CN109289546A - A kind of preparation method of graphene black matrix filter membrane - Google Patents
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Abstract
The invention discloses a kind of preparation methods of graphene black matrix filter membrane comprising following steps: preparing layered graphite oxide alkene；Layered graphite oxide alkene is soluble in water, configure graphene solution；Graphene solution is filtered onto PVDF thin film, and is dried, semi-finished product are obtained；Semi-finished product are placed in hydrazine hydrate, carry out reacting to obtain graphene black matrix filter membrane under heating conditions.The invention has the benefit that a kind of preparation method of graphene black matrix filter membrane of the present invention, using the absorber of light being made of PVDF and graphene, graphene monolithic is splendid absorbent material；Substrate pvdf membrane is porous structure, i.e., the surface that inside the described graphene black matrix filter membrane there are a large amount of capillaries hydrone to be transported to absorber increases its disengagement area, improves evaporitic environment temperature, increases evaporation rate；Improve the temperature when absorption and water evaporation of system light；The solar distilling effect of the i.e. described graphene black matrix filter membrane is apparently higher than traditional solar distilling effect.
Description
Technical field
The present invention relates to filter membrane fields, and in particular to a kind of preparation method of graphene black matrix filter membrane.
Background technique
Social progress with the development of economy, energy shortage and scarcity of fresh water resources, which have been increasingly becoming, restricts world's warp
The key factor of Ji development.In face of the challenge of water resources crisis, people make every effort to find a kind of water purification technology of cost effective.
Solar distilling, radiation of its energy from sun when exactly distilling.Distillation process substantially salt water vaporization,
It stays lysed salt in the solution, then makes water recovery and obtain fresh water.Traditional solar distilling is by black
The bottom that absorber is placed in seawater is absorbed heat, mainly based on ceiling mounted solar energy sea water desalination apparatus.Sunlight is through top
The sea water layer being irradiated to inside distilling apparatus after the transparency cover of canopy, sunlight are absorbed by the black absorption body of sea water layer bottom.It inhales
Acceptor converts light energy into energy heats seawater, and ocean temperature rises evaporation and generates water vapour.However traditional solar distilling is answered
With having the shortcomings that absorptance is low, evaporation rate is slow in the process.Therefore the solar distilling that a kind of absorptivity is high, evaporation rate is fast is found
Material is the key that solve the problems, such as this.
Summary of the invention
The object of the present invention is to provide the fast solar distilling material of a kind of absorptivity height, evaporation rate, the filters of graphene black matrix
The preparation method of film.
A kind of preparation method of graphene black matrix filter membrane, comprising the following steps:
(1) layered graphite oxide alkene is prepared；
A, it takes crystalline graphite powder and sodium nitrate to be put into beaker, under conditions of ice bath, the concentrated sulfuric acid is added into beaker, and
It stirs evenly, potassium permanganate is then added, be stirred to react；It is reacted under conditions of ice bath, the oxidisability of the concentrated sulfuric acid
It is lower, the driving force of intercalation cannot be provided, and after oxidant potassium permanganate is added, the edge of graphite level is by oxygen first
Change, that is, reacts and only carried out on the surface layer of graphite linings；Simultaneously hydrogen sulfate ion and have polar sulfuric acid molecule drawn by electrostatic
Power is adsorbed on the edge of graphite level；With the progress of oxidation process and the increase of strong oxidizer potassium permanganate additional amount, graphite
In carbon hexagonal network plane gradually become the plane macromolecular with positive charge, therefore hydrogen sulfate ion and have polar
Sulfuric acid molecule is also gradually inserted graphite layers, and ultimately forms sulfuric acid-compound between graphite layers；
B, reaction solution after the reaction was completed, is warmed naturally into room temperature, then further progress is reacted under heating conditions,
Obtain intermediate product；Ice bath is reacted, is converted to and is performed under heating conditions reaction, because of the oxidation of potassium permanganate in a heated condition
Property be reinforced, make the reaction of sulfuric acid-compound between graphite layers further occurrence deep oxidation, at this time oxygen atom and carbon atom with
Covalent bond combines, six annulus of carbon is reacted and carried out by the inside that the surface layer of graphite linings turns to graphite linings by partial destruction；
C, deionized water is added into the beaker for fill intermediate product, is stirred to react a period of time, adds hot water, continues
Stirring, is then added hydrogen peroxide, stands, clean to obtain layered graphite oxide alkene；A large amount of water enters sulfuric acid-stone of deep oxidation
Between layer of ink and it is expelled from sulfuric acid, and ion exchange then occurs with hydrogen sulfate ion for the hydroxyl in water, displaces part
Hydrogen sulfate ion, and combined with the carbon atom in graphite level；It is extra in reaction solution that the addition of hydrogen peroxide can remove
Potassium permanganate is oxidized to be dissolved in the divalent manganesetion of water；
(2) layered graphite oxide alkene is soluble in water, configure graphene solution；
(3) graphene solution is filtered onto PVDF thin film, and dried, obtain semi-finished product；PVDF thin film gathers inclined difluoro second
Alkene film is that a kind of common solid support, membrane aperture vary in immunoblotting, with the continuous reduction of membrane aperture,
Film is more secured to the protein binding of low molecular weight；The mechanical strength and toughness of PVDF thin film are higher, and heat-resistant stability is good, have
Fire-retardant, low cigarette, anti-ultraviolet property.
