CN205951427U - Multilayer composite construction's film complex film - Google Patents
Multilayer composite construction's film complex film Download PDFInfo
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- CN205951427U CN205951427U CN201620402445.7U CN201620402445U CN205951427U CN 205951427 U CN205951427 U CN 205951427U CN 201620402445 U CN201620402445 U CN 201620402445U CN 205951427 U CN205951427 U CN 205951427U
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Abstract
The utility model belongs to the technical field of pellicle separation technology, relate to multilayer composite construction's film complex film. The film complex film is the transition layer that nanofiber is plain and polyelectrolyte forms through equipment method layer upon layer that coats in proper order in porous supporting layer basement, and then the polyamide selectivity thin layer of coating through the formation of general interfacial polymerization reaction method. Film complex film structure can be applied to and receive the preparation of filter membrane, reverse osmosis membrane and forward osmotic membrane. The utility model discloses a multilayer composite construction's film complex film uses and includes: running water purification, municipal water supply, sewage purification, brackish water desalination, seawater desalination, the concentrated technology of beverage fruit juice, dairy industry, blood dialysis medicine industry and semiconductor trade.
Description
Technical field
This utility model belongs to the technical field of semi-transparent membrane separation process, is related to the thin-film composite membrane of multi-layer compound structure.
Described Film laminated membrane structure can be applicable to the preparation of NF membrane, reverse osmosis membrane and forward osmosis membranes.
Background technology
Semi-transparent membrane separation technique refers to that the mixture of different-grain diameter molecule on a molecular scale is realized when by semipermeable membrane
The technology of Selective Separation, semipermeable membrane can be divided into according to pore size：Micro-filtration membrane, ultrafilter membrane, NF membrane, reverse osmosis membrane.From
Since nineteen twenty-seven Sartorius company of Germany issue first commercialization semipermeable membrane of the mankind, Immunohistochemistry is paid close attention to gradually
Improve development with continuous, be especially made for first high flux and Gao Tuo from the Lip river cloth sixties in 20th century and Suo Li lashing wire professor
After the asymmetric seperation film of cellulose acetate of salt rate, semipermeable membrane technology has even more obtained development at full speed.Market master at present
Stream reverse osmosis membrane and NF membrane be all based on a kind of by Cadotte and Rozelle invention be called Film laminated membrane technology.Thin
Film composite membrane technology is using one layer of very thin dividing for film of coating in the porous support layer substrate playing mechanical support effect
The fine and close optional membrane's layer playing a decisive role from characteristic, so that film has high flux and high salt-stopping rate simultaneously.And prepare
The method of this optional membrane's layer has：Interfacial polymerization, layer assembly method, chemical crosslink technique and ultraviolet grafting.In these sides
In method, interfacial polymerization have passed through nearly more than 30 years updating and becoming better and approaching perfection day by day, and has become as business reverse osmosis membrane and receives
The main flow production technology of the thin-film composite membranes such as filter membrane, its advantage is film forming thickness is thin, aperture is little, surface is uniform etc..But it is traditional
The maximum weak point of Film laminated membrane structure itself is that porosity is relatively low because porous support layer is dense, hinders water
By so that its maximum water flux is restricted.And due to fine and close optional membrane's layer directly contact supporting layer so that water
The passage that is especially horizontally oriented of passage hindered, reduce further water flux.In order to overcome this defect, can lead to
Cross and add one layer of ultra-thin three-dimensional netted transition zone being made up of nano-fiber material in the middle of supporting layer and optional membrane's layer, with
Increase porosity and introduce the especially horizontal aquaporin of more aquaporins, thus reaching the water flux improving thin-film composite membrane.
Such as patent WO2008118228A2 using method of electrostatic spinning supporting layer with optional membrane's layer inter-coat one layer by surpassing
The transition film that thin PAN fiber is constituted.The intercommunicating pore nanofiber of method of electrostatic spinning preparation has great specific surface area, simultaneously
Form the secondary structures such as much small aperture or projection, therefore there is very strong adsorptivity and good mechanical performance, make
The flux obtaining film is largely increased.But electrostatic spinning requires the high pressure of thousand of or even tens of thousands of volts, not only operating difficultiess, power consumption
High, yield poorly, and the film species that may be used on is very limited, and in addition the superfine fibre diameter made by electrostatic spinning all exceedes
300nm, significantly limit specific surface area and the film properties of fiber.
Content of the invention
The purpose of this utility model is to overcome above-mentioned technical disadvantages, providing a kind of new making with nano-cellulose film
The thin-film composite membrane with multi-layer compound structure for transition zone.
