CN109289560A - A kind of preparation method of electromagnetic field regulation self-healing seperation film - Google Patents
A kind of preparation method of electromagnetic field regulation self-healing seperation film Download PDFInfo
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- CN109289560A CN109289560A CN201811254403.3A CN201811254403A CN109289560A CN 109289560 A CN109289560 A CN 109289560A CN 201811254403 A CN201811254403 A CN 201811254403A CN 109289560 A CN109289560 A CN 109289560A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 230000033228 biological regulation Effects 0.000 title claims abstract description 15
- 230000005672 electromagnetic field Effects 0.000 title claims abstract description 15
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 13
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 11
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 22
- 239000000178 monomer Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000003431 cross linking reagent Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- 230000005291 magnetic effect Effects 0.000 abstract description 18
- 238000000926 separation method Methods 0.000 abstract description 15
- 230000005684 electric field Effects 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 3
- 229920001577 copolymer Polymers 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 238000010257 thawing Methods 0.000 abstract description 2
- 238000004132 cross linking Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 210000004379 membrane Anatomy 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 12
- 239000000499 gel Substances 0.000 description 9
- 238000001914 filtration Methods 0.000 description 8
- 239000000706 filtrate Substances 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001612 separation test Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 230000003204 osmotic effect Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229920002492 poly(sulfone) Polymers 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- KVYRCBOUKXJXDK-UHFFFAOYSA-N 3,4-dimethylphenazine-1,2-diamine hydrochloride Chemical compound Cl.C1=CC=CC2=NC3=C(C)C(C)=C(N)C(N)=C3N=C21 KVYRCBOUKXJXDK-UHFFFAOYSA-N 0.000 description 1
- 229910002567 K2S2O8 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- DMLAVOWQYNRWNQ-UHFFFAOYSA-N azobenzene Chemical compound C1=CC=CC=C1N=NC1=CC=CC=C1 DMLAVOWQYNRWNQ-UHFFFAOYSA-N 0.000 description 1
- 210000002469 basement membrane Anatomy 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000005426 magnetic field effect Effects 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000009285 membrane fouling Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920003213 poly(N-isopropyl acrylamide) Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- 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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2649—Filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a kind of preparation methods of electromagnetic field regulation self-healing seperation film, it is characterized by: the copolymer that dimethylaminoethyl methacrylate and methacrylic acid are formed is as the material of main part of seperation film, nano ferriferrous oxide particle is used as the magnetic core of magnetic response, polyvinyl alcohol is used to realize self-healing function, and the carbon quantum dot that methacrylic acid and p-phenylenediamine generate during the reaction provides enhancing seperation film mechanical performance as the auxiliary crosslinking points of polyvinyl alcohol.Compared with prior art, the present invention has the advantages that this method prepares the seperation film with self-healing performance using pregel preparation, polymerization for the treatment of different things alike, three step of freeze thawing treatment, and it can control pore size when applying electric field or magnetic field and realize controllable separation, the preparation method of the seperation film is simple, there are multiple functions simultaneously, long service life, application value with higher.
Description
Technical field
The present invention relates to technical field of membrane separation, refer specifically to a kind of preparation method of electromagnetic field regulation self-healing seperation film.
Background technique
Separation science and technology all have important support work in many fields such as chemistry, chemical industry, pharmacy, environment, material
With wherein UF membrane science and technology has many advantages such as that low energy consumption, separative efficiency is high, obtains extensively in water treatment field
General application.UF membrane is the selective penetrated property according to film, seperation film is made wall, in pressure difference, concentration difference or potential difference
It is different through the rate of film by means of each component in fluid mixture under motive force, it is allowed to be enriched with respectively in the two sides of film, to reach point
From, purification, concentration and recycle purpose.Separation membrane material mainly includes inorganic and organic polymer two major classes, and organic
High molecular material is widely studied and applies because its is many kinds of.There are commonly celluloses for the high molecular material of preparative separation film
Esters, polysulfones, polyphenylene oxide, aromatic polyamides, polypropylene etc., and this kind of polymeric membrane for separation has been industrialized, commodity
Change application.