(4) semi-finished product are placed in hydrazine hydrate, carry out reacting to obtain graphene black matrix filter membrane under heating conditions.Hydrazine hydrate
For 50% hydrazine hydrate aqueous solution bought from traditional Chinese medicines.
Further, in step (1), the crystalline graphite powder, sodium nitrate and, the concentrated sulfuric acid and potassium permanganate molar ratio be
14:1:41:2.6；The temperature of the ice bath is 7-9 DEG C.
Further, it in step b, stays under condition of ice bath, is stirred to react 2-2.5 hours, then warm naturally to room temperature,
Then under conditions of heating temperature is 38-43 DEG C, it is stirred to react 2-2.5h, obtains intermediate product.
Further, in step c, the mole of added deionized water and crystalline graphite powder is 38-40:1；Addition go from
After sub- water is stirred to react 30min, the hot water for being 38-40:1 with crystalline graphite powder molar ratio, hot water temperature 95- are added
100 DEG C, it is stirred to react 10min, the hydrogen peroxide for being 1.8-2:1 with crystalline graphite powder molar ratio is added, stands 12-14h, into
Row removal of impurities.
Further, in step c, the removal of impurities are as follows: remove the supernatant for standing liquid, the lower layer that centrifuge washing stands liquid is heavy
Starch to pH be 7；Sediment after washing is ultrasonically treated, then is centrifuged, upper solution is taken, obtains layered graphite oxide alkene.
Further, after the sediment after washing being ultrasonically treated 2h, the centrifugal treating in the centrifuge of 8000r/min
5min takes first time upper solution；After first time upper solution is ultrasonically treated 2h, it is centrifuged in the centrifuge of 10000r/min
5min is handled, second of upper solution is taken；After second of upper solution is ultrasonically treated 2h, in the centrifuge of 10000r/min
Centrifugal treating 5min, takes upper solution, obtains layered graphite oxide alkene.
Further, in step (2), the concentration of the graphene solution is 0.009375mg/ml.
Further, in step (3), the temperature of the drying is 70-80 DEG C, drying time 12-14h.
Further, in step (4), the temperature of the heating reaction is 55-60 DEG C, reaction time 2-2.5h.
Further, in the graphene black matrix filter membrane graphene layer with a thickness of 8-12nm.
The invention has the benefit that a kind of preparation method of graphene black matrix filter membrane of the present invention, using by PVDF
The absorber of light formed with graphene, because (graphene as shown in Figure 2 has very in the full spectrum 200-2500nm of solar radiation
Strong optical absorption characteristics), for graphene monolithic light absorption up to 2.3%, thermal conductivity is up to 4840w/m*k, is splendid absorption
Body material；Substrate pvdf membrane is porous structure, i.e., has a large amount of capillaries inside the described graphene black matrix filter membrane (as shown in Figure 1
With the presence of a large amount of capillary pipe structures inside graphene black matrix filter membrane), hydrone is transported into absorber using the effect of capillary
Surface, increase its disengagement area, improve evaporitic environment temperature, increase evaporation rate；Compared with traditional solar distilling, by
In the presence of graphene black matrix, the temperature when absorption and water evaporation of system light is improved；The i.e. described graphene black matrix filter membrane
Solar distilling effect is apparently higher than traditional solar distilling effect.
