CN108525533A - A kind of preparation method of graphene high molecular polymer composite nanometer filtering film - Google Patents
A kind of preparation method of graphene high molecular polymer composite nanometer filtering film Download PDFInfo
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- CN108525533A CN108525533A CN201810310253.7A CN201810310253A CN108525533A CN 108525533 A CN108525533 A CN 108525533A CN 201810310253 A CN201810310253 A CN 201810310253A CN 108525533 A CN108525533 A CN 108525533A
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- 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
- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
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- 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
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- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/02—Inorganic material
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
- B01D2325/12—Adsorbents being present on the surface of the membranes or in the pores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/36—Hydrophilic membranes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses a kind of preparation methods of graphene high molecular polymer composite nanometer filtering film,Using ultrafiltration membrane as basement membrane,The cationic polyacrylamide and graphene solution blended liquid of one layer of 0.3~0.5mm thickness are applied on basement membrane using solution coating process,It is placed in 60~80 DEG C of baking oven and is crosslinked 0.5 3h,It is prepared for graphene high molecular polymer composite nanometer filtering film,It is with excellent adsorptivity,Low Temperature Far Infrared,It is antibacterial,The functions such as uvioresistant,There is high molecular polymer cation polypropylene acyl filtering to promote to make,Clarification purification and sedimentation facilitation,It can promote the purification of NF membrane,The ability of filtering,By the way that cationic polyacrylamide is added,Quaternary ammonium salt cationic group is introduced in nanofiltration film surface,Increase the hydrophily and selectivity of diaphragm,Graphene and high molecular polymer is added,Manufactured graphene high molecular polymer composite nanometer filtering film is significantly increased on film properties,There is preferable Selective Separation ability,The rejection of rejection and NaCl to Na2SO4 is significantly increased.
Description
Technical field
The present invention relates to a kind of composite nanometer filtering films, and in particular to a kind of system of graphene high molecular polymer composite nanometer filtering film
Preparation Method.
Background technology
Nanofiltration is a kind of novel membrane separation technique, and between reverse osmosis between ultrafiltration, aperture is in nano-scale range, one
As be 0.5-2.0nm.The preparation method of NF membrane mainly has composite algorithm, phase inversion, lotus electrochemical process and blending method etc. at present,
Middle composite algorithm includes surface application methods and interfacial polymerization.Composite algorithm is to use most, most effective nanofiltration film preparation side at present
Method, and production commercialization NF membrane kind is most, the maximum method of yield.This method is multiple in ultrafiltration or micro-filtration membrane surface
Closing last layer has the ultrathin functional layer in nanoscale aperture.The advantages of composite membrane be can choose different materials produce basement membrane and
Composite layer makes their performance respectively reach optimization, and ideal selective penetrated property may be implemented in wherein ultrathin functional layer, support
Layer can reach best intensity and pressure tightness.Graphene was the Two-dimensional Carbon atomic crystal of monoatomic thickness, from quilt in 2004
Since it was found that, the wide of scientific circles has just been attracted with its unique chemical constitution and excellent electricity, optics, calorifics and mechanical performance
General concern.Graphene oxide had not only had the monolayer honeycomb shape hexaplanar structure of graphene, but also contained a large amount of functional groups,
Such as-OH ,-COOH ,-O-, C=O, therefore the compatibility etc. with good dispersibility, hydrophily and polymer.But it is existing
The graphene oxide composite nano filter membrane that some is prepared by composite algorithm, flux is low, salt-stopping rate is low, film properties and service efficiency compared with
It is low.
Invention content
The technical problem to be solved by the present invention is to overcome the existing graphene oxide prepared by composite algorithm compound receive
Filter membrane, flux is low, salt-stopping rate is low, film properties and the relatively low problem of service efficiency.
In order to solve the above technical problem, the present invention provides the following technical solutions：
The present invention provides a kind of graphene high molecular polymer composite nanometer filtering films, include the composition of following weight percent
Point：Cement 40~50%, sand 20~50%, flyash 3~10%, stalk fibre account for 0.5~1%, aggregate 3~5%, slag 3
~5%, silica flour 3~5%, calcium nitrite 2~5%, polyvinyl chloride 2~5%, foaming agent 1~3%, foam stabilizer 0.3~0.6%,
Its surplus is tap water.
