CN106268323A - A kind of n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film and preparation method thereof - Google Patents
A kind of n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film and preparation method thereof, by the method deposited layer by layer, with 2 hydroxypropyltrimethyl ammonium chloride chitosan of lotus positive electricity as cationic polymer, polyacrylic acid is anionic polymer, then introducing NaCl solution and do support salt, alternating deposit, LBL self-assembly becomes composite membrane, last crosslinking in epoxychloropropane, obtains composite nanometer filtering film.The preparation method technique of the present invention is simple, and natural environmental-protective, the Positively charged composite nanofiltration membrane of preparation has good hydrophilicity, excellent mechanical performance and swelling behavior, and pure water infiltration coefficient is 19.29L h‑1·m‑2Mpa, molecular cut off is 989, and the separation that can be used for traces polluter especially lotus electropositive substance in water environment is removed.
Description
Technical field
The present invention relates to a kind of n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film and preparation method thereof, belong to membrance separation
Field.
Background technology
LBL self-assembly, it is simply that utilize the principle of polyelectrolyte successively alternating deposit, by target compound in solution with
The strong interaction (such as chemical bond etc.) of substrate surface functional group or weak interaction are (such as electrostatic attraction, hydrogen bond, coordinate bond
Deng), form structural integrity, stable performance, there is a special kind of skill of certain specific function thin film.Layer-by-layer can be real
Being modified film the most on a molecular scale, control the composition of film, structure and thickness, in film material with function field, application is wide
General.
Conventional LBL self-assembly polycation electrolyte has polypropylene amine (PAH), diallyl dimethyl ammoniumchloride
(PDADMAC), chitosan, polymine (PEI) etc., polyanion electrolyte has polyacrylic acid (PAA), polystyrolsulfon acid
(PSS), polyvinylsulfonic acid (PVS) etc..Yang Xiuli etc. use PEI to be polycation, and PAA is polyanion, prepare (PEI/
PAA) n composite nanometer filtering film, the hydrophilic of PEI is poor, composite membrane flux less (Yang Xiuli. LBL self-assembly composite nanometer filtering film
Research [D]. Hebei University of Technology, 2015).He Shuai etc. use graphene oxide (GO) to be polycation, chitosan for poly-cloudy from
Sub-LBL self-assembly prepares (GO/CS) n composite membrane, composite membrane lotus electropositive more weak (He Shuai, Liang Jingmei, the Hu Huilan prepared
Deng, the preparation of graphene oxide, chitosan self-assembled composite film layer by layer and the application in field of Environment Protection thereof, material Leader,
2016,3 (30), 1～5).Li Boqun etc. with polymine (PEI) as polycation electrolyte, polyacrylic acid (PAA), polyphenyl
Vinyl sulfonic acid sodium (PSS) is polyanion electrolyte, utilizes polyelectrolyte self-assembling technique to be prepared for self assembly composite nanometer filtering film,
Obtained preferable rejection effect, but flux relatively low (Li Boqun. NF membrane is prepared in charged polysulphones hyperfiltration membrane LBL self-assembly modification
And desalting performance research [D]. Wuhan Engineering Univ, 2015).
Summary of the invention
The problem that lotus electropositive is more weak and flux is relatively low existed for existing NF membrane, the invention provides a kind of season
Ammonium chitosan/polyacrylic acid ((HTCC/PAA) n) composite nanometer filtering film and preparation method thereof, should (HTCC/PAA) n composite nanometer filter
Film has preferable hydrophilic, good anti-microbial property and high rejection.
The technical solution of the present invention is:
A kind of n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film, described composite membrane is with n-trimethyl chitosan chloride (HTCC)
With polyacrylic acid (PAA) as polyelectrolyte active layer, by alternate immersion, prepared by LBL self-assembly method, especially by following
Prepared by step:
Step 1, preparation 4～6g/L HTCC solution and the PAA solution of 1～2g/L, with NaOH solution regulation PAA solution
PH is 6～8, is separately added into NaCl, is configured to, containing the casting solution that NaCl mass concentration is 0.05～0.1g/L, to be sufficiently stirred for, make
NaCl is uniformly dispersed；
Step 2, is first immersed in polyether sulfone (PES) basement membrane in HTCC casting solution, is immersed in PAA casting solution after cleaning again
In, form a bilayer, continue to soak alternating deposit in HTCC casting solution and PAA casting solution, LBL self-assembly become 3.5～
5.5 bilayers, obtain the composite membrane of surface lotus positive electricity；
Step 3, is dried LBL self-assembly composite membrane, be soaked in through KOH regulation, pH be 9 ± 1, mass concentration be
In the ethanol solution of the epoxychloropropane (ECH) of 1.3%～2.5%, 45～55 DEG C of cross-linking reactions 21-24h, crosslinking is dry after terminating
Dry, clean, obtain n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film.
