phenylene diamine (MPD) is dissolved in deionized water, is configured to the m-phenylenediamine solution of 2wt%；
(3) sodium chloride is added into the m-phenylenediamine solution of 2wt%, wherein the concentration of sodium chloride is 3wt%, and mixing is made
Solution；
(4) pyromellitic trimethylsilyl chloride is dissolved in hexane solution, forms the pyromellitic trimethylsilyl chloride solution of 0.2wt%；
(5) by polyacrylonitrile fibre supporting layer in the solution (NaCl for including 3wt%) of the m-phenylene diamine (MPD) containing 2wt%
Impregnate 2min；
(6) the polyacrylonitrile fibre supporting layer for drawing solute (NaCl) will have been reserved to take out, has blotted excessive moisture with filter paper
It is placed in Suction filtration device, single layer is made to be immersed in 30s in pyromellitic trimethylsilyl chloride/n-hexane of 0.2wt%, obtain polyamide activity
Layer, repeating the step makes the another side of supporting layer also prepare polyamide active layer；
(7) it reserved will draw solute double activated layer forward osmosis membrane and take out in the deionized water for be placed on 80 DEG C and handle 10min.
In the above way obtained polyacrylonitrile fibre membrane is tested for the property, and 0.5mol/L sodium chloride solution is to draw
Liquid, deionized water are feeding liquid, calculate separately and do not reserve and reserved the flux and salt removal rate for drawing the double activated of solute, room
The lower test result of temperature are as follows:
Double activated layer forward osmosis membrane is in the above way prepared, and it is living to prepare the not reserved list for drawing solute in the same way
Property layer polypropylene nitrile tunica fibrosa.Be to draw liquid with 0.5mol/L sodium chloride solution, the sodium alginate of 100ppm as feeding liquid,
After continuous operation 6h, 1h is rinsed with deionized water, is further continued for operation 6h.
Test result at room temperature are as follows: the reserved water flux for drawing solute double activated layer is gradually decreased to from 24.0LMH
23.1LMH, water flux almost absolutely restores after deionized water is rinsed；Single active layer forward osmosis membrane is under AL-DS mode, water
Flux drops to 7.6LMH from 15.2LMH, and water flux restores 80 percent after deionized water is rinsed.
Embodiment 2
It (1) is 100nm by aperture, the Kynoar supporting layer that porosity is 80% is rinsed with deionized water, and 50 DEG C
Under be dried for standby；
(2) m-phenylene diamine (MPD) is dissolved in deionized water, is configured to the m-phenylenediamine solution of 3wt%；
(3) sodium chloride is added into the m-phenylenediamine solution of 3wt%, wherein the concentration of sodium chloride is 3.5wt%, is made mixed
Close solution；
(4) pyromellitic trimethylsilyl chloride is dissolved in hexane solution, forms the pyromellitic trimethylsilyl chloride solution of 0.2wt%；
(5) by Kynoar supporting layer in the solution (NaCl for including 3.5wt%) of the m-phenylene diamine (MPD) containing 3wt%
Impregnate 2min；
(6) the Kynoar supporting layer for drawing solute (NaCl) will have been reserved to take out, after blotting excessive moisture with filter paper
It is placed in Suction filtration device, single layer is made to be immersed in 30s in pyromellitic trimethylsilyl chloride/n-hexane of 0.2wt%, obtain polyamide activity
Layer, repeating the step makes the another side of supporting layer also prepare polyamide active layer；
(7) it reserved will draw solute double activated layer forward osmosis membrane and take out in the deionized water for be placed on 80 DEG C and handle 10min.
In the above way obtained polyvinylidene fluoride film is tested for the property, and 0.5mol/L sodium chloride solution is to draw
Liquid, deionized water are feeding liquid, calculate separately and do not reserve and reserved the flux and salt removal rate for drawing the double activated of solute, room
The lower test result of temperature are as follows:
Double activated layer forward osmosis membrane is in the above way prepared, and it is living to prepare the not reserved list for drawing solute in the same way
Property strata vinylidene fluoride film.It is to draw liquid with 0.5mol/L sodium chloride solution, the sodium alginate of 100ppm is as feeding liquid, even
After reforwarding row 6h, 1h is rinsed with deionized water, is further continued for operation 6h.
Test result at room temperature are as follows: the reserved water flux for drawing solute double activated layer is gradually decreased to from 22.3LMH
21.0LMH, water flux almost absolutely restores after deionized water is rinsed；Single active layer forward osmosis membrane is under AL-DS mode, water
Flux drops to 7.8LMH from 16.4LMH, and water flux restores 80 percent after deionized water is rinsed.
Embodiment 3
It (1) is 300nm by aperture, the polyethers doughnut supporting layer of soughing that porosity is 90% is rinsed with deionized water, and
It is dried for standby at 40 DEG C；
(2) m-phenylene diamine (MPD) is dissolved in deionized water, is configured to the m-phenylenediamine solution of 4wt%；
(3) glucose is added into the m-phenylenediamine solution of 4wt%, wherein the concentration of glucose is 3.5wt%, is made mixed
Close solution；
(4) pyromellitic trimethylsilyl chloride is dissolved in hexane solution, forms the pyromellitic trimethylsilyl chloride solution of 0.15wt%；
(5) solution for m-phenylene diamine (MPD) of the flow velocity injection containing 4wt% soughed in hollow fiber film tube with 1m/s to polyethers is (interior
Glucose containing 3.5wt%), which continues 2min；
(6) high pressure gas, such as air, nitrogen, argon gas inert gas are used, 1min is purged with the flow velocity of 1m/s, removes table
The solution of face remnants, then pyromellitic trimethylsilyl chloride/hexane solution of 0.15wt%, the process are injected with the flow velocity of 1m/s into pipe
Continue 60s, polyamide active layer in managing is made, by hollow-fibre membrane both ends glue sealing, repeats same steps and outer layer is made
Polyamide active layer.
