CN104959048A - Reverse osmosis composite membrane containing layered nanometer clay - Google Patents
Reverse osmosis composite membrane containing layered nanometer clay Download PDFInfo
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- CN104959048A CN104959048A CN201510288805.5A CN201510288805A CN104959048A CN 104959048 A CN104959048 A CN 104959048A CN 201510288805 A CN201510288805 A CN 201510288805A CN 104959048 A CN104959048 A CN 104959048A
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Abstract
The present invention discloses a reverse osmosis composite membrane containing layered nanometer clay. The preparation method comprises: respectively immersing a polysulfone supporting membrane into a polyamine solution or polyacyl chloride solution, such that the polyacyl chloride and the polyamine are subjected to an interface polymerization reaction, wherein at least one of the polyamine solution or polyacyl chloride solution contains nanometer clay. According to the present invention, the reverse osmosis composite membrane material containing nanometer clay is provided, the preparation process is convenient, and the prepared reverse osmosis composite membrane containing layered nanometer clay has excellent stability, provides high desalination rate and high water flux rate compared with the polyamide reverse osmosis composite membrane, and has good pollution resistance on various pollutants.
Description
Technical field
The present invention relates to novel trans permeable membrane material field, particularly relate to a kind of nanoclay possessing high separability energy and anti-fouling performance and fill reverse osmosis composite membrane.
Background technology
Reverse osmosis technology has the high and environment facies of purification efficiency to advantages such as close friends, and the appearance of high-performance reverse osmosis composite membrane has driven the extensive use of reverse osmosis technology in various fields, and seawater and brackish water desalination are topmost applications.In addition, reverse osmosis technology is also used to the removal of micro heavy ion in water, and the process to waste water such as pharmacy, printing and dyeing and petrochemical industries.Reverse osmosis membrane is the core of reverse osmosis process, and wherein high flux and high rejection are the most critical key elements of reverse osmosis membrane performance, which determines separative efficiency and the cost of reverse osmosis process.In addition, anti-pollution is also weigh the important indicator of reverse osmosis membrane performance, and especially in the separation process that wastewater treatment etc. is more containing each pollutant, fouling membrane can cause film aquifer yield to decline, produce the problems such as water water degradation and film shorten service life.Therefore, the study hotspot that the reverse osmosis membrane with high separability energy and anti-fouling performance becomes field of membrane material is prepared.
In recent years, along with the fast development of nano science, multiple nanometer new material is proved to be has potential application in water treatment procedure, by inorganic nanoparticles is filled in continuous polymer phase as decentralized photo, in conjunction with organic and inorganic material advantageous property separately, high performance membrane material can be prepared.For reverse osmosis composite membrane, filler main is at present the nano material with loose structure, as molecular sieve and nanotube etc.Existing research mainly concentrates on and utilizes the sieving actoion of nano pore to improve the separating property of film, and need further excavation to other the functional utilizations of novel nano packing material.
Lamellar clay belongs to two-dimension nano materials, is usually made up of hydrosilicate, also can be made up of metal oxides such as silicon, aluminium, magnesium.Due to the layer structure of clay material uniqueness and the physical and chemical performance of many excellences, lamellar clay-polymer nanocomposites is the study hotspot of high-performance field of new.Different according to the ionic species between clay layer, lamellar clay can be divided into cationic clay and anionic clay.Cationic clay is with montmorillonite (montmorillonite, MMT) for representative, and its lamella itself is with negative electricity, and different sheet interlayer exists free cation.Anionic clay take hydrotalcite as representative, the main body of hydrotalcite is generally made up of the hydroxide of two kinds of metals, therefore also referred to as layered double-hydroxide (layered double hydroxides, LDH), lamella is because same order elements is with permanent positive charge, and interlayer exists free anion.Have benefited from that lamellar clay specific area is large, ion exchange capacity is high, the advantage such as lamella and interlamination region chemical composition easy-regulating, nanoclay is widely used in fields such as catalyst carrier, adsorbent, ion-exchanger and composites.Clay is prepared reverse osmosis composite membrane as inorganic nano packing material, utilizes the distinctive charge of clay layer and hydrophily to regulate and control membrane structure and surface nature, will be expected to obtain the novel trans permeable membrane material possessing high separability energy and anti-fouling performance.
