CN108404686A - A kind of preparation method of adsorption of metal ions sewage seperation film - Google Patents
A kind of preparation method of adsorption of metal ions sewage seperation film Download PDFInfo
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- CN108404686A CN108404686A CN201810426980.XA CN201810426980A CN108404686A CN 108404686 A CN108404686 A CN 108404686A CN 201810426980 A CN201810426980 A CN 201810426980A CN 108404686 A CN108404686 A CN 108404686A
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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
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D69/02—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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
- 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
- B01D2325/36—Hydrophilic membranes
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Abstract
The present invention relates to a kind of preparation methods of adsorption of metal ions sewage seperation film, this method is modified graphene oxide first with polyphenol compound, itself and Kynoar, perforating agent and organic solvent are configured to casting solution again, finally solution inversion of phases membrane formation process is used to make its film-forming.The present invention carries more hydrophily oxygen-containing functional group using graphene oxide and polyphenols, and the characteristic of chelatropic reaction can occur with metal ion, enable film adsorbing metal ions while detaching sewage.It is reusable by cleaning after absorption using adsorption of metal ions sewage seperation film made from this method, secondary pollution is avoided, while can be recycled to metal values.
Description
Technical field
The present invention relates to water process technical field of membrane, and in particular to a kind of preparation of adsorption of metal ions sewage seperation film
Method.
Background technology
Currently, the main method of harmless treatment metal ion waste water has membrane separation process, electrochemical deposition method, ion to hand over
Change method, absorption and biological treatment etc..Wherein, membrane separation technique has many advantages, such as compared to other techniques, such as selectively good,
Can be achieved the separation of molecular level other substance, can normal-temperature operation, change without phase-change, low energy consumption, expense be about concentrated by evaporation or freeze it is dense
The 1/3~1/8 of contracting.Therefore, membrane separation technique has broad application prospects in sewage treatment field.
Kynoar (PVDF) as a kind of good microfiltration membranes of comprehensive performance or ultrafiltration membrane material, have high temperature resistant,
The characteristics such as radiation hardness, wear-resisting, resistant to chemical etching, but pvdf membrane cannot be directly used to adsorption of metal ions.Blending is a kind of most simple
Single is also most common membrane modifying method, relative to other methods, blending and modifying have progress synchronous with film forming, it is simple for process not
Need cumbersome post-processing step, modifying agent that can cover film surface and fenestra inner wall, the destruction etc. that membrane structure will not be caused simultaneously
Advantage.
Graphene is continuously developed utilization because of its huge specific surface area in terms of absorption method is except impurity, and its derivative
Graphene oxide makes oxidation since plane and both sides of edges are there are the oxygen-containing polar group such as a large amount of hydroxyl, epoxy group and carboxyl
Graphene has stronger adsorption capacity to metal ion.However graphene oxide size is small, is used as adsorbent adsorbing metal ions
After be dispersed in water, be not easy the later stage removal, to bring secondary pollution of water.
Polyphenol compound, including tannin (Tannin, TA), dopamine (Dopamine, DA), pyrogallol
(Pyrogallol, PG), catechol, table roasted catechins etc. with metal ion containing can occur chelating and complexing faces a hydroxyl
Base has preferable adsorption effect to metal ion.In addition it can also be by oxidative coupling polymerization on graphene oxide, to oxygen
Graphite alkene is modified, and increases compound volume, referring specifically to Chinese patent CN104098860A, CN107638816A and
CN105944691A etc..
Based on this, the present invention is modified processing using polyphenol compounds such as tannin to graphene oxide first, later
With PVDF admixture of powder, a kind of adsorption of metal ions sewage seperation film has been made.Utilize a large amount of carboxyls, the phenol hydroxyl contained in the film
The oxygen-containing polar group such as base, epoxy group carries out efficient absorption and desorption to low-concentration metallic ion such as lead, copper etc.；Also with
The microcellular structure and hydrophilic functional groups of film itself have good barriering effect to bulky grain pollutant and oiliness pollutant.Due to
Interaction between graphene oxide and polyphenolic substance considerably increases the volume of compound so that it can in blend film
In be stabilized, will not be removed from blend film in absorption and filter process, thus can Reusability, while preventing oxidation
Secondary pollution of the graphene to water body.
