CN104548968A - Kevlar nanofiber composite forward osmosis membrane, and preparation method and application thereof - Google Patents
Kevlar nanofiber composite forward osmosis membrane, and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of membrane materials, and discloses a Kevlar nanofiber composite forward osmosis membrane, and a preparation method and application thereof. The preparation method comprises the following steps: stirring Kevlar fibers with an auxiliary agent, strong base and an organic solvent and dispersing to form a stable Kevlar nanofiber dispersion solution; adding a pore-foaming agent, and uniformly stirring to obtain a membrane casting solution; coating a glass plate with the membrane casting solution through blade coating to form a membrane, and soaking into a gel bath to form a gel membrane; soaking the gel membrane into an organic solution for solvent replacement to obtain a Kevlar nanofiber porous membrane; using the porous membrane as a substrate, diluting the Kevlar nanofiber dispersion solution, forming a membrane on the substrate through blade coating, soaking into the gel bath, taking out, and airing to obtain the Kevlar nanofiber composite forward osmosis membrane. The Kevlar nanofiber composite forward osmosis membrane has the advantages of high strength, high water flux and high salt intercepting rate, and is applicable to the field of water treatment.
Description
Technical field
The invention belongs to technology field of membrane materials, be specifically related to a kind of Kevlar nanofiber compound forward osmosis membrane and preparation method thereof and application.
Background technology
Positive phenomenon of osmosis is a kind of driving force utilizing the permeable pressure head of film both sides (instead of impressed pressure) to be used as water to be undertaken by film spreading, and impels the net migration of water throughout curve permeable membrane, can be used for from sewage extracting directly drinking water.Membrane separation technique is exactly do not need impressed pressure or run under very low impressed pressure relative to the most outstanding feature of the power-actuated membrane separation technique of external pressurized, and fouling membrane situation is relatively light, can operation for a long time and do not need cleaning, present the trend replacing pressure-driven membrane technology gradually in recent years.Membrane separation technique in the world such as Singapore of the U.S. Europe etc. countries and regions obtained large quantity research, make it at food, medicine, the energy, sewage is purified and field of seawater desalination, and there is application prospect very widely the aspects such as the hydration bag under drinking water lean condition used by army, emergency relief.Just permeating most popular film at present to be produced by HTI company of the U.S., primarily of porous support layer and surface compact layer composition.The multiplex Triafol T of surface compact layer of film or polyurethane synthesis, supporting layer is then polyester or polysulfones.But no matter which kind of is, in actual use, the corrosion resistance of film, the aspects such as water flux and salt rejection all need to be further improved.Therefore, need to find the needs that a kind of intensity is large, water flux is higher, the good film of salt rejection carrys out satisfied positive process of osmosis.
Kevlar fiber is a kind of high performance p-aramid fiber, and chemical name is poly terephthalic acid p-phenylenediamine (PPD), is usually abbreviated as PPTA, also can be described as aramid fiber-1414.It is developed in the sixties in last century by du pont company, achieves industrialization produce at the seventies.PPTA fiber is a kind of crystallization benzamide of cross-linked network, what form quite stable between amido link and phenyl ring grips structure altogether, molecule stretches vertically, the degree of orientation is high, intermolecular arrangements is regular, and there is very strong intermolecular hydrogen bonding, it is large that the feature of these molecular structures gives Kevlar fiber polarity, and intensity is high, modulus is high and the premium properties such as high temperature resistant, acid-fast alkali-proof corrosion.In view of these features of Kevlar fiber, it is obtained in the preparation of film with features such as high, the high water flux of intensity, good salt rejection and pays close attention to widely.
Using in current film-forming method is phase conversion method more widely, is also called L-S method, namely utilizes the solubility of polymer in different solvents to prepare film forming.But utilize at present in the technique of L-S legal system for PPTA film, need to use a large amount of concentrated sulfuric acids, easily cause the corrosion of machinery equipment, also easily occur danger, be unfavorable for suitability for industrialized production.In addition, the research also had shows, in NMP, form casting solution with the p-aramid fiber of the modification of synthesis, and recycling L-S legal system is for film forming.But a large amount of hydrophilic monomer adds the intensity that membership reduces p-aramid fiber in the synthesis of the modification p-aramid fiber in the method.
Summary of the invention
In order to solve the shortcoming and defect part of above prior art, primary and foremost purpose of the present invention is the preparation method providing a kind of Kevlar nanofiber compound forward osmosis membrane.
Another object of the present invention is to provide a kind of Kevlar nanofiber compound forward osmosis membrane prepared by said method.
Another object of the present invention is the application providing above-mentioned Kevlar nanofiber compound forward osmosis membrane.