Summary of the invention
The invention provides a kind of reverse osmosis composite membrane material containing nanoclay, the film of preparation has good separating property and anti-fouling performance.
Reverse osmosis composite membrane material containing nanoclay of the present invention, nanoclay comprises cationic clay montmorillonite (MMT) and anionic clay layered double-hydroxide (LDH), the clay layer lateral dimension used is nanoscale, by clay dispersion in interfacial polymerization aqueous phase or organic phase monomer solution, after film forming, nanoclay can be embedded in the polyamide-based of reverse osmosis membrane, thus can realize the regulation and control to film surface hydrophilicity and charge.
Containing a reverse osmosis composite membrane for layered nanoclay, its preparation method comprises: polysulfones support membrane is immersed in respectively polyamine solution or polynary solution of acid chloride, makes polynary acyl chlorides and polyamine carry out interface polymerization reaction; In described polyamine solution or polynary solution of acid chloride at least one containing nanoclay.
Preferred two kinds of methods are:
Containing a reverse osmosis composite membrane for layered nanoclay, comprising:
Shearing force is carried out to cationic clay MMT and anionic clay LDH and assists swelling lift-off processing, first clay powders is dispersed in water, stir 3 ~ 5 hours at 60 ~ 80 DEG C, make it fully swelling and be uniformly dispersed, recycling mechanical stirring device carries out stir process 7 ~ 12 days with the speed of 500 ~ 1000rpm to this dispersion liquid, after mechanical agitation terminates, sediment is removed in dispersion liquid sedimentation, collected by centrifugation product.
Cationic clay MMT is distributed in polynary solution of acid chloride, obtains mixture A; Anionic clay LDH is distributed in polynary solution of acid chloride, obtains mixture B.Polysulfones support membrane is immersed in the aqueous solution of polyamine, the immersion time is 1 ~ 10min, take out film and remove residual solution, itself and said mixture A or B are carried out interface polymerization reaction, the film after having reacted obtains the reverse osmosis composite membrane containing nanoclay through post processing.
Cationic clay MMT is distributed in polyamine solution, obtains mixture C; Anionic clay LDH is distributed in polyamine solution, obtains mixture D.Polysulfones support membrane is immersed in the polyamine aqueous solution containing nanoclay, the immersion time is 1 ~ 10min, take out film and remove residual solution, itself and polynary solution of acid chloride are carried out interface polymerization reaction, the film after having reacted obtains the reverse osmosis composite membrane containing nanoclay through post processing.
When preparing mixture A ~ D, for ensureing that nanoclay mixes with solution, carry out thermostatic ultrasonic process to mixture, the processing time is not less than 20 minutes.
In mixture A ~ D, the weight percent concentration of nanoclay is: 0.02 ~ 0.2%, and the weight percent concentration of preferred nanoclay is 0.05 ~ 0.1%.
As preferably, described cationic clay MMT selects na-montmorillonite (Na
+-MMT) or ca-montmorillonite (Ca
+-MMT); Described anionic clay LDH selects Mg/Al-Cl-LDH or Mg/Al-NO
3-LDH; The lamella lateral dimension of nanoclay is 100 ~ 200 nanometers, and radius-thickness ratio is 10 ~ 50.
As preferably, in the described polyamine aqueous solution, the weight percent concentration of polyamine is 0.5 ~ 3%, more preferably 1 ~ 3%, be further preferably 2%.
As preferably, the solvent of described polynary solution of acid chloride is C
5~ C
8fat alkane, in polynary solution of acid chloride, the weight percent concentration of polynary acyl chlorides is 0.05 ~ 1%, more preferably 0.1 ~ 0.5%, be further preferably 0.1%.In described polynary solution of acid chloride, preferred solvent is
As preferably, described polyamine is preferably m-phenylene diamine (MPD); Described polynary acyl chlorides is preferably pyromellitic trimethylsilyl chloride.