A problem existing for existing seperation film is: membrane aperture is substantially fixation, to the rejection or transmission of substance
Rate is relatively stable, cannot continuously separate a series of substances of different molecular weight ranges.Currently, having been done in terms of the performance improvement of film
A large amount of research, such as patent of invention " a kind of Low-resistance high-flux anti-pollution type water that number of patent application is CN201310320378.5
Process film and preparation method thereof " disclose a kind of Low-resistance high-flux anti-pollution type membrane for water treatment, the film with sulfonated polyether sulfone-polysulfones/
TiO2Ultrafiltration membrane is template, generates Fe in basement membrane duct by in-situ synthesized3O4Nanoparticle obtains Fe3O4/ sulfonated polyether
Sulfone-polysulfones/TiO2The characteristics of magnetic ultrafiltration membrane, the film, is: enhancing the hydrophily of film, lessening membrane fouling, extend film uses the longevity
Life；A series of substances of continuous separation different molecular weight ranges are realized by adjusting externally-applied magnetic field；The defect of the film is, real
The externally-applied magnetic field for now continuously separating a series of additional 0.4T~1T of material demands of different molecular weight ranges, increases energy consumption, limits
Its application is made, and service life is limited.
Summary of the invention
The technical problem to be solved by the invention for the present situation of prior art is to provide a kind of preparation methods simply, makes
With the service life is long, the preparation method of seperation film that is widely used and has both electromagnetic field regulation self-healing function.
The present invention solves technical solution used by first technical problem are as follows: a kind of electromagnetic field regulation self-healing seperation film
Preparation method, it is characterised in that the following steps are included:
(1) monomer dimethylaminoethyl methacrylate and methacrylic acid that molar ratio is 2:1~4:1 are mixed,
It stirs 1~3 hour at room temperature, 0.05~2% crosslinking agent N, N '-the methylene bisacrylamide acyl that dosage is monomer mass is added
Amine stirs 3~5 hours, then is 0.1~1% initiator K of monomer mass by dosage2S2O8It dissolves in deionized water, so
It is added dropwise under stiring in the mixed solution of aforementioned monomer and crosslinking agent afterwards；
(2) methacrylic acid and p-phenylenediamine that molar ratio is 1:1~3:1 are mixed into solution, deionized water is added and stirs
It mixes uniformly, wherein deionized water is 8:1~12:1 with the volume ratio of methacrylic acid and p-phenylenediamine mixed solution, in high pressure
It is sealed in hydrothermal reaction kettle, reacts 2~4 hours at 180~220 DEG C, then cooled to room temperature；
(3) polyvinyl alcohol is add to deionized water, is heated 1~3 hour at 90~100 DEG C, 20~40 points of ultrasound
The bubble in solution is removed after clock, obtains the polyvinyl alcohol water solution that concentration is 20~40wt%；
(4) the nano ferriferrous oxide particle for being 2~5wt% by the solution and concentration that are prepared in step (1) (2) (3)
Water slurry is mixed according to volume ratio 1:0.4~0.6:0.9~1.1:0.4~0.6, is stirred evenly；
(5) clean stainless steel mesh screen will be pre-processed to be immersed in immediately in the mixed solution of step (4), then by surface
The mesh screen of attachment viscosity solution steadily takes out, and is heat-treated 5~7 hours sample at 60~80 DEG C under nitrogen protection, is cooled to
Room temperature；
(6) sample of step (5) is freezed 6~10 hours at -20~-16 DEG C, is thawed 10~14 hours at room temperature, weight
Multiple progress repeatedly, is prepared and can be realized the isolated multi-functional seperation film of self-healing of electromagnetic field regulation.
Preferably, in step (1), the molar ratio of the monomer dimethylaminoethyl methacrylate and methacrylic acid is
3:1, the dosage of crosslinking agent are the 1% of monomer mass, and the initiator amount is the 0.5% of monomer mass.
Preferably, in step (2), the molar ratio of the methacrylic acid and p-phenylenediamine is 2:1, the deionized water with
The volume ratio of methacrylic acid and p-phenylenediamine mixed solution is 10:1.
