CN104772043A - Sodium alginate-graphite phase carbon nitride nano-sheet hybridized composite membrane as well as preparation and application of composite membrane - Google Patents
Sodium alginate-graphite phase carbon nitride nano-sheet hybridized composite membrane as well as preparation and application of composite membrane Download PDFInfo
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Abstract
The invention relates to a sodium alginate-graphite phase carbon nitride nano-sheet hybridized composite membrane. The composite membrane is prepared by the steps of firstly, with melamine as the raw material, preparing ultrathin and porous graphite phase carbon nitride nano-sheet by using a hot separation and liquid-phase separation combined method; blending the nano-sheet and sodium alginate to obtain a casting membrane liquid; defoaming, then preparing the membrane by using a spin-coating method; performing cross-linking with a calcium chloride solution; and finally drying to obtain the sodium alginate-graphite phase carbon nitride nano-sheet hybridized composite membrane. According to the hybridized composite membrane, by virtue of the structure characteristic that the graphite phase carbon nitride nano-sheet is planar, ultrathin and porous, the thicknesses of separation layers are reduced; an orderly transmission channel is built; the transmission resistance of water molecule is lowered; the ethyl alcohol molecule is prevented from transmitting; therefore the osmosis and the selectivity of the membrane are improved simultaneously. According to the hybridized composite membrane, the preparation process is simple, raw materials are easily available and the structure is controllable, and the composite membrane is used for ethyl alcohol/water mixture separation, and has relative high osmosis flux and separation coefficient.
Description
Technical field
The present invention relates to a kind of UF membrane field, particularly relate to a kind of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film and Synthesis and applications.
Background technology
The energy and environment are the 21 century global significant challenge faced, and alcohol fuel is subject to extensive concern as the reproducible clean energy resource of one.Ethanol/water mixture is azeotropic system, and traditional rectificating method is difficult to the efficient separation realized between component, and therefore fuel alcohol dewatering becomes the key technology of fuel ethanol production.As a kind of new separation technology, pervaporation technology utilizes physics chemical action different between each component of feed liquid and membrane material to realize being separated, do not limit by VLE, have easy and simple to handle, environmental friendliness, energy consumption are low, product purity advantages of higher, the separation for azeotropic system shows outstanding advantage.Membrane material is the core of pervaporation technology.For improving the application efficiency of process of pervaporation, membrane material should have high permeability and selective simultaneously.Take macromolecule as continuous phase, the inorganic filler macromolecular-inorganic hybrid membrane material that is decentralized photo owing to having the advantage of polymeric membrane and inoranic membrane concurrently, be expected to obtain higher permeability and selective simultaneously, become the forward position in osmotic evaporation film field.
There is following challenge in the design preparation of current hybridized film: the preparation of (1) small size filler.Membrane permeability and film thickness have approximate reverse proportionate relationship, are to improve the permeation flux of film, realize the ultrathin of film, need even, controlled to prepare small size filler; (2) preparation of porous fillers.On the one hand, the porosity of filler is higher, and permeable molecule diffusion rate is faster, and permeability of the membrane is higher.On the other hand, suitable pore size can hinder molecule that kinetic diameter is larger through, there is sieve effect, improve the selective of film.
Graphite phase carbon nitride is a kind Graphene profile material, be only by thickness that the monatomic lamella of 0.33nm is stacking to be formed, which floor by hot soarfing from means such as, liquid phase strippings, individual layer or ultra-thin graphite phase carbon nitride nanometer sheet can be obtained, the demand of osmotic evaporation film ultrathin can be met.Graphite phase carbon nitride nanometer sheet exists the micropore of a large amount of size uniformity, diameter is about 0.31nm, between hydrone (kinetic diameter is 0.26nm) and ethanol molecule (kinetic diameter is 0.45nm) size, hydrone can be allowed freely to pass through, hinder the transmission of ethanol molecule simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film and Synthesis and applications, hot soarfing is utilized to peel off from liquid phase the method combined, prepare ultra-thin porous graphite phase carbon nitride nanometer sheet, prepare hybridization film material by the physical blending of sodium alginate and graphite phase carbon nitride nanometer sheet, then be spun to support layer surface and prepare hybridization compounding film.Utilize the superthin structure of graphite phase carbon nitride nanometer sheet, can effectively reduce separating layer thickness, improve the permeation flux of film; Utilize the two-dimensional structure of graphite phase carbon nitride nanometer sheet, regular stratiform pattern can be formed in film, build orderly transmission channels; Utilize the loose structure of graphite phase carbon nitride nanometer sheet, hydrone can be reduced and transmit resistance, improve ethanol molecule and transmit resistance, improve permeability of the membrane and selective simultaneously.Hybridization compounding membrane material has following main feature: (1), by changing masking formula, can regulate and control membrane structure and physicochemical properties efficiently, neatly; (2) preparation process is simple, easily realizes ultrathin and the large-scale production of film.Can estimate, the membrane material that the method obtains has stronger stability and anti-Swelling Capacity.The membrane material that the method is obtained is used for the dehydration of ethanol/water mixed system pervaporation, there is higher permeation flux and separation factor.