As preferably, the reaction time of described interface polymerization reaction is 5 ~ 60 seconds, more preferably 20 ~ 30 seconds.
As preferably, the method removing residual solution can adopt natural air drying or extrude with rubber roll.
As preferably, after described interface polymerization reaction completes, film is heat-treated 5 ~ 10 minutes at 80 ~ 90 DEG C of baking ovens, after rinsing, obtain the reverse osmosis composite membrane containing nanoclay.
The invention provides a kind of containing nanoclay reverse osmosis composite membrane material, its preparation process is convenient, the excellent in stability containing lamellar clay reverse osmosis composite membrane of preparation, salt rejection rate and water flux, higher than polyamide reverse osmosis composite film, have good stain resistance to each pollutant.
Accompanying drawing explanation
The nanoclay TEM that Fig. 1 uses for embodiment 1 ~ 8 schemes, and wherein (a), (b) are Na
+-MMT, (c), (d) Mg/Al-Cl-LDH;
The surperficial SEM figure of the complex reverse osmosis membrane of Fig. 2 prepared by comparative example 1;
The surperficial SEM figure of the complex reverse osmosis membrane of Fig. 3 prepared by embodiment 3;
The surperficial SEM figure of the complex reverse osmosis membrane of Fig. 4 prepared by embodiment 7;
The protein contamination test result of the complex reverse osmosis membrane of Fig. 5 prepared by embodiment 3;
The cationic surfactant Contamination measurement result of the complex reverse osmosis membrane of Fig. 6 prepared by embodiment 7.
Detailed description of the invention
Reverse osmosis composite membrane prepared by the present invention is used for desalination, and salt rejection rate and water flux are two important parameters evaluating reverse osmosis composite membrane, and salt rejection rate R is defined as:
Wherein, C
frepresent the concentration of salt in the front water of process; C
prepresent the concentration of salt in the rear permeate of process.
Water flux is defined as: under certain operating conditions, and through the volume of the water of per membrane area in the unit interval, its unit is L/m
2h.
The test condition adopted in the present invention is: the sodium-chloride water solution of 2000ppm, and operating pressure is 232psi, and operating temperature is 25 DEG C.
Reverse osmosis composite membrane prepared by the present invention is for the treatment of the feed liquid containing pollutant, utilize bovine serum albumin (BSA), DTAB (DTAB) as simulating pollution thing, investigated the anti-fouling performance of film by the attenuation of normalization flux.
J in formula
nfor the normalization flux of film, J
ffor the transitory flux of film in running, J
0for the initial flux of film.
The polysulfones support membrane used in the embodiment of the present invention is the polysulfone porous milipore filter of 30 ~ 40 nanometers for average pore size, derives from Hangzhou Water Treatment Technological Research Development Center.
Comparative example 1
Polysulphone super-filter membrane being immersed in mass percent concentration is that in the m-phenylene diamine (MPD) aqueous solution of 2%, the immersion time is 2min, drains residual droplets in atmosphere, is the pyromellitic trimethylsilyl chloride of 0.1% immediately with mass percent concentration
solution carries out interface polymerization reaction 25 seconds obtained composite membranes, reaction terminates rear discharge organic phase solution, diaphragm is placed in forced air oven 90 DEG C of dryings 5 minutes, finally repeatedly rinse the diaphragm deionized water prepared to remove unreacted monomer and residual solvent, then be placed in deionized water and preserve to be measured.