Invention content
It is an object of the invention to overcome adsorbed film preparation process of the existing technology is complicated, performance is not good etc. enough to ask
Topic, provides a kind of preparation method of adsorption of metal ions sewage seperation film.Gold that can be in efficient absorption sewage using the seperation film
Belong to ion, while being filtered to remove the pollutants such as the large particulate matter in water body and colloid, the membrane material of adsorbing metal ions is through clear
After washing can high efficiente callback wherein metal values ion, seperation film may be reused.To achieve the above object, institute of the present invention
The technical solution of use is as follows：
A kind of preparation method of adsorption of metal ions sewage seperation film, includes the following steps：
(a) it by graphene oxide ultrasonic disperse in deionized water, adds polyphenol compound and stirs evenly, reacted
The graphene oxide of polyphenol modification is obtained at rear separation of solid and liquid；
(b) the graphene oxide ultrasonic disperse for being modified polyphenol adds Kynoar, drilling in organic solvent A
Agent is sufficiently stirred, and obtains casting solution；
(c) casting solution is poured over to scratch on tablet and is formed a film, then placed it in solution B and cure, finally take out through washing
It washs, dry, obtain adsorption of metal ions sewage seperation film.
In said program, the polyphenol compound is in tannin, dopamine, pyrogallol, catechol, table roasted catechins
One kind, the addition of polyphenol compound is 10-20 with graphene oxide mass ratio:1.
In said program, the Kynoar is powdered, and average molecular weight is 100,000-40 ten thousand.
In said program, the perforating agent is specially PVP K30.
In said program, the organic solvent A is selected from n,N-Dimethylformamide (DMF), n,N-dimethylacetamide
(DMAC), one kind in N-Methyl pyrrolidone (NMP).
In said program, the one kind of the solution B in water, ethyl alcohol, octanol.
In said program, the mass fraction for the graphene oxide that polyphenol is modified in casting solution is 1-2%, Kynoar
Mass fraction is 10%-15%, and the mass fraction of perforating agent is 0.5%-2%, and surplus is organic solvent A.
Further, the preparation method for the graphene oxide that polyphenol is modified is specific as follows：By graphene oxide ultrasonic disperse
In deionized water, it is heated to 30-60 DEG C and is stirred to react 8-16h, the membrane filtration for being then 0.1-0.5 μm with aperture, filter
Slag is washed, it is dry, grind to obtain the final product.
The method for preparing casting solution is specific as follows：By the graphene oxide ultrasonic disperse of polyphenol modification in organic solvent A,
The Kynoar and perforating agent dried in advance is added into dispersion liquid under protective atmosphere, is stirred to react 20-28h, it is last true
Empty de-bubble 4-8h to obtain the final product.
Compared with prior art, the present invention has following unexpected advantageous effect：
(1) use the method for polyphenol modified graphene oxide and polyvinylidene blending that adsorption of metal ions sewage has been made
Seperation film, wherein polyphenol modified graphene oxide are dispersed in plate membrane, both carry hydrophily oxygen-containing functional group, can
Chelation occurs with metal ion, makes film adsorbing metal ions while detaching sewage；
(2) bigger serface contained by graphene oxide, polyphenol compound and abundant oxygen-containing functional group are made full use of,
The complexing to metal ion is significantly improved, the seperation film is to the removal rate of low-concentration metallic ion up to 95% or more；
(3) polyphenol modified graphene oxide is stabilized in plate membrane in the seperation film, and adsorption treatment is carried out to sewage
By cleaning can Reusability, while can high efficiente callback wherein metal values ion；
(4) hydrophilic functional group for utilizing the microcellular structure of film and containing, can also be to oil while adsorbing metal ions
Contact scar object is detached；
(5) compared with CN107638816A, the application is first modified graphene oxide with polyphenol compound, increases its body
Product be allowed to be stabilized in the solution, when avoiding directly being blended adsorbent be detached from blend film, later again with polyvinylidene blending
And use solution phase inversion direct formation of film at surface.
Specific implementation mode
To make those of ordinary skill in the art fully understand technical scheme of the present invention and advantageous effect, below in conjunction with specific
Embodiment is further described.
Agents useful for same of the present invention is common commercially available.The adsorption efficiency of metal ion is measured with the following method：Pb used
(II) and Cu (II) solution is respectively by standard 100mg/L Pb (II) and Cu (II) storing solution dilution gained, then with NaOH and HCl
PH value of solution is adjusted to 5, with the metal ion solution of a concentration of 10mg/L of absorption membrane filtration 10mL obtained, is then with aperture
Clear liquid below 0.22 μm of filtering with microporous membrane, using the concentration of metal ion in Atomic Absorption Spectrometer filtrates tested, according to
Adsorption efficiency formula (1) is calculated.