A kind of sodium alginate provided by the invention-graphite phase carbon nitride nanometer sheet hybridization compounding film is using the polymer ultrafiltration membrane of porous as supporting layer, and sodium alginate-graphite phase carbon nitride nanometer sheet hybridized film is separating layer; The polymer ultrafiltration membrane of described porous is the one in polyacrylonitrile ultrafiltration film, polysulphone super-filter membrane, Sulfonated Polysulfone UF Membranes, poly (ether-sulfone) ultrafiltration membrane and polyimides milipore filter.The molecular cut off of the polymer ultrafiltration membrane of described porous is 100,000; The thickness of described sodium alginate-graphite phase carbon nitride nanometer sheet hybridized film is about 500nm.The preparation process of this hybridization compounding film is as follows:
Step one, sodium alginate added in deionized water and at 20-40 DEG C, stirs 1-2h, be mixed with the sodium alginate soln that mass concentration is 1-2%;
Step 2, in described sodium alginate soln, add graphite phase carbon nitride nanometer sheet, wherein, graphite phase carbon nitride nanometer sheet consumption is the 1-5wt.% of sodium alginate, pours in container at 20-40 DEG C after stirring 3-6h, room temperature leaves standstill 0.5-1h deaeration, obtains casting solution;
Step 3, described casting solution is spun to the surface of the polymer ultrafiltration membrane of porous, dry 24-72h under room temperature, obtains uncrosslinked sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film;
Step 4, described uncrosslinked sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film is immersed in the calcium chloride water of 0.5M, crosslinked 5-20min under room temperature, then rinse well with the calcium chloride solution of deionized water by film surface residual, dry 24-48h under room temperature, obtains sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film.
Further, the graphite phase carbon nitride nanometer sheet that step 2 adds take melamine as raw material, and concrete preparation process is: melamine is placed in crucible, puts into Muffle furnace roasting 3-5h at 500-600 DEG C, heating rate and rate of temperature fall all control at 2-5 DEG C/min, obtain yellow powder; After described yellow powder grinding, put into Muffle furnace roasting 1-3h at 500 DEG C, heating rate and rate of temperature fall all control at 3-8 DEG C/min, obtain graphite phase carbon nitride powder; Under room temperature, by described graphite phase carbon nitride powder dispersion in ionized water, make the dispersion liquid of 0.5-2mg/L, centrifugation after ultrasonic process 6-12h, vacuum drying at 30 DEG C, obtain graphite phase carbon nitride nanometer sheet.
Sodium alginate of the present invention-graphite phase carbon nitride nanometer sheet hybridization compounding film is used for the separation of ethanol/water mixture, permeation flux is 1915-2602g/m
2h, separation factor is 787-1653.
The invention has the advantages that: preparation process is easy to be controlled, and raw material is easy to get, mild condition.Obtained sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film, for the dehydration of ethanol/water mixture pervaporation, has higher separating property.
Accompanying drawing explanation
Fig. 1 is sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film high power SEM (SEM) cross-section photographs obtained in embodiment 3.
Fig. 2 is sodium alginate composite membrane high power SEM (SEM) cross-section photographs obtained in comparative example.
Detailed description of the invention
Below by concrete case study on implementation, specific description is done to the present invention.
A kind of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film that the present invention proposes is using the polymer ultrafiltration membrane of porous as supporting layer, and sodium alginate-graphite phase carbon nitride nanometer sheet hybridized film is separating layer; The molecular cut off of the polymer ultrafiltration membrane of described porous is 100,000, and the polymer ultrafiltration membrane of described porous can be the one in polyacrylonitrile ultrafiltration film, polysulphone super-filter membrane, Sulfonated Polysulfone UF Membranes, poly (ether-sulfone) ultrafiltration membrane and polyimides milipore filter; The thickness of described sodium alginate-graphite phase carbon nitride nanometer sheet hybridized film is about 500nm.