Embodiment 1-4
By the na-montmorillonite (Na after a certain amount of process
+-MMT) be dispersed in organic phase monomer solution (organic phase monomer solution to be mass percent concentration be 0.1% pyromellitic trimethylsilyl chloride
solution) in, wherein the lamella lateral dimension of montmorillonite is montmorillonite Shape measure result figure at about 200nm, Fig. 1 (a), (b).In monomer solution, the concentration of montmorillonite is 0.02wt%, 0.05wt%, 0.10wt%, 0.2wt%, ultrasonic process 20 minutes under normal temperature.Polysulphone super-filter membrane being immersed in mass percent concentration is that in the m-phenylene diamine (MPD) aqueous solution of 2%, the immersion time is 2min, drains residual droplets in atmosphere, immediately be the pyromellitic trimethylsilyl chloride of 0.1% containing the mass percent concentration of montmorillonite
solution carries out interfacial polymerization, reaction time is 25 seconds, reaction terminates rear discharge organic phase solution, diaphragm is placed in forced air oven 90 DEG C of dryings 5 minutes, finally repeatedly rinse the diaphragm deionized water prepared to remove unreacted monomer and residual solvent, then be placed in deionized water and preserve to be measured.
What prepare embodiment 3 (concentration of montmorillonite is 0.1wt%) carries out SEM sign containing nanoclay reverse osmosis composite membrane, and contrast with the reverse osmosis composite membrane (prepared by comparative example 1) not adding nanoclay, result as shown in Figures 2 and 3, Fig. 3 is the testing result figure containing nanoclay reverse osmosis composite membrane prepared by embodiment 3, as can be seen from Figure, there is more lobed projection structure in the surface containing nanoclay reverse osmosis composite membrane.
Separating property test case 1
Be 232psi at operating pressure, operating temperature is under the condition of 25 DEG C, respectively by the reverse osmosis composite membrane of the sodium-chloride water solution of 2000ppm by being prepared by the reverse osmosis composite membrane containing nano montmorillonite clay obtained and the comparative example 1 of embodiment 1 ~ 4 preparation, calculate flux and the salt rejection rate of each composite membrane respectively, test result is as shown in table 1: the reverse osmosis composite membrane containing nano montmorillonite clay that visible the present invention is prepared into, and is all significantly increased than the pure polyamide reverse osmosis composite film flux prepared under equal conditions and salt rejection rate.
Table 1
| Embodiment | Montmorillonite weight percent concentration (%) | Flux (L/m 2.h) | Salt rejection rate (%) |
| Comparative example 1 | 0 | 36.6 | 98.8 |
| 1 | 0.02 | 48.4 | 98.8 |
| 2 | 0.05 | 51.7 | 98.9 |
| 3 | 0.10 | 47.0 | 99.0 |
| 4 | 0.20 | 44.1 | 99.1 |
Anti-fouling performance test case 1
Under the operating condition of separating property test case 1, add 60ppm BSA as simulating pollution thing in feed liquid, run 30 hours, by investigating the flux decline situation of film, evaluated for film is to the tolerance of protein contamination.Fig. 5 is the anti-fouling performance test result of comparative example 1 and embodiment 3.After the Contamination measurement of 30 hours, the flux of pure PA membrane prepared by comparative example 1 drops to about 60%, and the membrane flux containing montmorillonite that under the same conditions prepared by embodiment 3 only drops to 81%, illustrates that anti-fouling performance significantly improves.This is because the filling of montmorillonite makes film surface electrical negativity strengthen, and contributes to forming hydration layer on film surface, and then reduces the suction-operated of film surface to hydrophobic protein.
Embodiment 5-8
Magnesium-aluminum-based laminar double hydroxide (Mg/Al-LDH) after a certain amount of process is dispersed in organic phase monomer solution, wherein the lamella lateral dimension of LDH is LDH Shape measure result figure at about 100nm, Fig. 1 (c), (d).In organic phase monomer solution, the concentration of LDH is 0.02wt%, 0.05wt%, 0.10wt%, 0.2wt%, ultrasonic process 20 minutes under normal temperature.Composite membrane preparation method is identical with embodiment 1-4.