The thin-film composite membrane of multi-layer compound structure of the present utility model is a kind of thin-film composite membrane comprising three-decker, institute
The structure of the thin-film composite membrane stated as shown in figure 1, be followed successively by mechanical porous support layer substrate nano-cellulose transition zone and
Optional membrane's layer.It is characterized in that：Described nano-cellulose transition zone is to pass through layer by layer nano-cellulose with polyelectrolyte
The method of assembling plated film is coated in form the three-dimensional netted transition zone with superelevation porosity on porous support layer, and its thickness is
0.005 to 0.1 μm；Described porous support layer aperture can be made up of any appropriate polymer less than 100,000 molecular weight, for example,
Support layer can be made up of separated polymer.Separated polymer is a kind of polymerization that can form perforated membrane in phase separation
Thing, described phase separation includes thermally induced phase separation, phase separation method and evaporation and causes phase separation method.It is separated
The example of polymer include but is not limited to polyether sulfone, polrvinyl chloride, polyvinylidene fluoride, polypropylene, polyacrylonitrile, polyamide,
Polyimides, polyarylsulfone (PAS), Polyphenylene Sulfone, polyphenylene oxide, PPSS, cellulose acetate fat, nylon and combinations thereof.Described supporting layer
Form can be：Thin film, doughnut, tubulose, its tranverse sectional thickness is 80 to 2000 μm.Described optional membrane's layer is thin
The top of film composite membrane, plays the detached effect of selection, by General Purpose Interface polyreaction method in described nanofiber transition zone table
Form the polyamide optional membrane retention layer that ultrathin is 0.02 to 1 μm above face.
A diameter of 3 to the 30nm of described nano-cellulose, length is 0.2 to 10 μm, and it is constitute cellulose fibre basic
One of component, can by cellulosic material through TEMPO (phenmethylol conversion thewire) oxidation pre-treatment method or cellulase in advance
Logos to obtain described nano-cellulose through high speed shear homogenize process after processing.Gained nano-cellulose has acetic acid sense
Group and negatively charged or positively charged after modified.The nano-cellulose film that the charging property of nano-cellulose does not affect to be made up of it
Tridimensional network.
Described nano-cellulose film transition zone is to be coated in porous support layer substrate by the method for layer assembly, bag
Include following steps：
(1) nano-cellulose of 0.1 to 20mg/mL concentration is prepared with deionized water, and heavy through high speed centrifugation washing removal
Transparent nanofiber element suspension is obtained after the insoluble fiber cellulose aggregate forming sediment；
(2) it is also referred to as polyelectrolyte from the electropolymer with nano-cellulose oppositely charged, and joined with deionized water
The solution of system 0.02 to 10mg/mL concentration, and add NaCl or KCl or CaCl of 0.01 to 1 molar concentration2Deng inorganic salt, institute
State polyelectrolyte to be selected from according to required charging property with the polyelectrolyte in the following group：Polyethyleneimine, poly- diethyl allyl ammonium chloride,
Poly diallyldimethylammonium chloride, polyvinylamine, polyvinyl benzyl trimethyl ammonium chloride, shitosan, sulfonated polystyrene, poly- first
Base acrylic acid, sodium polyacrylate, polyvinyl alcohol, sodium apolate and their mixture；
(3) the film surface of porous support membrane substrate is soaked 3 to 30 minutes in nano-cellulose suspension, make Nanowire
Dimension element is reacted by the active forces such as electrostatic force, hydrogen bond force, hydrophobic force and basement membrane surface, forms the poly- of single layer nanometer structure
Electrolyte complex film；
(4) deionized water rinses out the redundant solution of polyelectrolyte composite film surface；
(5) continue for this basement membrane above-mentioned to soak 3 to 30 minutes in the solution that (2) step is configured so that being dissolved in
The polyelectrolyte of this solution and the polyelectrolyte composite membrane coated by step (3) are again by electrostatic force, hydrogen bond force, hydrophobic force etc.