Preferably, in step (3), the concentration of the polyvinyl alcohol water solution is 35wt%.
Preferably, in step (4), the concentration of the nano ferriferrous oxide particle suspension is 3wt%.
Preferably, in step (4), the solution and nano ferriferrous oxide particle water prepared in step (1) (2) (3) is outstanding
Volume ratio when supernatant liquid mixes is 1:0.5:1:0.5.
Compared with the prior art, the advantages of the present invention are as follows:
(1) dimethylaminoethyl methacrylate and methacrylic acid and crosslinking agent N, N '-methylene bisacrylamide acyl are utilized
The soft gel of amine copolymer object realizes Selective Separation function as the material of main part of seperation film；
(2) polyvinyl alcohol, which is utilized, makes it have certain self-healing performance, can be real when seperation film is lesser damaged
Existing selfreparing is able to extend the service life of seperation film；
(3) it is further increased using the carbon dots that methacrylic acid and p-phenylenediamine reaction generate as polyvinyl alcohol crosslinked point
The mechanical strength of self-healing seperation film；
(4) carboxyl and amido in the composite material is utilized to have the function of ionization, under the electric field hydrogel intermediate ion
The osmotic pressure for changing hydrogel can be moved, so that the gel seperation film generates deformation and then changes pore size, realizes electric field
Regulate and control separating capacity；
(5) it using the nanometer Fe 3 O 4 magnetic particle being added when preparing the seperation film, is generated by externally-applied magnetic field
Magnetic field force effect realizes that magnetic field regulates and controls separating capacity so that the gel seperation film generates deformation and then changes pore size；
(6) although the seperation film belongs to soft gel rubber material, but improves in preparation using stainless steel metal silk screen as support
Mechanical strength is conducive to be separated by filtration use.
This method prepares point with self-healing performance using pregel preparation, polymerization for the treatment of different things alike, three step of freeze thawing treatment
From film, and it can control pore size when applying electric field or magnetic field and realize controllable separation, the preparation method of the seperation film is simple,
There is multiple functions, long service life, application value with higher simultaneously.
Specific embodiment
Present invention is further described in detail with reference to embodiments.
Comparative example 1, comparative example 2 and embodiment 1~15:
(1) monomer dimethylaminoethyl methacrylate and methacrylic acid are mixed, is stirred at room temperature 2 hours, adds
Enter crosslinking agent N, N '-methylene-bisacrylamide stirs 4 hours, then by initiator K2S2O8It dissolves in deionized water (herein
It is suitable for just being dissolved with a small amount of deionized water), it is then added dropwise to the mixed solution of aforementioned monomer and crosslinking agent under stiring
In；
(2) methacrylic acid and p-phenylenediamine are mixed into solution, deionized water is added and stirs evenly, it is anti-in high pressure hydro-thermal
It answers in kettle and seals, react 3 hours at 200 DEG C, then cooled to room temperature；This step reaction generates carbon dots solution；
(3) polyvinyl alcohol is add to deionized water, is heated 2 hours at 95 DEG C, ultrasound removed solution after 30 minutes
In bubble, obtain polyvinyl alcohol water solution；
(4) the nano ferriferrous oxide particle for being 2~5wt% by the solution and concentration that are prepared in step (1) (2) (3)
Water slurry is mixed according to volume ratio 1:0.5:1:0.5, is stirred evenly；
(5) clean stainless steel mesh screen will be pre-processed to be immersed in immediately in the mixed solution of step (4), then by surface
The mesh screen of attachment viscosity solution steadily takes out, and is heat-treated 6 hours sample at 70 DEG C under nitrogen protection, is cooled to room temperature；
(6) sample of step (5) is freezed 8 hours at -18 DEG C, is thawed 12 hours at room temperature, repeated three times, system
It is standby to obtain can be realized the isolated multi-functional seperation film of self-healing of electromagnetic field regulation.
Above-mentioned all comparative examples and the reaction condition of embodiment are as shown in table 1.