The object of the invention is achieved through the following technical solutions:
A preparation method for Kevlar nanofiber compound forward osmosis membrane, comprises following operating procedure:
(1) Kevlar fiber is placed in container, adds auxiliary agent, highly basic and organic solvent, under room temperature, mechanical agitation dispersion, forms stable Kevlar nanofiber dispersion liquid solution;
(2) add pore-foaming agent in the solution formed to step (1), mechanical agitation evenly forms the casting solution of stable homogeneous afterwards;
(3) by the casting solution of step (2) certain thickness film of blade coating on cleaned glass plate, gel film forming in immersion precipitation bath subsequently;
(4) gel mould in step (3) is soaked removing pore-foaming agent after glass plate takes off in water, then solvent displacement is carried out in immersion in organic solution, dry under then taking out gel mould room temperature and obtain Kevlar nano fiber porous film;
(5) with the Kevlar nano fiber porous film formed in step (4) for substrate, by make in step (1) Kevlar nanofiber dispersion liquid solution dilution after in this substrate knifing, then soak in immersion precipitation bath, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
Organic solvent described in step (1) refers at least one in DMF and dimethyl sulfoxide (DMSO) (DMSO); Preferred dimethyl sulfoxide (DMSO).
Described auxiliary agent is methyl alcohol, and its consumption is 5% of organic solvent quality.
Described highly basic is at least one in potassium tert-butoxide or NaOH; Preferred potassium tert-butoxide; The addition of described highly basic is 50% of Kevlar fiber quality.
Described mechanical agitation dispersion refers to dispersed with stirring 2 days.
In described fiber dispersion liquid solution, the concentration of Kevlar fiber is 5wt%.
Pore-foaming agent described in step (2) comprises at least one in polyethylene glycol, lithium chloride and nano silicon; Being preferably number-average molecular weight is the polyethylene glycol of 600 ~ 2000; The consumption of described perforating agent is 20% ~ 50% of Kevlar fiber quality.
Described in step (3), the thickness of blade coating film forming is 300 ~ 500um; DMSO/ distilled water or distilled water that ethanol/distilled water that the composition preferred volume ratio of described coagulation bath is 50/50, volume ratio are 10/90; Be more preferably distilled water, to reduce the use of organic solvent.
In organic solution, soak the process of carrying out solvent displacement described in step (4) is: first in industrial alcohol, soak time is after 10h, then soaks 12h in n-hexane.
Dilution described in step (5) refers to that by the concentration dilution of Kevlar nanofiber dispersion liquid solution be 0.1% ~ 1%; The thickness of described knifing is 10 ~ 30 μm; Described coagulation bath refers to distilled water.
A kind of Kevlar nanofiber compound forward osmosis membrane, is prepared by above preparation method.
The application of above-mentioned Kevlar nanofiber compound forward osmosis membrane in water treatment field.
Had the following advantages and beneficial effect by preparation method of the present invention and the product tool that obtains:
(1) compound forward osmosis membrane of the present invention utilizes aramid fiber to prepare completely, the aramid fiber counterdie of porous and fine and close aramid fiber film are combined with each other and make forward osmosis membrane, gained forward osmosis membrane has the advantage that intensity is high, water flux large, salt rejection is good, in addition, the characteristic of the acid-alkali-corrosive-resisting of Kevlar own makes film have good solvent resistance, extends the application of film greatly;
(2) preparation method of forward osmosis membrane of the present invention compared with prior art, simple gentleness, avoid the use of the severe corrosive reagent such as the concentrated sulfuric acid, stable Kevlar nanofiber dispersion liquid solution can be obtained by the mode of organic solvent adding assistant, without the need to carrying out modification to Kevlar fiber, remain the performances such as its excellent high strength, high-modulus and solvent resistant;
(3) the present invention is simple to operate in preparation method, film-forming process is fast, the time is short, cost is low, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the front compacted zone structure of the Kevlar nanofiber forward osmosis membrane that the embodiment of the present invention 3 obtains;
Fig. 2 is the loose porous Rotating fields of reverse side of the Kevlar nanofiber forward osmosis membrane that the embodiment of the present invention 3 obtains.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 70.2L/m
2h, salt rejection is 99.1%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 158MPa.
Embodiment 2
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-1000 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 73.7L/m
2h, salt rejection is 98.9%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 149MPa.
Embodiment 3
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-2000 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 75.6L/m
2h, salt rejection is 98.1%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 145MPa.
The Facad structure of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains as shown in Figure 1; Its inverse layer structure as shown in Figure 2.As can be seen from Figure, Kevlar nanofiber compound forward osmosis membrane of the present invention has the loose porous structure of front densification, reverse side.
Embodiment 4
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 30% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 74.9L/m
2h, salt rejection is 98.5%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 138MPa.
Embodiment 5
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 50% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 76.0L/m
2h, salt rejection is 97.6%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 121MPa.
Embodiment 6
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 400um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 68.1L/m
2h, salt rejection is 99.3%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 162MPa.
Embodiment 7
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 500um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 67.0L/m
2h, salt rejection is 98.9%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 172MPa.
Embodiment 8
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.5%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 68.2L/m
2h, salt rejection is 99.2%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 160MPa.
Embodiment 9
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by step (2) casting solution, is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 1%wt, then knifing in substrate, film thickness is 10 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 66.2L/m
2h, salt rejection is 98.9%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 165MPa.
Embodiment 10
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 20 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 64.3L/m
2h, salt rejection is 99.3%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 165MPa.