As a preferred technical solution of the present invention, the preparation method is as follows：
Step 1：Configure nitration mixture, the concentrated sulfuric acid (98%): concentrated phosphoric acid (85%)=9: 1 is put into container；Weigh appropriate height
Potassium manganate；
Step 2：Appropriate graphite is taken, nitration mixture is slowly poured into along wall of cup in the container for fill graphite and is mixed；
Step 3：Above-mentioned mixed reactant is placed in the magnetic agitation oil bath pan for being previously heated to 50 DEG C, and is opened
Beginning is slowly added into potassium permanganate；
Step 4：After adding potassium permanganate, vessel port is closed, in case impurity etc. is fallen into container.Again by reaction system
It is heated 6 hours at 50 DEG C；
Step 5：Then, continue the hydrogen peroxide after dilution is added into mixture for 50 DEG C of heating stirrings, add
The standard of how many hydrogen peroxide is：Solution colour becomes purplish finally to glassy yellow by black, is until no longer generating bubble
Only；
Step 6：Again by after the reaction system of step 5 50 DEG C of continuation heating stirring 3 hours, it is cooled to room temperature, waits centrifuging
Carrying out washing treatment；
Step 7：The product reacted by step 6 is diluted with water, and is then centrifuged every time three to five minutes with 9000rpm,
Only just with water centrifugation, last pH is approximately equal to 6；
Step 8：During centrifuge washing and to after having washed five times, centrifugation is all very sticky, will finally obtain
Centrifugation be placed in centrifuge tube and dried at 90 DEG C, dry obtained graphene powder；
Step 9：Graphene powder obtained in step 8 is carried out in ultra-pure water to ultrasonic disperse, and to obtain graphene molten
Liquid, addition ultra-pure water are diluted to a concentration of 0.2-500mg/L of graphene solution；
Step 10：Cationic polyacrylamide solution is added in the graphene solution that step 9 obtains and is sufficiently stirred altogether
It is mixed；
Step 11：Using ultrafiltration membrane as basement membrane, it is thick that one layer of 0.3~0.5mm is applied on basement membrane using solution coating process
The cationic polyacrylamide that step 10 obtains and graphene solution blended liquid, are placed in 60~80 DEG C of baking oven and are crosslinked 0.5-
3h；It is prepared for graphene high molecular polymer composite nanometer filtering film.
As a preferred technical solution of the present invention, the mixed proportion of potassium permanganate and nitration mixture is in the step 1
20ml∶1g。
As a preferred technical solution of the present invention, per 1g expansible graphite additions 55-70ml's in the step 2
Nitration mixture.
As a preferred technical solution of the present invention, the cationic polyacrylamide is 0.1%-0.5% solution.
In technical scheme of the present invention, cationic polyacrylamide is chain macromolecule compound, since it is with a variety of
Active group, water-soluble high molecular polymer.Due to containing a certain number of polar groups in its strand, it can pass through
The solids that suspend in absorption water make to build bridge between particle or so that particle coacervation is formed big flocculate by charging neutrality.Institute
With it can accelerate the sedimentation of particle in suspension, have and obviously accelerate solution clarification, promote to filter equivalent pectin/polyvinyl alcohol
It is a kind of quite extensive high molecular weight water soluble polymer of purposes, it is nontoxic, there is unique strong cohesive property, flatness, resistance to
The characteristics such as oiliness, resistance to dissolubility, gas barrier performance, wearability, protecting colloid, and specially treated water resistance can be made it have,
Its aqueous solution has that good film forming, emulsion stability, transparency are high, adhesion strength is strong, moisture-proof is good.Graphene is monatomic
The Two-dimensional Carbon atomic crystal of thickness, since 2004 are found, just with its unique chemical constitution and excellent electricity, light
, calorifics and mechanical performance have attracted the extensive concern of scientific circles.Both the monolayer honeycomb shape hexagonal with graphene is flat for graphene
Face structure, and contain a large amount of functional groups, such as-OH ,-COOH ,-O-, C=O, therefore with good dispersed, hydrophilic
Property, with the compatibility etc. of polymer.Preferably divided in polar solvent (such as water, N,N-dimethylformamide) based on graphene
Property is dissipated, a kind of graphene composite nanometer filtering film of high-throughput, high salt-stopping rate is prepared by composite algorithm, to effectively improve the performance of film
And service efficiency, it is of great significance for the scale application of NF membrane.