Detailed description of the invention
Fig. 1: the SEM figure of the graphene black matrix filter membrane；
Fig. 2: absorbance of the graphene black matrix filter membrane within the scope of 200nm-2500nm light wave；
Specific embodiment
Embodiment one
A kind of preparation method of graphene black matrix filter membrane, comprising the following steps:
(1) layered graphite oxide alkene is prepared；
A, it takes crystalline graphite powder and sodium nitrate to be put into beaker, under conditions of ice bath, the concentrated sulfuric acid is added into beaker, and
It stirs evenly, potassium permanganate is then added, be stirred to react；
B, reaction solution after the reaction was completed, is warmed naturally into room temperature, then further progress is reacted under heating conditions,
Obtain intermediate product；
C, deionized water is added into the beaker for fill intermediate product, is stirred to react a period of time, adds hot water, continues
Stirring, is then added hydrogen peroxide, stands, clean to obtain layered graphite oxide alkene；
(2) layered graphite oxide alkene is soluble in water, configure graphene solution；
(3) graphene solution is filtered onto PVDF thin film, and dried, obtain semi-finished product；
(4) semi-finished product are placed in hydrazine hydrate, carry out reacting to obtain graphene black matrix filter membrane under heating conditions.
Embodiment two
A kind of preparation method of graphene black matrix filter membrane, comprising the following steps:
(1) layered graphite oxide alkene is prepared；
A, it takes crystalline graphite powder and sodium nitrate to be put into beaker, under conditions of temperature is 7 DEG C of ice baths, is added into beaker
The concentrated sulfuric acid, and stir evenly, potassium permanganate is then added, is stirred to react；Added crystalline graphite powder, sodium nitrate, the concentrated sulfuric acid
Molar ratio with potassium permanganate is 14:1:41:2.6；
Under conditions of ice bath, the oxidisability of the concentrated sulfuric acid is lower, cannot provide the driving force of intercalation, and oxygen is being added
After agent potassium permanganate, the edge of graphite level is aoxidized first, that is, is reacted and only carried out on the surface layer of graphite linings；
B, it stays under condition of ice bath, is stirred to react 2 hours, reaction solution is warmed naturally into room temperature, then in heating temperature
Reaction 2h is futher stirred under conditions of being 38 DEG C, obtains intermediate product；
The oxidisability of potassium permanganate is reinforced in a heated condition, makes sulfuric acid-graphite linings compound further occurrence depth
Oxidation reaction, at this time oxygen atom is combined with carbon atom with covalent bond, and six annulus of carbon is by partial destruction, i.e., reaction is by graphite linings
Surface layer turn to the inside of graphite linings and carry out, and ultimately form sulfuric acid-compound between graphite layers；
C, deionized water, the mole of added deionized water and crystalline graphite powder are added into the beaker for fill intermediate product
For 38:1, after addition deionized water is stirred to react 30min, the hot water for being 38:1 with crystalline graphite powder molar ratio is added, it is added
The temperature of hot water is 95 DEG C, continues to be stirred to react 10min, and the hydrogen peroxide for being 1.8:1 with crystalline graphite powder molar ratio is then added,
Stand 12h, remove stand liquid supernatant, centrifuge washing stand liquid lower sediment thing to pH be 7, by the sediment after washing
After being ultrasonically treated 2h, the centrifugal treating 5min in the centrifuge of 8000r/min takes first time upper solution；By first time upper layer
After solution is ultrasonically treated 2h, the centrifugal treating 5min in the centrifuge of 10000r/min takes second of upper solution；It will be second
After upper solution is ultrasonically treated 2h, centrifugal treating 5min, takes upper solution in the centrifuge of 10000r/min, obtains stratiform oxidation
Graphene；
A large amount of water enters sulfuric acid-graphite layers of deep oxidation and is expelled from sulfuric acid, and the hydroxyl in water then with sulphur
Ion exchange occurs for sour hydrogen radical ion, displaces part of sulfuric acid hydrogen radical ion, and mutually tie with the carbon atom in graphite level
It closes；The addition of hydrogen peroxide can remove potassium permanganate extra in reaction solution, be oxidized to be dissolved in the divalent manganesetion of water.
(2) layered graphite oxide alkene is soluble in water, configuration graphene solution obtains the graphite that concentration is 0.009375mg/ml
Alkene solution；
(3) graphene solution is filtered onto PVDF thin film, dries 12h under conditions of temperature is 70 DEG C, obtains semi-finished product；
(4) semi-finished product are placed in hydrazine hydrate, reaction 2h obtains graphene layer thickness under conditions of temperature is 55 DEG C of heating
For the graphene black matrix filter membrane of 8nm.