Active force forms a new strata electrolyte complex film；
(6) deionized water rinses out the redundant solution of polyelectrolyte composite film surface；
(7) step of repetition (3) to (6) 1-20 time, makes the nano-cellulose of oppositely charged and selected polyelectrolyte exist
Basement membrane surface Layer-by-layer assembly, forms and has nano-cellulose and 1 to 20 double-layer nanometer of polyelectrolyte co-assemble
The nano-cellulose transition zone of structure；
(8) as needed, can first carry out step (5) and step (6) before the first step step (3) once, make final institute
Prepared nano-cellulose transition zone can active force and basement membrane surface between higher；
(9) as needed, step (3) and step (4) can also be repeated after step (7) final step step once,
Make finally made nano-cellulose transition zone outermost layer institute electrically charged electrically charged identical with nano-cellulose institute；
The superiors' optional membrane's layer of described sandwich diaphragm structure is by many officials using General Purpose Interface polyreaction method
Energy amine and multifunctional carboxylic acid halides carry out the polyamide film of chemical crosslink reaction generation, comprise the following steps that：
(1) the film surface of nano-cellulose transition zone is impregnated 0.5 to 5 minute in the aqueous solution kind of polyfunctional amine, and
Take out from solution, remove membrane removal excess surface drop；
(2) the nano-cellulose transition membrane surface after dipped polyfunctional amine aqueous solution is immersed the water of multifunctional carboxylic acid halides
0.1 to 10 minute in insoluble solution；
(3) scrape excess surface drop after film being taken out from the water-insoluble solution of multifunctional carboxylic acid halides, be placed in vacuum drying oven
Carry out heat treatment, the temperature of adjustment heat treatment is 40 to 80 DEG C, the time of heat treatment is 20 to 60 minutes, occurs interfacial polymerization anti-
Should rear synthesizing polyamides thin film；
(4) property entered Chemical cleaning removes residue and finally gives polyamide optional membrane's layer after being dried.
This utility model carries out performance test to the thin-film composite membrane of preparation：Be 225ppm sodium-chloride water solution with concentration Lai
Measure salt-stopping rate (R), operating pressure is 225psi, 25 DEG C of temperature, salt-stopping rate (R) and water flux (J) are calculated as follows respectively：
Wherein, CpAnd CfIt is respectively the electrolyte concentration in feeding liquid and permeate, change concentration and pass through to measure electrical conductivity of solution
To quantify, V is the permeate volume in the range of minute t by effective membrane area A.
Compared with the prior art the thin-film composite membrane of multi-layer compound structure described in the utility model, has following notable spy
Point：
1. with the tradition that interface polymerization reaction generation polyamide film is directly directly carried out on porous support layer substrate
The small throughput of polyamide film composite membrane is compared, and this utility model passes through in the middle of porous support layer substrate and polyamide film
One layer of interpolation three-dimensional netted transition zone through the high porosity of layer assembly with polyelectrolyte by nano-cellulose, to increase
The especially horizontal nanoscale aquaporin of the aquaporin of composite membrane, thus considerably increase the water flux of composite membrane, to Film laminated
Film expands application, reduction film plays progradations using power consumption.
2. compared with existing technology (for example patent WO2008118228A2 adopts the transition film of electrostatic spinning synthesis), originally
The nano-cellulose film of the layer assembly method synthesis that utility model is adopted, due to less (the 5nm relative patent of diameter
More than 300nm in WO2008118228A2), therefore specific surface area is bigger, advantageously forms more aquaporins.
The layer assembly method that this utility model is adopted is relative to prior art (such as method of electrostatic spinning), equipment requirements letter
Single, low cost, and toxic organic solvents, environmental friendliness need not be adopted, suitable heavy industrialization continuously produces.
Brief description
Fig. 1 is the structural representation of thin-film composite membrane described in the utility model.
Specific embodiment
Comparative example 1
The porous polysulfone supporting layer substrate including 200 μ m-thick of backing non-woven fabrics is directly carried out interface according to following steps
The step that polyreaction generates polyamide optional membrane's layer is as follows：
(1) by porous polysulfone supporting layer basement membrane surface in the aqueous solution kind containing 2% m-diaminobenzene. (MPD) polyfunctional amine
Dipping, after 0.5 minute, takes out from solution, removes membrane removal excess surface drop；
(2) will be multifunctional containing 0.1% pyromellitic trimethylsilyl chloride for the basement membrane surface immersion after dipped polyfunctional amine aqueous solution
10 seconds in the hexane solution of carboxylic acid halides；
(3) scrape excess surface drop after film being taken out from the water-insoluble solution of multifunctional carboxylic acid halides, be placed in vacuum drying oven
Carry out heat treatment, the temperature of adjustment heat treatment is 40 DEG C, the time of heat treatment is 20 minutes, synthesizes after there is interface polymerization reaction
Polyamide film；
(4) property entered Chemical cleaning removes residue and finally gives polyamide optional membrane's layer after being dried.