Steps are as follows for performance test:
(1) raw sample is tested: using the seperation film of preparation as filter membrane, being filtered separation examination with the artificial water sample of preparation
It tests；
(2) it destroys sample test: the common sewing-needle of seperation film being pricked into 10~20 holes, immediately with the artificial water sample prepared
It is filtered separation test；
(3) self-healing sample test: the seperation film punctured is cleaned up with deionized water, is placed 24 hours at room temperature
Self-healing is carried out, is filtered separation test with the artificial water sample of preparation；
(4) extra electric field sample test: DC power anode will be connected on the stainless steel mesh of seperation film, cathode connects
Ground, application+12V voltage are filtered separation test with the artificial water sample of preparation；It is changed to application -12V voltage again and repeats filtering point
Separating test；
(5) externally-applied magnetic field sample test: one flat plate type permanent magnet is placed in seperation film, with the artificial water sample of preparation
It is filtered separation test；Again that above-mentioned permanent magnet is oppositely positioned, repetition is separated by filtration test.
The performance test results of above-mentioned all comparative examples and embodiment are as shown in table 2.Wherein, mixed sample is manually prepared
Product contain the following substances (weight ratio): 3%100~150nm silicon dioxide granule, 1% chloroform, the nanometer of 0.5%40~60nm
Gold particle, 0.1% dimethyl diaminophenazine chloride, by being vigorously stirred to cloudy state before testing；× representative species are trapped, zero representative species into
Enter in filtrate, △ representative species small part is trapped, largely enters in filtrate, and ▼ representative species are largely trapped, lack portion
Divide and enters in filtrate.
By table 1~2 it can be seen that
(1) it is filtered separation test with raw sample, silicon dioxide granule and chloroform are trapped, nano Au particle and neutrality
It is red to enter in filtrate, illustrate that seperation film has the function of to efficiently separate；
(2) it carries out being separated by filtration test after being destroyed with sewing-needle, part of silica particle and chloroform enter filtrate, still have
Part is trapped, and is not achieved and is efficiently separated；It carries out being separated by filtration test after self-healing, silica and chloroform can be cut completely
It stays, has restored to efficiently separate function, therefore seperation film has self-healing function, this is mainly attributed to have in polyvinyl alcohol structures
The many Hydrogenbonds having；
(3) it carries out being separated by filtration test, silica and chloroform after application+12V voltage and be retained completely, nano Au particle
Part retention part enters filtrate, illustrates that separate membrane aperture becomes smaller under electric field action；It is filtered after application -12V voltage point
Separating test, part of silica enter filtrate, illustrate that separate membrane aperture becomes larger under electric field action；Therefore seperation film has electric field
The ability of adjustment aperture size；
(4) it carries out being separated by filtration test after applying positive magnetic field, silica, chloroform and nanogold are retained completely, said
Bright separation membrane aperture becomes smaller under magnetic fields；It carrying out being separated by filtration test after applying opposing magnetic field, separation test result is identical,
Illustrate that externally-applied magnetic field effect can become smaller the separation membrane aperture；
Why separation membrane aperture can be regulated and controled by electric field magnetic field, be because intelligent aqueous gel is a kind of with three
Dimension network structure, dilatancy is good, water imbibition is strong, the new functional macromolecule material of easy the features such as being retained, is super bionical, due to its conjunction
At being joined in the process with special construction, the monomer of group or macromolecular raw material, as polyacrylamide (PNIPA) class is divided greatly
(having on macromolecular chain can be with for son, acid/base group (such as carboxyl and amino), acrylic acid, poly- Ammonia, azobenzene (As), polyelectrolyte
The group of ionization) etc., therefore intelligent aqueous gel be can according to the temperature of the environment, acidity, electric field, magnetic field, illumination, pressure etc.