Embodiment 1, a kind of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film, its preparation process is as follows:
Step one, sodium alginate added in deionized water and at 30 DEG C, stirs 2h, be mixed with the sodium alginate soln that mass concentration is 1.5%, stand-by;
Step 2, be raw material with melamine, hot soarfing is utilized to peel off from liquid phase the method combined, preparation graphite phase carbon nitride nanometer sheet: 5g melamine is placed in crucible, puts into Muffle furnace roasting 4h at 550 DEG C, heating rate and rate of temperature fall all control at 3 DEG C/min, obtain yellow powder; With mortar by after described yellow powder grinding, put into Muffle furnace roasting 2h at 500 DEG C, heating rate and rate of temperature fall all control at 5 DEG C/min, obtain graphite phase carbon nitride powder; Under room temperature, by described graphite phase carbon nitride powder dispersion in ionized water, make the dispersion liquid of 1mg/L, centrifugation after ultrasonic process 6h, vacuum drying at 30 DEG C, obtain graphite phase carbon nitride nanometer sheet;
Step 3, in the obtained sodium alginate soln of step one, add the obtained graphite phase carbon nitride nanometer sheet of step 2, wherein, graphite phase carbon nitride nanometer sheet consumption is the 1wt.% of sodium alginate, pour into stir 4h at 30 DEG C after in container, room temperature leaves standstill 1h deaeration, obtains sodium alginate-graphite phase carbon nitride nanometer sheet casting solution;
Step 4, casting solution step 3 prepared are spun to the surface of the polyacrylonitrile ultrafiltration film of porous, dry 48h under room temperature, obtain uncrosslinked sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film;
Step 5, uncrosslinked sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film step 4 prepared immerse in the calcium chloride water of 0.5M, crosslinked 10min under room temperature, then rinse well with the calcium chloride solution of deionized water by film surface residual, dry 24h under room temperature, obtains sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film.
The sodium alginate prepared by embodiment 1-graphite phase carbon nitride nanometer sheet hybridization compounding film carries out the test of ethanol/water separating property.Adopt membrane separation plant, at 76 DEG C, in material liquid, ethanol/water mass ratio is carry out the test of ethanol/water separating property under the condition of 9:1, and permeation flux is 1915g/m
2h, separation factor is 787.
Embodiment 2, a kind of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film, its preparation process is substantially the same manner as Example 1, difference is only, in step 3, is changed graphite phase carbon nitride nanometer sheet consumption into account for sodium alginate 2wt.% by the 1wt.% accounting for sodium alginate.
The sodium alginate prepared by embodiment 2-graphite phase carbon nitride nanometer sheet hybridization compounding film carries out the test of ethanol/water separating property.Adopt membrane separation plant, at 76 DEG C, in material liquid, ethanol/water mass ratio is carry out the test of ethanol/water separating property under the condition of 9:1, and permeation flux is 2232g/m
2h, separation factor is 1254.
Embodiment 3, a kind of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film, its preparation process is substantially the same manner as Example 1, difference is only, in step 3, is changed graphite phase carbon nitride nanometer sheet consumption into account for sodium alginate 3wt.% by the 1wt.% accounting for sodium alginate.The high power SEM cross-section photographs of the sodium alginate finally obtained-graphite phase carbon nitride nanometer sheet hybridization compounding film as shown in Figure 1.
The sodium alginate prepared by embodiment 3-graphite phase carbon nitride nanometer sheet hybridization compounding film carries out the test of ethanol/water separating property.Adopt membrane separation plant, at 76 DEG C, in material liquid, ethanol/water mass ratio is carry out the test of ethanol/water separating property under the condition of 9:1, and permeation flux is 2469g/m
2h, separation factor is 1653.
Embodiment 4, a kind of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film, its preparation process is substantially the same manner as Example 1, difference is only, in step 3, is changed graphite phase carbon nitride nanometer sheet consumption into account for sodium alginate 4wt.% by the 1wt.% accounting for sodium alginate.
The sodium alginate prepared by embodiment 4-graphite phase carbon nitride nanometer sheet hybridization compounding film carries out the test of ethanol/water separating property.Adopt membrane separation plant, at 76 DEG C, in material liquid, ethanol/water mass ratio is carry out the test of ethanol/water separating property under the condition of 9:1, and permeation flux is 2250g/m
2h, separation factor is 1331.