SEM sign is carried out containing nanoclay LDH reverse osmosis composite membrane to what prepare, and the pure polyamide reverse osmosis composite film prepared containing nanoclay LDH reverse osmosis composite membrane and comparative example 1 embodiment 7 (concentration of LDH is 0.10wt%) prepared contrasts, result as shown in Figure 2 and Figure 4, Fig. 4 be embodiment 7 prepare containing nanoclay LDH reverse osmosis composite membrane testing result figure, as can be seen from Figure, little containing changing compared with former film prepared by surface texture and the comparative example 1 of LDH reverse osmosis composite membrane, but can observe on film surface the LDH nanoclay lamella be embedded in polyamide.
Performance test example 2
What the method identical with performance test example 1 prepared embodiment 5 ~ 8 tests containing LDH reverse osmosis composite membrane, and test result is as shown in table 2.Result shows, the reverse osmosis composite membrane flux containing LDH that the present invention prepares and the purer PA membrane of rejection significantly improve, but flux lifting amplitude does not have embodiment 1 ~ 4 remarkable.
Table 2
Anti-fouling performance test case 2
Under the operating condition of separating property test case 2, in feed liquid, add 25ppm DTAB as simulating pollution thing, run 12 hours, by investigating the flux decline situation of film, the tolerance that evaluated for film is polluted cationic surfactant.Fig. 6 is the anti-fouling performance test result of comparative example 1 and embodiment 7.In 1 hour after DTAB adds feed liquid, the flux of film sharply declines, and after this tends towards stability gradually, and the film surface rapid adsorption be deposited as pollution layer of the DTAB of lotus positive electricity at bear electricity is described.Can obviously be found out by comparative film flux decline situation, the mixed substrate membrane containing nano-grade molecular sieve adding LDH has better anti-fouling performance, and after the anti-pollution test of 12 hours, the flux of film drops to about 40% of original flux; And under the same conditions, the flux of pure PA membrane has dropped to about 25% of original flux.The introducing of LDH nanoclay improves the anti-fouling performance of film to cationic surfactant, this is mainly because mixed substrate membrane containing nano-grade molecular sieve surface bear electrically weakens, reduce the electrostatic adsorption power on pollutant and film surface, thus decrease the deposition of pollutant, make film be provided with good tolerance to lotus positive electricity type pollutant.
Above embodiment result shows, the more former film of separating property containing the reverse osmosis composite membrane of nanoclay increases, and it is better when in mixed liquor, nanoclay weight percent concentration is 0.05 ~ 0.1%, the filling of dissimilar nanoclay can also regulate and control hydrophily and the charge on film surface, thus significantly improves the tolerance of film to different pollutant.The reverse osmosis composite membrane containing layered nanoclay prepared by the present invention has high separability energy and anti-fouling performance concurrently.
Claims (10)
1., containing a reverse osmosis composite membrane for layered nanoclay, it is characterized in that, its preparation method comprises: polysulfones support membrane is immersed in respectively polyamine solution or polynary solution of acid chloride, makes polynary acyl chlorides and polyamine carry out interface polymerization reaction; In described polyamine solution or polynary solution of acid chloride at least one containing nanoclay.
2. the reverse osmosis composite membrane containing layered nanoclay according to claim 1, it is characterized in that, described nanoclay is selected from cationic clay MMT or anionic clay LDH.
3. the reverse osmosis composite membrane containing layered nanoclay according to claim 2, it is characterized in that, described cationic clay MMT is selected from Na
+-MMT or Ca
+-MMT; Described anionic clay LDH is selected from Mg/Al-Cl-LDH or Mg/Al-NO
3-LDH.
4. the reverse osmosis composite membrane containing layered nanoclay according to the arbitrary claim of claim 1-3, it is characterized in that, described nanoclay is obtained by following method:
First clay powders is dispersed in water, stir 3 ~ 5 hours at 60 ~ 80 DEG C, make it fully swelling and be uniformly dispersed, recycling mechanical stirring device carries out stir process 7 ~ 12 days with the speed of 500 ~ 1000rpm to this dispersion liquid, after mechanical agitation terminates, sediment is removed in dispersion liquid sedimentation, collected by centrifugation product, obtains nanoclay.