Embodiment three
A kind of preparation method of graphene black matrix filter membrane, comprising the following steps:
(1) layered graphite oxide alkene is prepared；
A, it takes crystalline graphite powder and sodium nitrate to be put into beaker, under conditions of temperature is 8 DEG C of ice baths, is added into beaker
The concentrated sulfuric acid, and stir evenly, potassium permanganate is then added, is stirred to react；Added crystalline graphite powder, sodium nitrate, the concentrated sulfuric acid
Molar ratio with potassium permanganate is 14:1:41:2.6；
Under conditions of ice bath, the oxidisability of the concentrated sulfuric acid is lower, cannot provide the driving force of intercalation, and oxygen is being added
After agent potassium permanganate, the edge of graphite level is aoxidized first, that is, is reacted and only carried out on the surface layer of graphite linings；
B, it stays under condition of ice bath, is stirred to react 2.2 hours, reaction solution is warmed naturally into room temperature, then in heating temperature
Degree futher stirs reaction 2.2h under conditions of being 40 DEG C, obtain intermediate product；
The oxidisability of potassium permanganate is reinforced in a heated condition, makes sulfuric acid-graphite linings compound further occurrence depth
Oxidation reaction, at this time oxygen atom is combined with carbon atom with covalent bond, and six annulus of carbon is by partial destruction, i.e., reaction is by graphite linings
Surface layer turn to the inside of graphite linings and carry out, and ultimately form sulfuric acid-compound between graphite layers；
C, deionized water, the mole of added deionized water and crystalline graphite powder are added into the beaker for fill intermediate product
For 39:1, after addition deionized water is stirred to react 30min, the hot water for being 39:1 with crystalline graphite powder molar ratio is added, it is added
The temperature of hot water is 98 DEG C, continues to be stirred to react 10min, and the hydrogen peroxide for being 1.9:1 with crystalline graphite powder molar ratio is then added,
Stand 13h, remove stand liquid supernatant, centrifuge washing stand liquid lower sediment thing to pH be 7, by the sediment after washing
After being ultrasonically treated 2h, the centrifugal treating 5min in the centrifuge of 8000r/min takes first time upper solution；By first time upper layer
After solution is ultrasonically treated 2h, the centrifugal treating 5min in the centrifuge of 10000r/min takes second of upper solution；It will be second
After upper solution is ultrasonically treated 2h, centrifugal treating 5min, takes upper solution in the centrifuge of 10000r/min, obtains stratiform oxidation
Graphene；
A large amount of water enters sulfuric acid-graphite layers of deep oxidation and is expelled from sulfuric acid, and the hydroxyl in water then with sulphur
Ion exchange occurs for sour hydrogen radical ion, displaces part of sulfuric acid hydrogen radical ion, and mutually tie with the carbon atom in graphite level
It closes；The addition of hydrogen peroxide can remove potassium permanganate extra in reaction solution, be oxidized to be dissolved in the divalent manganesetion of water.
(2) layered graphite oxide alkene is soluble in water, configuration graphene solution obtains the graphite that concentration is 0.009375mg/ml
Alkene solution；
(3) graphene solution is filtered onto PVDF thin film, dries 13h under conditions of temperature is 75 DEG C, obtains semi-finished product；
(4) semi-finished product are placed in hydrazine hydrate, reaction 2.2h obtains graphene thickness under conditions of temperature is 58 DEG C of heating
Degree is the graphene black matrix filter membrane of 10nm.