In formula, E- adsorption of metal ions efficiency, C0Metal ion initial concentration, mg/L；It is dense after C- adsorption of metal ions
Degree, mg/L.
The present invention measures the adsorption capacity of metal ion with the following method：Adsorbed film made from certain mass is taken, by it
It is placed in conical flask, certain volume, the fixed metal ion solution of concentration is added, vibrates 12h in 30 DEG C of constant temperature oscillator,
Concentration of metal ions is tested using Atomic Absorption Spectrometer, is calculated according to adsorption capacity formula (2).
In formula, C0Metal ion initial concentration, mg/L；CeConcentration of metal ions when adsorption equilibrium, mg/L；VfMetal
Ion volume；W- dry film quality.
The present invention measures desorption rate with the following method：Adsorbed film after adsorption equilibrium is washed with deionized to filtrate
In do not contain metal ion, then mix with the hydrochloric acid solution of the 0.1M of certain volume, in constant temperature oscillator vibrate one periodically
Between, effects of ion concentration is measured, desorption rate is calculated according to formula (3).
In formula, η-desorption rate, the concentration of metal ion, mg/L in C- eluents；V- effluent volumes, L；Q- elutes cephacoria
The adsorption capacity of adsorbent, mg/g；The quality of m- adsorbed films.
The present invention measures rejection of the adsorbed film obtained to bovine serum albumin(BSA) (BSA) with the following method, to table
The separating effect to organic pollution is levied, detailed process is as follows：BSA powder is dissolved in PBS buffer solutions (pH=7.4) and is made into
The BSA solution of 200mg/L collects penetrating fluid with filtering membrane filtration BSA solution obtained.Utilize ultraviolet-visible spectrophotometer
The absorbance of penetrating fluid at 278nm is measured, rejection is calculated according to formula (4).
In formula, R- rejections；CpThe mass concentration of penetrating fluid BSA, mg/L；CfThe mass concentration of BSA, mg/ in material liquid
L。
Embodiment 1
First by 100mg graphene oxides ultrasonic disperse in 100mL deionized waters, 2g tannin is added, solution is heated
It is warming up to 50 DEG C and is stirred to react 12h, the membrane filtration in 0.2 μm of aperture of product, drying and grinding preserves after then cleaning, and obtains polyphenol
Modified graphene oxide (TA-GO).
By 2gTA-GO ultrasonic disperses in 84g DMF, in N212.5g dryings are slowly added under protection into dispersion liquid
Pretreated PVDF powder (average molecular weight 100,000-40 ten thousand) and 1.5g perforating agent PVP K30s, are stirred to react
Make casting solution uniform, stable for 24 hours, finally places it in deaeration 6h in vacuum drying chamber.
Casting solution obtained is poured on glass plate, the plate membrane that thickness is uniform, consistent is scraped with scraper, then by it
It is placed in film-forming in water coagulating bath.Multipass is cleaned with deionized water, preserve in deionized water or drying at room temperature ring after taking-up
In border.
Embodiment 2
First by 100mg graphene oxides ultrasonic disperse in 100mL deionized waters, 2g dopamines are added, by solution
50 DEG C of stirring 12h are heated to, the membrane filtration in 0.2 μm of aperture of product, drying and grinding preserves after then cleaning, and obtains DOPA
Amine modified graphene oxide (DA-GO).
By 1gDA-GO ultrasonic disperses in 84g DMF, in N213.5g dryings are slowly added under protection into dispersion liquid
Pretreated PVDF powder (average molecular weight 100,000-40 ten thousand) and 1.5g perforating agent PVP K30s, are stirred to react
Make casting solution uniform, stable for 24 hours, finally places it in deaeration 6h in vacuum drying chamber.
Casting solution obtained is poured on glass plate, the plate membrane that thickness is uniform, consistent is scraped with scraper, then by it
It is placed in film-forming in water coagulating bath.Multipass is cleaned with deionized water, preserve in deionized water or drying at room temperature ring after taking-up
In border.