5. the reverse osmosis composite membrane containing layered nanoclay according to claim 1, is characterized in that, in described polyamine solution or polynary solution of acid chloride, the weight percent concentration of clay is 0.02 ~ 0.2%.
6. the reverse osmosis composite membrane containing layered nanoclay according to claim 1, it is characterized in that, in described polyamine solution, the weight percent concentration of polyamine is 0.5 ~ 3%.
7. the reverse osmosis composite membrane containing layered nanoclay according to claim 1 or 6, it is characterized in that, polyamine is m-phenylene diamine (MPD), and in the polyamine aqueous solution, solvent is water.
8. the reverse osmosis composite membrane containing layered nanoclay according to claim 1, it is characterized in that, in described polynary solution of acid chloride, the weight percent concentration of polynary acyl chlorides is 0.05 ~ 1%.
9. the reverse osmosis composite membrane containing layered nanoclay according to claim 1 or 8, it is characterized in that, polynary acyl chlorides is pyromellitic trimethylsilyl chloride, and the solvent of polynary solution of acid chloride is C
5~ C
8fat alkane.
10. the reverse osmosis composite membrane containing layered nanoclay according to claim 1, it is characterized in that, the reaction time of described interface polymerization reaction is 5 ~ 60 seconds.
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| CN108854587A (en) * | 2018-06-28 | 2018-11-23 | 山东大学 | A kind of high-throughput, antibacterial type doping hectorite-metal ion reverse osmosis composite membrane preparation method |
| CN109289544A (en) * | 2018-09-26 | 2019-02-01 | 同济大学 | A method of preparing two-dimentional montmorillonite/cellulose composite filtering film |
| CN111001298A (en) * | 2019-12-30 | 2020-04-14 | 天津天元新材料科技有限公司 | Preparation method of modified reverse osmosis membrane |
| CN111085117A (en) * | 2019-11-28 | 2020-05-01 | 丁水英 | High-water-permeability reverse osmosis membrane and preparation method thereof |
| CN111686588A (en) * | 2020-07-02 | 2020-09-22 | 厦门理工学院 | Composite nanofiltration membrane with layered double hydroxide as modified template and preparation method thereof |
| CN112588124A (en) * | 2020-11-25 | 2021-04-02 | 常州大学 | Metal hydroxide modified polyamide composite nanofiltration membrane as well as preparation method and application thereof |
| CN115318101A (en) * | 2022-09-05 | 2022-11-11 | 北京工业大学 | Preparation method of layered double-metal hydroxide nanofiltration membrane for magnesium-lithium separation |
| CN115400612A (en) * | 2022-08-31 | 2022-11-29 | 西北工业大学 | Modified polyamide separation membrane for resisting scaling and oxidation and preparation method thereof |
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| CN108854587A (en) * | 2018-06-28 | 2018-11-23 | 山东大学 | A kind of high-throughput, antibacterial type doping hectorite-metal ion reverse osmosis composite membrane preparation method |
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| CN109289544A (en) * | 2018-09-26 | 2019-02-01 | 同济大学 | A method of preparing two-dimentional montmorillonite/cellulose composite filtering film |
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| CN111686588A (en) * | 2020-07-02 | 2020-09-22 | 厦门理工学院 | Composite nanofiltration membrane with layered double hydroxide as modified template and preparation method thereof |
| CN111686588B (en) * | 2020-07-02 | 2022-04-01 | 厦门理工学院 | Composite nanofiltration membrane with layered double hydroxide as modified template and preparation method thereof |
| CN112588124A (en) * | 2020-11-25 | 2021-04-02 | 常州大学 | Metal hydroxide modified polyamide composite nanofiltration membrane as well as preparation method and application thereof |
| CN115400612A (en) * | 2022-08-31 | 2022-11-29 | 西北工业大学 | Modified polyamide separation membrane for resisting scaling and oxidation and preparation method thereof |
| CN115318101A (en) * | 2022-09-05 | 2022-11-11 | 北京工业大学 | Preparation method of layered double-metal hydroxide nanofiltration membrane for magnesium-lithium separation |
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