After tested, the salt-stopping rate of gained composite membrane is 98.3%, and pure water flux is 2.1L/m2·h·bar.
Embodiment 1
The porous polysulfone supporting layer substrate including 200 μ m-thick of backing non-woven fabrics is carried out nanofiber according to following steps
The coating of plain transition zone：
(1) acetic acid nano-cellulose sodium is prepared with TEMPO method：Over dry (never-dried) softwood chemical pulp by 20g
Fiber is placed in trough-style pulp beater and adds the water of 1500g, after discongesting 40min, adds the TEMPO of 0.25g, the NaBr of 2.5g with
And the NaClO solution that the mass percentage concentration of 5mL is 12%, stir and fully reacted, centre adds 0.5 molar concentration frequently
Sodium hydroxide solution and the hydrochloric acid solution of 0.5 molar concentration slurry pH is maintained 10.5, reaction was aoxidized after 24 hours
Fiber obtains the oxidized fibre that carboxyl-content is 0.30mmol/g with waste water after separating；Gained oxidized fibre is utilized high pressure homogenize
Machine carries out nanorize and processes the acetic acid nano-cellulose sodium oleo stock solution obtaining transparent and homogeneous；
(2) step (1) gained acetic acid nano-cellulose sodium oleo stock solution is dense to add deionized water preparation 0.1mg/mL
The acetic acid nano-cellulose sodium solution of degree, and obtain transparent after the insoluble fiber cellulose aggregate that high speed centrifugation washing removes precipitation
Acetic acid nano-cellulose sodium suspension；
(3) prepare the chitosan solution of 0.05mg/mL concentration with deionized water, and add the NaCl of 1 molar concentration, will be molten
The liquid pH acetic acid of 4% concentration is adjusted to 6 so that chitosan solution positively charged；
(4) the film surface of porous polysulfones support membrane substrate is soaked 5 minutes in acetic acid nano-cellulose sodium suspension, make
Nano-cellulose is reacted by the active forces such as electrostatic force, hydrogen bond force, hydrophobic force and basement membrane surface, forms monolayer nano junction
The polyelectrolyte composite membrane of structure；
(5) deionized water rinses out the redundant solution on film surface；
(6) continue to soak 5 minutes this basement membrane above-mentioned in the solution that (3) step is configured so as to be dissolved in this molten
The polyelectrolyte of liquid is acted on again by electrostatic force, hydrogen bond force, hydrophobic force etc. with the polyelectrolyte composite membrane coated by step (4)
Power forms a new strata electrolyte complex film；
(7) deionized water rinses out the redundant solution of polyelectrolyte composite film surface；
(8) step 1 time repeating (4) to (7) obtains 2 double-layer nanostructured nano-cellulose transition zones；
Then interface polymerization reaction method polyamide coating is begun through on above-mentioned made nano-cellulose transition zone select
Property thin layer, step is as follows：
(9) by the film surface of nano-cellulose transition zone in the aqueous solution kind containing 2% m-diaminobenzene. (MPD) polyfunctional amine
Dipping, after 0.5 minute, takes out from solution, removes membrane removal excess surface drop；
(10) the nano-cellulose transition membrane surface immersion after dipped polyfunctional amine aqueous solution is contained 0.1% equal benzene three
10 seconds in the hexane solution of formyl chloride multifunctional carboxylic acid halides；
(11) scrape excess surface drop after film being taken out from the water-insoluble solution of multifunctional carboxylic acid halides, be placed in vacuum drying oven
Carry out heat treatment, the temperature of adjustment heat treatment is 40 DEG C, the time of heat treatment is 20 minutes, synthesizes after there is interface polymerization reaction
Polyamide film；
(12) property entered Chemical cleaning removes residue and finally gives polyamide optional membrane's layer after being dried.
After tested, the salt-stopping rate of gained composite membrane is 98.6%, and pure water flux is 2.5L/m2·h·bar.
Embodiment 2
Essentially identical with the process described in embodiment 1, but the number of repetition of the inner step to (4) to (7) of step (8) is 5
Secondary obtain 6 double-layer nanostructured nano-cellulose transition zones, other parameters are constant.After tested, section salt of gained composite membrane
Rate is 98.8%, and pure water flux is 3.1L/m2·h·bar.
Embodiment 3
Essentially identical with the process described in embodiment 1, but the number of repetition of the inner step to (4) to (7) of step (8) is 20
Secondary obtain 21 double-layer nanostructured nano-cellulose transition zones, other parameters are constant.After tested, section salt of gained composite membrane
Rate is 99.2%, and pure water flux is 3.0L/m2·h·bar.