Embodiment 3
First by 100mg graphene oxides ultrasonic disperse in 100mL deionized waters, 2g pyrogallols are added, by solution plus
Heat is warming up to 50 DEG C of stirring 12h, and the membrane filtration in 0.2 μm of aperture of product, drying and grinding preserves after then cleaning, and obtains pyrogallol
Modified graphene oxide (PG-GO).
By 1.5g PG-GO ultrasonic disperses in 84g DMF, in N213.5g is slowly added to through drying into dispersion liquid under protection
Pretreated PVDF powder (average molecular weight 100,000-40 ten thousand) and 1g perforating agent PVP K30s are done, is stirred to react
Make casting solution uniform, stable for 24 hours, finally places it in deaeration 6h in vacuum drying chamber.
Casting solution obtained is poured on glass plate, the plate membrane that thickness is uniform, consistent is scraped with scraper, then by it
It is placed in film-forming in water coagulating bath.Multipass is cleaned with deionized water, preserve in deionized water or drying at room temperature ring after taking-up
In border.
Embodiment 4
First by 100mg graphene oxides ultrasonic disperse in 100mL deionized waters, 2g pyrogallols are added, by solution plus
Heat is warming up to 50 DEG C of stirring 12h, and the membrane filtration in 0.2 μm of aperture of product, drying and grinding preserves after then cleaning, and obtains pyrogallol
Modified graphene oxide (PG-GO).
By 2g PG-GO ultrasonic disperses in 84g DMF, in N2It is pre- that 13g dryings are slowly added into dispersion liquid under protection
The PVDF powder (average molecular weight 100,000-40 ten thousand) and 1g perforating agent PVP K30s of processing, be stirred to react makes for 24 hours
Casting solution is uniform, stablizes, and finally places it in deaeration 6h in vacuum drying chamber.
Casting solution obtained is poured on glass plate, the plate membrane that thickness is uniform, consistent is scraped with scraper, then by it
It is placed in film-forming in water coagulating bath.Multipass is cleaned with deionized water, preserve in deionized water or drying at room temperature ring after taking-up
In border.
Embodiment 5
First by 100mg graphene oxides ultrasonic disperse in 100mL deionized waters, 2g tannin is added, solution is heated
50 DEG C of stirring 12h are warming up to, the membrane filtration in 0.2 μm of aperture of product, drying and grinding preserves after then cleaning, and obtains tannin modification
Graphene oxide (TA-GO).
By 1.5g TA-GO ultrasonic disperses in 84.5g DMF, in N213.5g warps are slowly added under protection into dispersion liquid
Pretreated PVDF powder (average molecular weight 100,000-40 ten thousand) and 0.5g perforating agent PVP K30s are dried, stirring is anti-
It should make casting solution uniform, stable for 24 hours, finally place it in deaeration 6h in vacuum drying chamber.
Casting solution obtained is poured on glass plate, the plate membrane that thickness is uniform, consistent is scraped with scraper, then by it
It is placed in film-forming in water coagulating bath.Multipass is cleaned with deionized water, preserve in deionized water or drying at room temperature ring after taking-up
In border.
Embodiment 6
First by 100mg graphene oxides ultrasonic disperse in 100mL deionized waters, 2g dopamines are added, by solution plus
Heat is warming up to 50 DEG C of stirring 12h, and the membrane filtration in 0.2 μm of aperture of product, drying and grinding preserves after then cleaning, and obtains dopamine
Modified graphene oxide (DA-GO).
By 1g DA-GO alkene ultrasonic disperses in 84g DMF, in N214g dryings are slowly added under protection into dispersion liquid
Pretreated PVDF powder (average molecular weight 100,000-40 ten thousand) and 1g perforating agent PVP K30s, are stirred to react for 24 hours
Keep casting solution uniform, stable, finally places it in deaeration 6h in vacuum drying chamber.
Casting solution obtained is poured on glass plate, the plate membrane that thickness is uniform, consistent is scraped with scraper, then by it
It is placed in film-forming in water coagulating bath.Multipass is cleaned with deionized water, preserve in deionized water or drying at room temperature ring after taking-up
In border.
Adsorption of metal ions sewage seperation film made from embodiment 1-6 has carried out dependence test according to the method described above, obtains
Adsorption efficiency contrast table as shown in Table 1.
The adsorption efficiency contrast table of adsorption of metal ions sewage seperation film made from 1 embodiment 1-6 of table
As can be seen from Table 1, polyphenol modified graphene oxide has very low-concentration metallic solion as adsorbent
High adsorption efficiency can reach 95% or more.Thus obtained seperation film is for the metal ion sewage disposal in life
There is larger application value.