Embodiment 11
The preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane of the present embodiment, concrete operation step is as follows:
(1) 2g Kevlar fiber (Dupont company provides) is placed in round-bottomed flask, add 2g auxiliary agent methyl alcohol, 1g potassium tert-butoxide and 40g organic solvent dimethyl sulfoxide (DMSO), under room temperature, mechanical agitation disperses 2 days, forms the dark red Kevlar nanofiber dispersion liquid solution of stable homogeneous;
(2) add the pore-foaming agent PEG-600 of Kevlar fiber quality 20% in the solution formed to step (1), mechanical agitation 5h makes it form the casting solution of stable homogeneous, and standing and defoaming 12h is stand-by;
(3) being sprawled on cleaned glass plate by the casting solution of step (2), is the film of 300um with blade applicator striking thickness, immerses gel film forming in distilled water coagulation bath;
(4) gel mould in step (3) is soaked one day after glass plate takes off distilled water, then in industrial alcohol, 10h is soaked, 12h is soaked again in n-hexane, carry out solvent displacement, then taking out gel mould is fixed on filter paper, dries and obtain Kevlar nano fiber porous film under room temperature;
(5) be that glass pane surface is fixed in substrate with the Kevlar nano fiber porous film formed in step (4), the Kevlar nanofiber dispersion liquid solution dimethyl sulfoxide (DMSO) made in step (1) being diluted to concentration is standing and defoaming after 0.1%wt, then knifing in substrate, film thickness is 30 μm, immerse in distilled water coagulation bath after leaving standstill 10s in atmosphere and soak, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
The strainability test of the Kevlar nanofiber compound forward osmosis membrane that the present embodiment obtains: material liquid is distilled water, and drive liquid to be the sodium chloride solution of 1M, test under room temperature, the testing time is 1h, and the water flux of gained film is 60.8L/m
2h, salt rejection is 99.5%.
The hot strength being recorded the Kevlar nanofiber compound forward osmosis membrane of the present embodiment by hot strength test (GBT1040.3-2006) is 170MPa.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a preparation method for Kevlar nanofiber compound forward osmosis membrane, is characterized in that: comprise following operating procedure:
(1) Kevlar fiber is placed in container, adds auxiliary agent, highly basic and organic solvent, under room temperature, mechanical agitation dispersion, forms stable Kevlar nanofiber dispersion liquid solution;
(2) add pore-foaming agent in the solution formed to step (1), mechanical agitation evenly forms the casting solution of stable homogeneous afterwards;
(3) by the casting solution of step (2) certain thickness film of blade coating on cleaned glass plate, gel film forming in immersion precipitation bath subsequently;
(4) gel mould in step (3) is soaked removing pore-foaming agent after glass plate takes off in water, then solvent displacement is carried out in immersion in organic solution, dry under then taking out gel mould room temperature and obtain Kevlar nano fiber porous film;
(5) with the Kevlar nano fiber porous film formed in step (4) for substrate, by make in step (1) Kevlar nanofiber dispersion liquid solution dilution after in this substrate knifing, then soak in immersion precipitation bath, dry after taking-up, obtain Kevlar nanofiber compound forward osmosis membrane.
2. the preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane according to claim 1, is characterized in that: the organic solvent described in step (1) refers to DMF or dimethyl sulfoxide (DMSO); Described auxiliary agent is methyl alcohol; Described highly basic comprises at least one in NaOH and potassium tert-butoxide.
3. the preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane according to claim 1, is characterized in that: described in step (1), the consumption of auxiliary agent is 5% of organic solvent quality; The consumption of described highly basic is 50% of fiber quality; In described fiber dispersion liquid solution, the concentration of Kevlar fiber is 5wt%.
4. the preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane according to claim 1, it is characterized in that: the pore-foaming agent described in step (2) comprises at least one in polyethylene glycol, lithium chloride and nano silicon, the consumption of described pore-foaming agent is 20% ~ 50% of Kevlar fiber quality.
5. the preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane according to claim 4, is characterized in that: described polyethylene glycol refers at least one in PEG-600, PEG-1000 and PEG-2000.
6. the preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane according to claim 1, is characterized in that: described in step (3), the thickness of blade coating film forming is 300 ~ 500um; Described coagulation bath consist of volume ratio be 50/50 ethanol/distilled water, volume ratio be 10/90 DMSO/ distilled water or distilled water.
7. the preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane according to claim 1, is characterized in that: described in step (3), coagulation bath consists of distilled water; The process of carrying out solvent displacement of soaking in organic solution described in step (4) is: first in industrial alcohol, soak time is after 10h, then soaks 12h in n-hexane.
8. the preparation method of a kind of Kevlar nanofiber compound forward osmosis membrane according to claim 1, is characterized in that: the dilution described in step (5) refers to the dilution of Kevlar nanofiber dispersion liquid solution as mass concentration is the solution of 0.1% ~ 1%; The thickness of described knifing is 10 ~ 30 μm; Described coagulation bath is distilled water.
9. a Kevlar nanofiber compound forward osmosis membrane, is characterized in that: described forward osmosis membrane is prepared by the method described in any one of claim 1 ~ 8.
10. the application of Kevlar nanofiber compound forward osmosis membrane according to claim 9 in water treatment field.
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