The advantageous effect that is reached of the present invention is：In the preparation process of the NF membrane, by the way that graphene is added, with excellent
There is filtering to promote for the functions such as different adsorptivity, Low Temperature Far Infrared, antibacterial, uvioresistant, high molecular polymer cation polypropylene acyl
Into work, clarification purification and sedimentation facilitation, the ability of purification, the filtering of NF membrane can be promoted, it is cationic poly- by being added
Acrylamide introduces quaternary ammonium salt cationic group in nanofiltration film surface, increases the hydrophily and selectivity of diaphragm, graphite is added
Alkene and high molecular polymer, manufactured graphene high molecular polymer composite nanometer filtering film are significantly increased on film properties, have compared with
Good Selective Separation ability, the rejection of rejection and NaCl to Na2SO4 are significantly increased.
Specific implementation mode
Embodiment 1
The present invention provides a kind of graphene high molecular polymer composite nanometer filtering film, and preparation method is as follows：
Step 1：Configure nitration mixture, the concentrated sulfuric acid (98%): concentrated phosphoric acid (85%)=9: 1 is put into container；Weigh appropriate height
Potassium manganate；
Step 2：Appropriate graphite is taken, nitration mixture is slowly poured into along wall of cup in the container for fill graphite and is mixed；
Step 3：Above-mentioned mixed reactant is placed in the magnetic agitation oil bath pan for being previously heated to 50 DEG C, and is opened
Beginning is slowly added into potassium permanganate；
Step 4：After adding potassium permanganate, vessel port is closed, in case impurity etc. is fallen into container.Again by reaction system
It is heated 6 hours at 50 DEG C；
Step 5：Then, continue the hydrogen peroxide after dilution is added into mixture for 50 DEG C of heating stirrings, add
The standard of how many hydrogen peroxide is：Solution colour becomes purplish finally to glassy yellow by black, is until no longer generating bubble
Only；
Step 6：Again by after the reaction system of step 5 50 DEG C of continuation heating stirring 3 hours, it is cooled to room temperature, waits centrifuging
Carrying out washing treatment；
Step 7：The product reacted by step 6 is diluted with water, and is then centrifuged every time three to five minutes with 9000rpm,
Only just with water centrifugation, last pH is approximately equal to 6；
Step 8：During centrifuge washing and to after having washed five times, centrifugation is all very sticky, will finally obtain
Centrifugation be placed in centrifuge tube and dried at 90 DEG C, dry obtained graphene powder；
Step 9：Graphene powder obtained in step 8 is carried out in ultra-pure water to ultrasonic disperse, and to obtain graphene molten
Liquid, addition ultra-pure water are diluted to a concentration of 0.2-500mg/L of graphene solution；
Step 10：Cationic polyacrylamide solution is added in the graphene solution that step 9 obtains and is sufficiently stirred altogether
It is mixed；
Step 11：Using ultrafiltration membrane as basement membrane, it is thick that one layer of 0.3~0.5mm is applied on basement membrane using solution coating process
The cationic polyacrylamide that step 10 obtains and graphene solution blended liquid, are placed in 60~80 DEG C of baking oven and are crosslinked 0.5-
3h；It is prepared for graphene high molecular polymer composite nanometer filtering film.
The mixed proportion of potassium permanganate and nitration mixture is 20ml: 1g in step 1.
Per the nitration mixture of 1g expansible graphite additions 55-70ml in step 2.
Cationic polyacrylamide is 0.1%-0.5% solution.
Embodiment 2
The present invention provides a kind of graphene high molecular polymer composite nanometer filtering film, and preparation method is as follows：
Step 1：Configure nitration mixture, the concentrated sulfuric acid (98%): concentrated phosphoric acid (85%)=9: 1 is put into container；Weigh appropriate height
Potassium manganate；
Step 2：Appropriate graphite is taken, nitration mixture is slowly poured into along wall of cup in the container for fill graphite and is mixed；
Step 3：Above-mentioned mixed reactant is placed in the magnetic agitation oil bath pan for being previously heated to 50 DEG C, and is opened
Beginning is slowly added into potassium permanganate；
Step 4：After adding potassium permanganate, vessel port is closed, in case impurity etc. is fallen into container.Again by reaction system
It is heated 6 hours at 50 DEG C；
Step 5：Then, continue the hydrogen peroxide after dilution is added into mixture for 50 DEG C of heating stirrings, add
The standard of how many hydrogen peroxide is：Solution colour becomes purplish finally to glassy yellow by black, is until no longer generating bubble
Only；
Step 6：Again by after the reaction system of step 5 50 DEG C of continuation heating stirring 3 hours, it is cooled to room temperature, waits centrifuging
Carrying out washing treatment；
Step 7：The product reacted by step 6 is diluted with water, and is then centrifuged every time three to five minutes with 9000rpm,
Only just with water centrifugation, last pH is approximately equal to 6；
Step 8：During centrifuge washing and to after having washed five times, centrifugation is all very sticky, will finally obtain
Centrifugation be placed in centrifuge tube and dried at 90 DEG C, dry obtained graphene powder；
Step 9：Graphene powder obtained in step 8 is carried out in ultra-pure water to ultrasonic disperse, and to obtain graphene molten
Liquid, addition ultra-pure water are diluted to a concentration of 0.2-500mg/L of graphene solution；
Step 10：Cationic polyacrylamide solution is added in the graphene solution that step 9 obtains；
Step 11：Using ultrafiltration membrane as basement membrane, it is thick that one layer of 0.3~0.5mm is applied on basement membrane using solution coating process
Cationic polyacrylamide that step 10 obtains and graphene solution blended liquid, are prepared for that graphene high molecular polymer is compound to be received
Filter membrane.