Regular structure and volume adjustment are made in variation, or gel is caused to form changed novel intelligent biochemistry water-setting
Glue material, intelligence and responsiveness with higher.Since intelligent aqueous gel belongs to soft material, nanometer four is added wherein and aoxidizes
Three ferromagnetic particles, can be allowed to that deformation occurs by means of external magnetic field.If such soft gel is prepared into seperation film, pass through magnetic field
The pore size that power can also regulate and control seperation film realizes separation selectivity.The carboxyl that methacrylic acid contains has ionization energy
Power promotes ionization and ion mobile to change osmotic pressure, the seperation film being made from it is in electric field force under DC Electric Field
Under effect, it can also be changed by osmotic pressure and lead to the change for separating membrane aperture, realize the control to separation process.
The reaction condition of table 1 all comparative examples and embodiment
The performance test results of table 2 all comparative examples and embodiment
Claims (6)
1. a kind of preparation method of electromagnetic field regulation self-healing seperation film, it is characterised in that the following steps are included:
(1) monomer dimethylaminoethyl methacrylate and methacrylic acid that molar ratio is 2:1~4:1 are mixed, in room temperature
Lower stirring 1~3 hour is added 0.05~2% crosslinking agent N, N '-methylene-bisacrylamide that dosage is monomer mass, stirs
It mixes 3~5 hours, then is 0.1~1% initiator K of monomer mass by dosage2S2O8Dissolution in deionized water, is then being stirred
It mixes down and is added dropwise in the mixed solution of aforementioned monomer and crosslinking agent；
(2) methacrylic acid and p-phenylenediamine that molar ratio is 1:1~3:1 are mixed into solution, it is equal that deionized water stirring is added
It is even, wherein deionized water is 8:1~12:1 with the volume ratio of methacrylic acid and p-phenylenediamine mixed solution, in high pressure hydro-thermal
It is sealed in reaction kettle, reacts 2~4 hours at 180~220 DEG C, then cooled to room temperature；
(3) polyvinyl alcohol is add to deionized water, is heated 1~3 hour at 90~100 DEG C, ultrasound 20~after forty minutes
The bubble in solution is removed, the polyvinyl alcohol water solution that concentration is 20~40wt% is obtained；
(4) the nano ferriferrous oxide particle water that the solution and concentration that prepare in step (1) (2) (3) are 2~5wt% is hanged
Supernatant liquid is mixed according to volume ratio 1:0.4~0.6:0.9~1.1:0.4~0.6, is stirred evenly；
(5) clean stainless steel mesh screen will be pre-processed to be immersed in immediately in the mixed solution of step (4), then adheres to surface
The mesh screen of viscosity solution steadily takes out, and is heat-treated 5~7 hours sample at 60~80 DEG C under nitrogen protection, is cooled to room temperature；
(6) sample of step (5) is freezed at -20~-16 DEG C 6~10 hours, thawed 10~14 hours at room temperature, repeat into
Row repeatedly, is prepared and can be realized the isolated multi-functional seperation film of self-healing of electromagnetic field regulation.
2. the preparation method of electromagnetic field regulation self-healing seperation film according to claim 1, it is characterised in that: step (1)
In, the molar ratio of the monomer dimethylaminoethyl methacrylate and methacrylic acid is 3:1, and the dosage of crosslinking agent is single
The 1% of weight, the initiator amount are the 0.5% of monomer mass.
3. the preparation method of electromagnetic field regulation self-healing seperation film according to claim 1, it is characterised in that: step (2)
In, the molar ratio of the methacrylic acid and p-phenylenediamine is that 2:1, the deionized water and methacrylic acid and p-phenylenediamine are mixed
The volume ratio for closing solution is 10:1.
4. the preparation method of electromagnetic field regulation self-healing seperation film according to claim 1, it is characterised in that: step (3)
In, the concentration of the polyvinyl alcohol water solution is 35wt%.
5. the preparation method of electromagnetic field regulation self-healing seperation film according to claim 1, it is characterised in that: step (4)
In, the concentration of the nano ferriferrous oxide particle suspension is 3wt%.
6. the preparation method of electromagnetic field regulation self-healing seperation film according to claim 1, it is characterised in that: step (4)
In, the volume ratio when solution and nano ferriferrous oxide particle water slurry prepared in step (1) (2) (3) mixes is 1:
0.5:1:0.5。
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