Desorption efficiency comparative's table of adsorption of metal ions sewage seperation film made from 2 embodiment 1-6 of table
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Lead ion desorption rate | 95.4% | 94.6% | 93.3% | 96.5% | 95.2% | 90.8% |
| Copper ion desorption rate | 97.1% | 96.4% | 96.6% | 98.3% | 97.9% | 95.7% |
As can be seen from Table 2, de- to metal ion using adsorption of metal ions sewage seperation film made from the method for the present invention
Attached rate is also very high, therefore can use it for the recycle aspect to precious metals ion.
It chooses adsorption of metal ions sewage seperation film made from embodiment 5 and carries out cleaning and regeneration absorption test, as a result such as table 3
It is shown.
3 embodiment of table, 5 adsorption of metal ions sewage seperation film cleaning and regeneration number and adsorption efficiency relation table
As can be seen from Table 3, using adsorption of metal ions sewage seperation film made from the method for the present invention by being cleaned multiple times
It is still very high to the adsorption efficiency of metal ion after regeneration, illustrate that polyphenol modified graphene oxide is stabilized in adsorbed film,
Without departing from adsorbed film and then secondary pollution, more safety and environmental protection are caused to water body.
Adsorption of metal ions sewage seperation film is to bovine serum albumin(BSA) rejection contrast table made from 4 embodiment 1-6 of table
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Rejection | 60% | 57% | 61% | 62% | 61% | 56% |
As can be seen from Table 4, using adsorption of metal ions sewage seperation film made from the method for the present invention to bovine serum albumin
There is preferable rejection effect in vain, this is because protein is lyophobic dust, with the addition of polyphenol modified graphene oxide, film
The raising of surface hydrophilicity is unfavorable for passing through for protein, therefore retention rate of proteins increases.
Claims (9)
1. a kind of preparation method of adsorption of metal ions sewage seperation film, which is characterized in that include the following steps：
(a) it by graphene oxide ultrasonic disperse in deionized water, adds polyphenol compound and stirs evenly, after the completion of reaction
It is separated by solid-liquid separation and obtains the graphene oxide of polyphenol modification；
(b) the graphene oxide ultrasonic disperse for being modified polyphenol adds Kynoar, perforating agent fills in organic solvent A
Divide stirring, obtains casting solution；
(c) casting solution is poured over to scratch on tablet and is formed a film, then placed it in solution B and cure, finally take out washed, dry
It is dry, obtain adsorption of metal ions sewage seperation film.
2. preparation method as described in claim 1, it is characterised in that：The polyphenol compound is selected from tannin, dopamine, coke
One kind in gallate, catechol, table roasted catechins, addition and the graphene oxide mass ratio of polyphenol compound are 10-20:
1。
3. preparation method as described in claim 1, it is characterised in that：The Kynoar is powdered, mean molecule
Amount is 100,000-40 ten thousand.
4. preparation method as described in claim 1, it is characterised in that：The perforating agent is specially PVP K30.
5. preparation method as described in claim 1, it is characterised in that：The organic solvent A be selected from N,N-dimethylformamide,
One kind in DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone.
6. preparation method as described in claim 1, it is characterised in that：The one kind of the solution B in water, ethyl alcohol, octanol.
7. preparation method as described in claim 1, it is characterised in that：The quality for the graphene oxide that polyphenol is modified in casting solution
Score is 1%-2%, and the mass fraction of Kynoar is 10%-15%, and the mass fraction of perforating agent is 0.5%-2%, remaining
Amount is organic solvent A.
8. preparation method as described in claim 1, which is characterized in that the preparation method for the graphene oxide that polyphenol is modified is specific
It is as follows：By graphene oxide ultrasonic disperse in deionized water, it is heated to 30-60 DEG C and is stirred to react 8-16h, then use hole
Diameter is 0.1 μm -0.5 μm of membrane filtration, filter residue is washed, it is dry, grind to obtain the final product.
9. preparation method as described in claim 1, which is characterized in that the method for preparing casting solution is specific as follows：Polyphenol is changed
Property graphene oxide ultrasonic disperse in organic solvent A, be added into dispersion liquid under protective atmosphere dry in advance it is poly- partially
Vinyl fluoride and perforating agent are stirred to react 20-28h, and last froth in vacuum 4-8h to obtain the final product.
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