Preferably, in step 1, the concentration of described HTCC solution is 5g/L.
Preferably, in step 2, the soak time at casting solution is 10～20min, and the described self assembly number of plies is 4.5 layers.
In step 2, the molecular cut off of polyether sulfone basement membrane is 10000, and effective area is 12.56cm2。
Preferably, in step 3, the mass concentration of the ethanol solution of described epoxychloropropane is 1.9%, described crosslinking
Temperature is 50 DEG C.
Compared with prior art, the n-trimethyl chitosan chloride of the present invention/polyacrylic acid composite nanometer filtering film has good retaining
Effect and flux, pure water infiltration coefficient is 19.29, and molecular cut off is 989；Use polyacrylic acid as polyelectrolyte, have
Well acid resistance and alkali resistance, have good antibacterial effect simultaneously, notable to the trace organic substance removal effect in water.
Accompanying drawing explanation
Fig. 1 is the preparation flow schematic diagram of the present invention (HTCC/PAA) n composite membrane.
Fig. 2 is the result figure that embodiment 6 prepares the pure water infiltration coefficient of (HTCC/PAA) n composite membrane.
Fig. 3 is the result figure that embodiment 6 prepares the molecular cut off of (HTCC/PAA) n composite membrane.
Fig. 4 is that embodiment 6 prepares (HTCC/PAA) n composite membrane to the rejection result figure to five kinds of inorganic salts.
Fig. 5 is that embodiment 6 prepares (HTCC/PAA) the n composite membrane clearance result figure to four kinds of PPCPs.
Detailed description of the invention
With embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings.
HTCC (2-hydroxypropyl-trimethyl ammonium chloride) list of references (Liu, the Z.J. used in the embodiment of the present invention
(2014),Preparation and performance of positively charged 2-hydroxypropyl
trimethyl ammonium chloride chitosan(HTCC)/poly(polyether sulfone)composite
membrane.M.Sc.thesis,Dept.Environ.Sci.Eng.,Nanjing Univ.of sci.techno.,
China.) preparing, its substitution value is 88.65%.
Embodiment 1
The preparation HTCC solution of 5g/L and the PAA solution of 1g/L, regulate PAA pH value of solution respectively to 4 by NaOH solution, and 7,
10, HTCC solution and PAA solution is separately added into NaCl as supporting salt, makes HTCC that NaCl concentration is 0.05g/L casting
Film liquid and PAA casting solution.3 PES basement membranes are immersed in 15min in HTCC casting solution, clean with pure water, obtain surface lotus positive electricity
Composite membrane；3 films obtained soak in the PAA solution of 3 kinds of different pH 15min more respectively, and pure water cleans, obtains surface
The composite membrane of bear electricity, completes a bilayer.Repeating to soak, obtaining the number of plies is 4.5 double-deck composite membranes.Then, 3 are done
Film be soaked in respectively through KOH regulation, pH be 9, mass concentration be 1.3% the ethanol solution of epoxychloropropane in, 50 DEG C of crosslinkings
Reaction 21h, after cross-linking reaction, is dried, and through deionized water wash, is placed in pure water immersion more than 24h, to be determined.
3 films prepared MgCl to 1g/L2Solution rejection be followed successively by 36.17%, 81.71%, 53.87%,
The rejection effect of film is affected very big by the pH understanding PAA solution, and when pH is 7, rejection effect is best.