Comparative example, a kind of sodium alginate hybridization compounding film, its preparation process is as follows:
Step one, sodium alginate added in deionized water and at 30 DEG C, stirs 2h, be mixed with the sodium alginate soln that concentration is 1.5wt.%.Then pour in container after continuing to stir 4h at 30 DEG C, room temperature leaves standstill 1h deaeration, obtains sodium alginate casting solution;
Step 2, casting solution step one prepared are spun to the surface of the polyacrylonitrile ultrafiltration film of porous, dry 48h under room temperature, obtain uncrosslinked sodium alginate composite membrane;
Step 3, uncrosslinked sodium alginate composite membrane step 2 prepared immerse in the calcium chloride water of 0.5M, crosslinked 10min under room temperature, then rinse well with the calcium chloride solution of deionized water by film surface residual, dry 24h under room temperature, obtain sodium alginate hybridization compounding film.The high power SEM cross-section photographs of the sodium alginate composite membrane finally obtained as shown in Figure 2.
The sodium alginate composite membrane prepared by comparative example carries out the test of ethanol/water separating property.Adopt membrane separation plant, at 76 DEG C, in material liquid, ethanol/water mass ratio is carry out the test of ethanol/water separating property under the condition of 9:1, and permeation flux is 1544g/m
2h, separation factor is 511.
To sum up, it is easy to be controlled that the present invention prepares sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding membrane process, and raw material is easy to get, mild condition, obtained sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film is used for the dehydration of ethanol/water mixture pervaporation, has higher separating property.The sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film properties of preparation in embodiment 3 is best, flux comparatively in comparative example sodium alginate composite membrane improve 59.9%, separation factor improves 223.5%.
Although invention has been described for composition graphs above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; when not departing from present inventive concept, can also make a lot of distortion, these all belong within protection of the present invention.
Claims (5)
1. sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film, is characterized in that: this hybridization compounding film is using the polymer ultrafiltration membrane of porous as supporting layer, sodium alginate-graphite phase carbon nitride nanometer sheet hybridized film is separating layer; The molecular cut off of the polymer ultrafiltration membrane of described porous is 100,000; The thickness of described sodium alginate-graphite phase carbon nitride nanometer sheet hybridized film is about 500nm.
2. sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film according to claim 1, is characterized in that: the polymer ultrafiltration membrane of described porous is the one in polyacrylonitrile ultrafiltration film, polysulphone super-filter membrane, Sulfonated Polysulfone UF Membranes, poly (ether-sulfone) ultrafiltration membrane and polyimides milipore filter.
3. a preparation method for sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film as claimed in claim 1, is characterized in that, comprise the following steps:
Step one, sodium alginate added in deionized water and at 20-40 DEG C, stirs 1-2h, be mixed with the sodium alginate soln that mass concentration is 1-2%;
Step 2, in described sodium alginate soln, add graphite phase carbon nitride nanometer sheet, wherein, graphite phase carbon nitride nanometer sheet consumption is the 1-5wt.% of sodium alginate, pours in container at 20-40 DEG C after stirring 3-6h, room temperature leaves standstill 0.5-1h deaeration, obtains casting solution;
Step 3, described casting solution is spun to the surface of the polymer ultrafiltration membrane of porous, dry 24-72h under room temperature, obtains uncrosslinked sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film;
Step 4, described uncrosslinked sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film is immersed in the calcium chloride water of 0.5M, crosslinked 5-20min under room temperature, then rinse well with the calcium chloride solution of deionized water by film surface residual, dry 24-48h under room temperature, obtains sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film.
4. the preparation method of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film according to claim 3, wherein, the graphite phase carbon nitride nanometer sheet that step 2 adds take melamine as raw material, prepares according to following step:
Step one, melamine is placed in crucible, put into Muffle furnace roasting 3-5h at 500-600 DEG C, heating rate and rate of temperature fall all control at 2-5 DEG C/min, obtain yellow powder;
Step 2, by after the grinding of described yellow powder, put into Muffle furnace roasting 1-3h at 500 DEG C, heating rate and rate of temperature fall all control at 3-8 DEG C/min, obtain graphite phase carbon nitride powder;
Under step 3, room temperature, by described graphite phase carbon nitride powder dispersion in ionized water, make the dispersion liquid of 0.5-2mg/L, centrifugation after ultrasonic process 6-12h, vacuum drying at 30 DEG C, obtain graphite phase carbon nitride nanometer sheet.
5. the application of sodium alginate-graphite phase carbon nitride nanometer sheet hybridization compounding film in the dehydration of ethanol/water mixture pervaporation as claimed in claim 1.
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