The mixed proportion of potassium permanganate and nitration mixture is 20ml: 1g in step 1.
Per the nitration mixture of 1g expansible graphite additions 55-70ml in step 2.
Cationic polyacrylamide is 0.1%-0.5% solution.
Embodiment 3
The present invention provides a kind of graphene high molecular polymer composite nanometer filtering film, and preparation method is as follows：
Step 1：Configure nitration mixture, the concentrated sulfuric acid (98%): concentrated phosphoric acid (85%)=9: 1 is put into container；Weigh appropriate height
Potassium manganate；
Step 2：Appropriate graphite is taken, nitration mixture is slowly poured into along wall of cup in the container for fill graphite and is mixed；
Step 3：Above-mentioned mixed reactant is placed in the magnetic agitation oil bath pan for being previously heated to 50 DEG C, and is opened
Beginning is slowly added into potassium permanganate；
Step 4：After adding potassium permanganate, vessel port is closed, in case impurity etc. is fallen into container.Again by reaction system
It is heated 6 hours at 50 DEG C；
Step 5：Then, continue the hydrogen peroxide after dilution is added into mixture for 50 DEG C of heating stirrings, add
The standard of how many hydrogen peroxide is：Solution colour becomes purplish finally to glassy yellow by black, is until no longer generating bubble
Only；
Step 6：Again by after the reaction system of step 5 50 DEG C of continuation heating stirring 3 hours, it is cooled to room temperature, waits centrifuging
Carrying out washing treatment；
Step 7：The product reacted by step 6 is diluted with water, and is then centrifuged every time three to five minutes with 9000rpm,
Only just with water centrifugation, last pH is approximately equal to 6；
Step 8：During centrifuge washing and to after having washed five times, centrifugation is all very sticky, will finally obtain
Centrifugation be placed in centrifuge tube and dried at 90 DEG C, dry obtained graphene powder；
Step 9：Graphene powder obtained in step 8 is carried out in ultra-pure water to ultrasonic disperse, and to obtain graphene molten
Liquid, addition ultra-pure water are diluted to a concentration of 0.2-500mg/L of graphene solution；
Step 10：Using ultrafiltration membrane as basement membrane, the step of one layer of 0.3~0.5mm thickness is applied on basement membrane using solution coating process
Rapid nine obtained graphene solutions, are placed in 60~80 DEG C of baking oven and are crosslinked 0.5-3h；It is prepared for graphene high molecular polymer
Composite nanometer filtering film.
Foaming agent is sodium sulfate of polyethenoxy ether of fatty alcohol.
Foam stabilizer is hydroxyethylmethylcellulose.
Cationic polyacrylamide is 0.1%-0.5% solution.