Embodiment 2
The HTCC solution of preparation 5g/L, then take quantitative PAA pure water and be configured to 0.5g/L, 1g/L, 1.5g/L, 2g/ respectively
L, 2.5g/LPAA solution, with NaOH solution regulation PAA pH value of solution to 7, then is separately added into NaCl work in HTCC and PAA solution
For supporting salt, make HTCC casting solution and PAA casting solution that NaCl mass concentration is 0.05g/L.5 PES basement membranes are immersed in
15min in HTCC casting solution, cleans with pure water, obtains the composite membrane of surface lotus positive electricity；Again by 5 films obtaining respectively at 5 kinds
Soaking 15min in variable concentrations PAA solution, pure water cleans, and obtains the composite membrane of surface bear electricity, completes a bilayer.Repeat
Soaking, obtaining the number of plies is 4.5 double-deck composite membranes.Then, 5 dry films are soaked in respectively through KOH reconcile, pH be 9, quality
Concentration is in the ethanol solution of the epoxychloropropane of 1.9%, 50 DEG C of cross-linking reactions 21h, after cross-linking reaction, is dried, through going
Ionized water washs, and is placed in pure water immersion more than 24h, to be determined.
5 films prepared MgCl to 1g/L2The rejection of solution is followed successively by 73.45%, 81.71%, 70.57%,
62.76%, 58.32%, it is seen that polyacrylic acid optium concentration is 1g/L, increase polyacrylic concentration, lotus electropositive reduces, right
Cation rejection reduces.
Embodiment 3
Take quantitative HTCC pure water and be configured to the HTCC solution of 4g/L, 5g/L, 6g/L respectively, prepare 1g/LPAA solution, use
NaOH solution regulation PAA pH value of solution to 7, then be separately added in HTCC and PAA solution NaCl as support salt, make NaCl matter
Amount concentration is HTCC casting solution and the PAA casting solution of 0.05g/L.3 PES basement membranes are immersed in 15min in HTCC casting solution, use
Pure water cleans, and obtains the composite membrane of surface lotus positive electricity；Again 3 films obtained are soaked respectively in 5 kinds of variable concentrations PAA solution
15min, pure water cleans, and obtains the composite membrane of surface bear electricity, completes a bilayer.Repeating to soak, obtaining the number of plies is 4.5 pairs
The composite membrane of layer.Then, 3 dry films are soaked in respectively through KOH reconcile, pH be 9, mass concentration be the epoxy chloropropionate of 2.5%
In the ethanol solution of alkane, 50 DEG C of cross-linking reactions 21h, after cross-linking reaction, it is dried, through deionized water wash, is placed in pure water
Soak more than 24h, to be determined.
3 films prepared MgCl to 1g/L2Solution rejection be followed successively by 71.83%, 81.71%, 88.69%,
Flux is 8.97L m-2·h-1、8.20L·m-2·h-1、6.58L·m-2·h-1, it is seen that HTCC concentration increases, the lotus positive electricity of film
Property strengthen, rejection raise, but flux reduce, so HTCC concentration is difficult to too high.
Embodiment 4
The preparation HTCC solution of 5g/L and the PAA solution of 1g/L, regulate PAA pH value of solution respectively to 7 by NaOH solution,
HTCC solution and PAA solution are separately added into NaCl as support salt, make NaCl concentration and be respectively the casting solution of 0.05g/L.
PES basement membrane is immersed in 15min in HTCC casting solution, cleans with pure water, obtain the composite membrane of surface lotus positive electricity；Film will be obtained again
Soaking 15min respectively in PAA solution, pure water cleans, and obtains the composite membrane of surface bear electricity, completes a bilayer.Repeat leaching
Bubble, obtaining the number of plies is 1.5,2.5,3.5,4.5,5.5 double-deck composite membranes.Then, 5 dry films are soaked in respectively through KOH
Reconcile, pH be 9, mass concentration be 1.9% the ethanol solution of epoxychloropropane in, 50 DEG C of cross-linking reactions 21h, cross-linking reaction is complete
Bi Hou, is dried, and through deionized water wash, is placed in pure water immersion more than 24h, to be determined.
5 films prepared MgCl to 1g/L2Solution rejection be followed successively by 31.59%, 50.76%, 69.88%,
81.71%, 83.62%, flux is 15.04L m-2·h-1、11.87L·m-2·h-1、9.61L·m-2·h-1、8.20L·m-2·h-1、5.49L·m-2·h-1, it is seen that the number of plies increases, and rejection substantially increases, but flux reduces, so the layer of film to be controlled
Number, is difficult to excessive.