Embodiment 4
Essentially identical with the process described in embodiment 1, but the number of repetition of the inner step to (4) to (7) of step (8) is 10
Secondary obtain 11 double-layer nanostructured nano-cellulose transition zones, and the NaCl concentration being added in step (3) is changed into
0.01 molar concentration, other parameters are constant.After tested, the salt-stopping rate of gained composite membrane is 98.1%, and pure water flux is 2.4L/
m2·h·bar.
Embodiment 5
Essentially identical with the process described in embodiment 1, but the number of repetition of the inner step to (4) to (7) of step (8) is 10
Secondary obtain 11 double-layer nanostructured nano-cellulose transition zones, and the polyelectrolyte in step (3) is transformed to polyethylene
Imines, and the concentration of polyelectrolyte increases as 10mg/mL, and other parameters are constant.After tested, the salt-stopping rate of gained composite membrane is
98.4%, pure water flux is 2.8L/m2·h·bar.
Embodiment 6
Essentially identical with the process described in embodiment 2, but before first step (4) starts, first carry out a step (6)
Obtain 6.5 double-layer nanostructured nano-cellulose transition zones with step (7), other parameters are constant.After tested, gained is combined
The salt-stopping rate of film is 98.6%, and pure water flux is 2.7L/m2·h·bar.
Embodiment 7
Essentially identical with the process described in embodiment 2, but after last step (8), then carry out a step (4)
Obtain 6.5 double-layer nanostructured nano-cellulose transition zones with step (5), other parameters are constant.After tested, gained is combined
The salt-stopping rate of film is 97.1%, and pure water flux is 3.3L/m2·h·bar.
The salt-stopping rate of embodiment 1 to 7 see table compared with comparative example with water flux.
Claims (4)
1. a kind of thin-film composite membrane of multi-layer compound structure is it is characterised in that include：
(1) porous support layer substrate；
(2) in porous support layer suprabasil nano-cellulose film transition zone；And
(3) through the polyamide optional membrane of General Purpose Interface polymerisation process synthesis on nano-cellulose film transition zone
Layer.
2. thin-film composite membrane as described in claim 1 is it is characterised in that described porous support layer substrate is by selected from the following group
In at least one be separated polymer make：Polyether sulfone, polrvinyl chloride, polyvinylidene fluoride, polypropylene, polyacrylonitrile, poly-
Amide.
3. thin-film composite membrane as described in claim 1 it is characterised in that described nano-cellulose film thickness be 3 to
1000nm.
4. thin-film composite membrane as described in claim 1 is it is characterised in that described nano-cellulose film transition zone is by nanometer
Cellulose and polyelectrolyte are through the nanostructured of layer assembly.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106823866A (en) * | 2017-03-01 | 2017-06-13 | 上海洁晟环保科技有限公司 | A kind of separating and filtering film and its preparation method and application |
| CN113731190A (en) * | 2021-07-20 | 2021-12-03 | 浙大宁波理工学院 | Nano-cellulose layered self-assembled film and preparation method thereof |
| CN113731190B (en) * | 2021-07-20 | 2024-06-25 | 浙大宁波理工学院 | Nanocellulose layer-by-layer self-assembled film and preparation method thereof |
-
2016
- 2016-05-05 CN CN201620402445.7U patent/CN205951427U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106823866A (en) * | 2017-03-01 | 2017-06-13 | 上海洁晟环保科技有限公司 | A kind of separating and filtering film and its preparation method and application |
| CN106823866B (en) * | 2017-03-01 | 2019-09-20 | 上海洁晟环保科技有限公司 | A kind of separating and filtering film and its preparation method and application |
| CN113731190A (en) * | 2021-07-20 | 2021-12-03 | 浙大宁波理工学院 | Nano-cellulose layered self-assembled film and preparation method thereof |
| CN113731190B (en) * | 2021-07-20 | 2024-06-25 | 浙大宁波理工学院 | Nanocellulose layer-by-layer self-assembled film and preparation method thereof |
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Effective date of registration: 20200318 Address after: 215000 Room 401, building 01, northwest area, Suzhou nano City, No. 99, Jinjihu Avenue, Suzhou Industrial Park, Jiangsu Province (nw-01 401) Patentee after: Suzhou Puxi Environmental Protection Technology Co., Ltd Address before: 350001 No.9 701, Qianlong Yujing, No.189, North fufei Road, Jin'an District, Fuzhou City, Fujian Province Patentee before: Lin Xiaofeng |