Graphene high molecular polymer composite nanometer filtering film made from embodiment 1-3 is subjected to pure water flux, initial salt rejection rate
With initial permeate flux performance measurement, measurement result is in following table：
This kind of graphene high molecular polymer composite nanometer filtering film essential element contrast table
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (4)
1. a kind of graphene high molecular polymer composite nanometer filtering film, which is characterized in that preparation method is as follows：
Step 1：Configure nitration mixture, the concentrated sulfuric acid (98%): concentrated phosphoric acid (85%)=9: 1 is put into container；Weigh appropriate permanganic acid
Potassium；
Step 2：Appropriate graphite is taken, nitration mixture is slowly poured into along wall of cup in the container for fill graphite and is mixed；
Step 3：Above-mentioned mixed reactant is placed in the magnetic agitation oil bath pan for being previously heated to 50 DEG C, and is started slow
It is slow that potassium permanganate is added；
Step 4：After adding potassium permanganate, vessel port is closed, in case impurity etc. is fallen into container.Again by reaction system 50
It is heated 6 hours at DEG C；
Step 5：Then, continue the hydrogen peroxide after dilution is added into mixture for 50 DEG C of heating stirrings, add few
The standard of hydrogen peroxide is：Solution colour becomes purplish finally to glassy yellow, until no longer generating bubble by black；
Step 6：Again by after the reaction system of step 5 50 DEG C of continuation heating stirring 3 hours, it is cooled to room temperature, waits for centrifuge washing
Processing；
Step 7：The product reacted by step 6 is diluted with water, and is then centrifuged every time three to five minutes with 9000rpm, is only used
Water centrifuges just, and last pH is approximately equal to 6；
Step 8：During centrifuge washing and to after having washed five times, centrifugation is all very sticky, will finally obtain from
Heart precipitation is placed in centrifuge tube dries at 90 DEG C, dry obtained graphene powder；
Step 9：Graphene powder obtained in step 8 is subjected to ultrasonic disperse in ultra-pure water and obtains graphene solution, is added
Ultra-pure water is added to be diluted to a concentration of 0.2-500mg/L of graphene solution；
Step 10：Cationic polyacrylamide solution is added in the graphene solution that step 9 obtains and is sufficiently stirred blending；
Step 11：Using ultrafiltration membrane as basement membrane, the step of one layer of 0.3~0.5mm thickness is applied on basement membrane using solution coating process
Ten obtained cationic polyacrylamide and graphene solution blended liquid, are placed in 60~80 DEG C of baking oven and are crosslinked 0.5-3h；System
For graphene high molecular polymer composite nanometer filtering film.
2. a kind of preparation method of graphene high molecular polymer composite nanometer filtering film according to claim 1, feature exist
In the mixed proportion of potassium permanganate and nitration mixture is 20ml: 1g in the step 1.
3. a kind of preparation method of graphene high molecular polymer composite nanometer filtering film according to claim 1, feature exist
In per the nitration mixture of 1g expansible graphite additions 55-70ml in the step 2.
4. a kind of preparation method of graphene high molecular polymer composite nanometer filtering film according to claim 1, feature exist
In the cationic polyacrylamide is 0.1%-0.5% solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110157069A (en) * | 2019-04-16 | 2019-08-23 | 常州华祥碳材料科技有限公司 | A kind of composite radiating grapheme material and manufacturing method |
| CN112206660A (en) * | 2020-09-16 | 2021-01-12 | 北创清源(北京)科技有限公司 | Enhanced anti-pollution low-cost ultrafiltration membrane and preparation method thereof |
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| CN104841291A (en) * | 2015-05-21 | 2015-08-19 | 南京工业大学 | Method for effectively enhancing dehydration performance of graphene oxide membrane |
| CN106076132A (en) * | 2016-06-27 | 2016-11-09 | 天津工业大学 | A kind of graphene oxide modified polyamide composite nanometer filtering film and preparation method thereof |
| CN106731868A (en) * | 2016-12-12 | 2017-05-31 | 苏州富艾姆工业设备有限公司 | A kind of processing technology of high-performance NF membrane |
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| CN104815608A (en) * | 2015-05-04 | 2015-08-05 | 哈尔滨工业大学 | Preparation method of multifunctional oil-water separation material based on graphene oxide nanobelt |
| CN104841291A (en) * | 2015-05-21 | 2015-08-19 | 南京工业大学 | Method for effectively enhancing dehydration performance of graphene oxide membrane |
| CN106076132A (en) * | 2016-06-27 | 2016-11-09 | 天津工业大学 | A kind of graphene oxide modified polyamide composite nanometer filtering film and preparation method thereof |
| CN106731868A (en) * | 2016-12-12 | 2017-05-31 | 苏州富艾姆工业设备有限公司 | A kind of processing technology of high-performance NF membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110157069A (en) * | 2019-04-16 | 2019-08-23 | 常州华祥碳材料科技有限公司 | A kind of composite radiating grapheme material and manufacturing method |
| CN112206660A (en) * | 2020-09-16 | 2021-01-12 | 北创清源(北京)科技有限公司 | Enhanced anti-pollution low-cost ultrafiltration membrane and preparation method thereof |
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