Embodiment 5
The preparation HTCC solution of 5g/L and the PAA solution of 1g/L, regulate PAA pH value of solution respectively to 7 by NaOH solution,
HTCC solution and PAA solution are separately added into NaCl as support salt, make NaCl concentration and be respectively 0.025g/L, 0.05g/L,
The casting solution of 0.075g/L, 0.1g/L.4 PES basement membranes are immersed in 4 kinds there is different support in salinity HTCC casting solution
15min, cleans with pure water, obtains the composite membrane of surface lotus positive electricity；Again obtain 4 films had different support at 4 kinds respectively
Soaking 15min in salinity PAA solution, pure water cleans, and obtains the composite membrane of surface bear electricity, completes a bilayer.Repeat leaching
Bubble, obtaining the number of plies is 4.5 double-deck composite membranes.Then, 4 dry films are soaked in respectively through KOH reconcile, pH be 9, quality dense
Degree is in the ethanol solution of the epoxychloropropane of 1.9%, 50 DEG C of cross-linking reactions 21h, after cross-linking reaction, be dried, through go from
Sub-water washs, and is placed in pure water immersion more than 24h, to be determined.
4 films prepared MgCl to 1g/L2Solution rejection be followed successively by 54.47%, 70.69%, 81.71%,
73.56%, it is seen that supporting salinity increases, film surface charge particle combines tightr, increases inorganic salt rejection, but concentration
Too high, rejection effect can be reduced on the contrary.
Embodiment 6
The preparation HTCC solution of 5g/L and the PAA solution of 1g/L, regulate PAA pH value of solution respectively to 7 by NaOH solution,
HTCC solution and PAA solution is separately added into NaCl as supporting salt, make HTCC casting solution that NaCl concentration is 0.05g/L and
PAA casting solution.PES basement membrane is immersed in 10min in HTCC casting solution, cleans with pure water, obtain the composite membrane of surface lotus positive electricity；
The film obtained soaks in PAA solution 10min again, and pure water cleans, and obtains the composite membrane of surface bear electricity, completes one pair
Layer.Repeating to soak, obtaining the number of plies is 4.5 double-deck composite membranes.Then, composite membrane is soaked in through KOH reconcile, pH be 9, matter
Amount concentration is in the ethanol solution of epoxychloropropane of 1.9%, and 45 DEG C of cross-linking reactions 21h, after cross-linking reaction, are dried, warp
Deionized water wash, is placed in pure water immersion more than 24h, to be determined.
The film the prepared MgCl to 1g/L2Solution rejection be 70.36%.Understand, shorten soak time, reduce and hand over
Connection temperature can affect deposition effect, cross-links insufficient, reduces the rejection of film.
Embodiment 7
The preparation HTCC solution of 5g/L and the PAA solution of 1g/L, regulate PAA pH value of solution respectively to 7 by NaOH solution,
HTCC solution and PAA solution is separately added into NaCl as supporting salt, make HTCC casting solution that NaCl concentration is 0.05g/L and
PAA casting solution.PES basement membrane is immersed in 20min in HTCC casting solution, cleans with pure water, obtain the composite membrane of surface lotus positive electricity；
The film obtained soaks in PAA solution 20min again, and pure water cleans, and obtains the composite membrane of surface bear electricity, completes one pair
Layer.Repeating to soak, obtaining the number of plies is 4.5 double-deck composite membranes.Then, composite membrane is soaked in through KOH reconcile, pH be 9, matter
Amount concentration is in the ethanol solution of epoxychloropropane of 1.9%, and 55 DEG C of cross-linking reactions 21h, after cross-linking reaction, are dried, warp
Deionized water wash, is placed in pure water immersion more than 24h, to be determined.
The film the prepared MgCl to 1g/L2Solution rejection be 79.62%, it is known that long soaking time, crosslinking temperature
Spend height and can reduce rejection effect, suitable soak time and crosslinking temperature should be selected.
As seen from the above embodiment, the preparation method of the chitosan Positively charged composite nanofiltration membrane of the present invention is by regulation PAA
The concentration of pH, PAA solution of solution, the addition of support salt NaCl, inquired into the impact on film properties of the different masking factor.When
When the pH of PAA solution is 7, the concentration of PAA solution is 1g/L, support salt NaCl concentration is 0.05g/L, the film of gained is to 1g/L's
The rejection of MgCL2 reaches peak 81.71%, and corresponding water flux is 8.20L m-2·h-1, this condition is optimal masking
Condition.