(7) it reserved will draw solute double activated layer forward osmosis membrane and take out in the deionized water for be placed on 90 DEG C and handle 15min.
In the above way obtained polyethers hollow-fibre membrane of soughing is tested for the property, and 0.5mol/L sodium chloride solution is to draw
Liquid is taken, deionized water is feeding liquid, it calculates separately and does not reserve and reserved the flux and salt removal rate for drawing the double activated of solute,
Test result at room temperature are as follows:
Double activated layer forward osmosis membrane is in the above way prepared, and it is living to prepare the not reserved list for drawing solute in the same way
Property strata ether is soughed hollow-fibre membrane.Be to draw liquid with 0.5mol/L sodium chloride solution, the sodium alginate of 100ppm as feeding liquid,
After continuous operation 6h, 1h is rinsed with deionized water, is further continued for operation 6h.
Test result at room temperature are as follows: the reserved water flux for drawing solute double activated layer is gradually decreased to from 23.0LMH
20.6LMH, water flux almost absolutely restores after deionized water is rinsed；Single active layer forward osmosis membrane is under AL-DS mode, water
Flux drops to 6.9LMH from 14.6LMH, and water flux restores 80 percent after deionized water is rinsed.
Embodiment described above, only typical embodiment in the present invention, does not constitute improper limitations of the present invention, therefore
It is all according to obvious change described in scope of the present invention patent and other changes for not departing from essence of the invention,
It should include within protection scope of the present invention.
Claims (10)
1. a kind of double activated layer forward osmosis membrane has supporting layer and the fine and close active layer positioned at supporting layer upper and lower surfaces；
It is characterized in that, containing in the perforated membrane using perforated membrane as supporting layer and drawing solute.
2. double activated layer forward osmosis membrane according to claim 1, which is characterized in that the solute that draws is in perforated membrane
Content is percent 10-80% of added concentration.
3. double activated layer forward osmosis membrane according to claim 1, which is characterized in that the perforated membrane is organic polymer
Film.
4. double activated layer forward osmosis membrane according to claim 1, which is characterized in that the material of the perforated membrane be nylon,
Polyethers soughs, polyacrylonitrile, Kynoar, Triafol T or the organic miillpore filter of cellulose acetate.
5. double activated layer forward osmosis membrane according to claim 1 or 2, which is characterized in that the pore diameter range of the perforated membrane
Are as follows: 50-1000nm, porosity ranges are 20~98%.
6. double activated layer forward osmosis membrane according to claim 1 or 2 or 3, which is characterized in that the perforated membrane is plate
Film, tubular type, capillary type or hollow-fibre membrane.
7. double activated layer forward osmosis membrane according to claim 1, which is characterized in that the solute that draws is organic matter, nothing
Machine salt or synthetic material；The organic matter is glucose, fructose, sucrose, ethyl alcohol, sodium formate, sodium acetate, magnesium acetate or propionic acid
Sodium；The inorganic salts sulfate, nitrate, chloride or carbonate；
The synthetic material can be the dimethyl machine imidazolium compounds of polyacrylic acid magnetic nano-particle, unit price or divalent, poly- third
Sour sodium, high-molecular gel, acyl group-TAEA (three acyl group tren derivatives).
8. double activated layer forward osmosis membrane according to claim 1, which is characterized in that
The sulfate be potassium sulfate, sodium sulphate, magnesium sulfate or copper sulphate,
The nitrate be potassium nitrate, sodium nitrate or calcium nitrate,
The chloride be potassium chloride, sodium chloride, calcium chloride or ammonium chloride,
The carbonate is sodium bicarbonate or saleratus.
9. the preparation method of double activated layer forward osmosis membrane described in claim 1-5 any one, which is characterized in that the activity
Layer generates polyamide active layer by interfacial polymerization.
10. preparation method according to claim 7, which comprises the following steps:
Step A, the perforated membrane is rinsed with deionized water, and dry 1~60min at 40-60 DEG C；
Step B, polyamine is dissolved in deionized water, forms the polynary amine aqueous solution of 1~7wt%；
Step C, solute will be drawn, the resulting polynary amine aqueous solution of step B is added, drawing solute concentration is 0~15wt%, is made mixed
Close solution；
Step D, polynary acyl chlorides is dissolved in hexane solution, forms the polynary solution of acid chloride of 0.01~1wt%；
Step E, the perforated membrane after processing of step A is soaked in 1~30min in the resulting mixed solution of step C；；
Step F, a single side of perforated membrane is immersed in 10-120s in the resulting polynary solution of acid chloride of step D, obtains polyamide
Active layer；
Step G, it repeats step F and polyamide active layer is prepared in the another side of perforated membrane；
Step H, film is put to 1~20min of processing in the baking oven for place into deionized water 80~100 DEG C.
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| CN112808020A (en) * | 2020-12-31 | 2021-05-18 | 华中科技大学 | Forward osmosis base membrane with optimized surface charge on side of drawing solution and preparation method thereof |
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