Embodiment 8
The preparation HTCC solution of 5g/L and the PAA solution of 1g/L, regulate PAA pH value of solution respectively to 7 by NaOH solution,
HTCC solution and PAA solution is separately added into NaCl as supporting salt, make HTCC casting solution that NaCl concentration is 0.05g/L and
PAA casting solution.PES basement membrane is immersed in 15min in HTCC casting solution, cleans with pure water, obtain the composite membrane of surface lotus positive electricity；
The film obtained soaks in PAA solution 15min again, and pure water cleans, and obtains the composite membrane of surface bear electricity, completes one pair
Layer.Repeating to soak, obtaining the number of plies is 4.5 double-deck composite membranes.Then, dry film is soaked in through KOH reconcile, pH be 9, quality
Concentration is in the ethanol solution of the epoxychloropropane of 1.9%, 50 DEG C of cross-linking reactions 21h, after cross-linking reaction, is dried, through going
Ionized water washs, and is placed in pure water immersion more than 24h, to be determined.
Understanding in conjunction with Fig. 2, the pure water infiltration coefficient of composite membrane is 19.29L h-1·m-2·Mpa；Understand in conjunction with Fig. 3, multiple
The molecular cut off closing film is 989, belongs to molecular cut off (200-2000) scope of NF membrane；Understand in conjunction with Fig. 4, composite membrane
MgCl to 1g/L2, NaCl, KCl, MgSO4, Na2SO4Rejection be followed successively by 81.71%, 60.65%, 52.83%,
29.02%, 23.79%, present positively charged nanofiltration membranes retains characteristic；Understanding in conjunction with Fig. 5, composite membrane is to four kinds of PPCPs Malaysias
Acid amlodipine, atenolol, carbamazepine, the rejection of ibuprofen is followed successively by 86.7%, 80.1%, 71.4%, 63.9%,
Also illustrate that composite nanometer filtering film lotus electropositive.
Claims (5)
1. the preparation method of n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film, it is characterised in that specifically comprise the following steps that
Step 1, preparation 4～6g/L n-trimethyl chitosan chloride solution and the polyacrylic acid solution of 1～2g/L, poly-with NaOH solution regulation
The pH of acrylic acid solution is 6～8, is separately added into NaCl, is configured to containing the casting solution that NaCl mass concentration is 0.05～0.1g/L,
It is sufficiently stirred for, makes NaCl be uniformly dispersed；
Step 2, is first immersed in polyether sulfone basement membrane in n-trimethyl chitosan chloride casting solution, is immersed in polyacrylic acid casting film after cleaning again
In liquid, form a bilayer, continue to soak alternating deposit in n-trimethyl chitosan chloride casting solution and polyacrylic acid casting solution, layer by layer
It is self-assembled into 3.5～5.5 bilayers, obtains the composite membrane of surface lotus positive electricity；
Step 3, is dried LBL self-assembly composite membrane, be soaked in through KOH regulation, pH be 9 ± 1, mass concentration be 1.3%～
In the ethanol solution of the epoxychloropropane of 2.5%, 45～55 DEG C of cross-linking reactions 21～24h, crosslinking is dried after terminating, cleans,
To n-trimethyl chitosan chloride/polyacrylic acid composite nanometer filtering film.
The preparation method of n-trimethyl chitosan chloride the most according to claim 1/polyacrylic acid composite nanometer filtering film, its feature exists
In, in step 1, the concentration of described n-trimethyl chitosan chloride solution is 5g/L.
The preparation method of n-trimethyl chitosan chloride the most according to claim 1/polyacrylic acid composite nanometer filtering film, its feature exists
In, in step 2, the soak time at casting solution is 10～20min, and the described self assembly number of plies is 4.5 layers, polyether sulfone basement membrane
Molecular cut off is 10000, and effective area is 12.56cm2。
The preparation method of n-trimethyl chitosan chloride the most according to claim 1/polyacrylic acid composite nanometer filtering film, its feature exists
In, in step 3, the mass concentration of the ethanol solution of described epoxychloropropane is 1.9%, and described crosslinking temperature is 50 DEG C.
5. n-trimethyl chitosan chloride/polyacrylic acid the composite nanometer filter prepared according to the arbitrary described preparation method of Claims 1-4
Film.
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