Example IV
A kind of preparation method of graphene black matrix filter membrane, comprising the following steps:
(1) layered graphite oxide alkene is prepared；
A, it takes crystalline graphite powder and sodium nitrate to be put into beaker, under conditions of temperature is 9 DEG C of ice baths, is added into beaker
The concentrated sulfuric acid, and stir evenly, potassium permanganate is then added, is stirred to react；Added crystalline graphite powder, sodium nitrate, the concentrated sulfuric acid
Molar ratio with potassium permanganate is 14:1:41:2.6；
Under conditions of ice bath, the oxidisability of the concentrated sulfuric acid is lower, cannot provide the driving force of intercalation, and oxygen is being added
After agent potassium permanganate, the edge of graphite level is aoxidized first, that is, is reacted and only carried out on the surface layer of graphite linings；
B, it stays under condition of ice bath, is stirred to react 2.5 hours, reaction solution is warmed naturally into room temperature, then in heating temperature
Degree futher stirs reaction 2.5h under conditions of being 43 DEG C, obtain intermediate product；
The oxidisability of potassium permanganate is reinforced in a heated condition, makes sulfuric acid-graphite linings compound further occurrence depth
Oxidation reaction, at this time oxygen atom is combined with carbon atom with covalent bond, and six annulus of carbon is by partial destruction, i.e., reaction is by graphite linings
Surface layer turn to the inside of graphite linings and carry out, and ultimately form sulfuric acid-compound between graphite layers；
C, deionized water, the mole of added deionized water and crystalline graphite powder are added into the beaker for fill intermediate product
For 40:1, after addition deionized water is stirred to react 30min, the hot water for being 40:1 with crystalline graphite powder molar ratio is added, it is added
The temperature of hot water is 00 DEG C, continues to be stirred to react 10min, and the hydrogen peroxide for being 2:1 with crystalline graphite powder molar ratio is then added, quiet
14h is set, the supernatant for standing liquid is removed, the lower sediment thing of centrifuge washing standing liquid is 7 to pH, and the sediment after washing is surpassed
After sonication 2h, the centrifugal treating 5min in the centrifuge of 8000r/min takes first time upper solution；First time upper layer is molten
After liquid is ultrasonically treated 2h, the centrifugal treating 5min in the centrifuge of 10000r/min takes second of upper solution；It will be on second
After layer solution ultrasonic treatment 2h, centrifugal treating 5min, takes upper solution in the centrifuge of 10000r/min, obtains stratiform oxidation stone
Black alkene；
A large amount of water enters sulfuric acid-graphite layers of deep oxidation and is expelled from sulfuric acid, and the hydroxyl in water then with sulphur
Ion exchange occurs for sour hydrogen radical ion, displaces part of sulfuric acid hydrogen radical ion, and mutually tie with the carbon atom in graphite level
It closes；The addition of hydrogen peroxide can remove potassium permanganate extra in reaction solution, be oxidized to be dissolved in the divalent manganesetion of water.
(2) layered graphite oxide alkene is soluble in water, configuration graphene solution obtains the graphite that concentration is 0.009375mg/ml
Alkene solution；
(3) graphene solution is filtered onto PVDF thin film, dries 14h under conditions of temperature is 80 DEG C, obtains semi-finished product；
(4) semi-finished product are placed in hydrazine hydrate, reaction 2.5h obtains graphene thickness under conditions of temperature is 60 DEG C of heating
Degree is the graphene black matrix filter membrane of 12nm.
The present invention is not limited to above-mentioned preferred forms, anyone can show that other are various under the inspiration of the present invention
The product of form, however, make any variation in its details, it is all that there is technical solution identical or similar to the present application,
It is within the scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene black matrix filter membrane, which comprises the following steps:
(1) layered graphite oxide alkene is prepared；
A, it takes crystalline graphite powder and sodium nitrate to be put into beaker, under conditions of ice bath, the concentrated sulfuric acid is added into beaker, and stir
Uniformly, potassium permanganate is then added, is stirred to react；
B, after the reaction was completed, reaction solution is warmed naturally into room temperature, then further progress is reacted under heating conditions, is obtained
Between product；
C, deionized water is added into the beaker for fill intermediate product, is stirred to react a period of time, adds hot water, continue to stir
It mixes, hydrogen peroxide is then added, stand, clean to obtain layered graphite oxide alkene；
(2) layered graphite oxide alkene is soluble in water, configure graphene solution；
(3) graphene solution is filtered onto PVDF thin film, and dried, obtain semi-finished product；
(4) semi-finished product are placed in hydrazine hydrate, carry out reacting to obtain graphene black matrix filter membrane under heating conditions.
2. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that described in step (1)
Crystalline graphite powder, sodium nitrate, the concentrated sulfuric acid and potassium permanganate molar ratio be 14:1:41:2.6；The temperature of the ice bath is 7-9
℃。
3. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that in step b, stay in ice
It under the conditions of bath, is stirred to react 2-2.5 hours, then warm naturally to room temperature, the condition for being then 38-43 DEG C in heating temperature
Under, it is stirred to react 2-2.5h, obtains intermediate product.
4. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that added to go in step c
The mole of ionized water and crystalline graphite powder is 38-40:1；It is added after deionized water is stirred to react 30min, adds and scale
Graphite powder molar ratio is the hot water of 38-40:1, and hot water temperature is 95-100 DEG C, is stirred to react 10min, adds and scale stone
Ink powder molar ratio is the hydrogen peroxide of 1.8-2:1, stands 12-14h, cleans.
5. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that described to remove in step c
It is miscellaneous are as follows: remove stand liquid supernatant, centrifuge washing stand liquid lower sediment thing to pH be 7；By the sediment after washing into
Row ultrasonic treatment, then be centrifuged, upper solution is taken, layered graphite oxide alkene is obtained.
6. a kind of preparation method of graphene black matrix filter membrane according to claim 5, which is characterized in that by the precipitating after washing
After object is ultrasonically treated 2h, the centrifugal treating 5min in the centrifuge of 8000r/min takes first time upper solution；It will be on first time
After layer solution ultrasonic treatment 2h, the centrifugal treating 5min in the centrifuge of 10000r/min takes second of upper solution；By second
After secondary upper solution ultrasonic treatment 2h, centrifugal treating 5min, takes upper solution in the centrifuge of 10000r/min, obtains stratiform oxygen
Graphite alkene.
7. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that described in step (2)
The concentration of graphene solution is 0.009375mg/ml.
8. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that described in step (3)
The temperature of drying is 70-80 DEG C, drying time 12-14h.
9. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that described in step (4)
The temperature of heating reaction is 55-60 DEG C, reaction time 2-2.5h.
10. a kind of preparation method of graphene black matrix filter membrane according to claim 1, which is characterized in that the graphene is black
Graphene layer with a thickness of 8-12nm in body filter membrane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109910418A (en) * | 2019-03-22 | 2019-06-21 | 四川大学 | Thermally conductive polytetrafluoroethylene film with porous structure and preparation method thereof |
| WO2020248017A1 (en) * | 2019-06-12 | 2020-12-17 | Newsouth Innovations Pty Limited | Filtration membrane and method of production thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150103480A (en) * | 2014-03-03 | 2015-09-11 | 한국과학기술연구원 | Membrane Distillation Module |
| CN105542333A (en) * | 2015-12-15 | 2016-05-04 | 东华大学 | Reduced graphene oxide composite film and preparation method thereof |
| CN106000362A (en) * | 2016-05-18 | 2016-10-12 | 上海交通大学 | Composite thin film integrating photothermal conversion performance and adsorption characteristics as well as preparation and application of composite thin film |
| CN106750296A (en) * | 2017-03-20 | 2017-05-31 | 西北工业大学 | A kind of modified graphene/polyimides heat-conductive composite material and preparation method thereof |
| CN106865528A (en) * | 2017-02-24 | 2017-06-20 | 湖北大学 | A kind of oxidation graphene film and its preparation method and application |
| CN107106986A (en) * | 2014-10-03 | 2017-08-29 | 威廉马歇莱思大学 | Surface modified porous membrane is used for the purposes that fluid distills |
| US20170333848A1 (en) * | 2013-10-04 | 2017-11-23 | New Jersey Institute Of Technology | Nanocarbon immobilized membranes |
| CN207016517U (en) * | 2017-04-24 | 2018-02-16 | 东华大学 | A kind of new type solar energy photo-thermal seawater evaporator |
| CN108043242A (en) * | 2017-11-30 | 2018-05-18 | 商丘师范学院 | A kind of preparation method of the adjustable graphene oxide membrane of surface wettability energy |
| CN108176247A (en) * | 2018-02-28 | 2018-06-19 | 长沙理工大学 | Nano composite filtering membrane for brine separation and preparation method and application thereof |
-
2018
- 2018-10-26 CN CN201811255302.8A patent/CN109289546A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170333848A1 (en) * | 2013-10-04 | 2017-11-23 | New Jersey Institute Of Technology | Nanocarbon immobilized membranes |
| KR20150103480A (en) * | 2014-03-03 | 2015-09-11 | 한국과학기술연구원 | Membrane Distillation Module |
| CN107106986A (en) * | 2014-10-03 | 2017-08-29 | 威廉马歇莱思大学 | Surface modified porous membrane is used for the purposes that fluid distills |
| CN105542333A (en) * | 2015-12-15 | 2016-05-04 | 东华大学 | Reduced graphene oxide composite film and preparation method thereof |
| CN106000362A (en) * | 2016-05-18 | 2016-10-12 | 上海交通大学 | Composite thin film integrating photothermal conversion performance and adsorption characteristics as well as preparation and application of composite thin film |
| CN106865528A (en) * | 2017-02-24 | 2017-06-20 | 湖北大学 | A kind of oxidation graphene film and its preparation method and application |
| CN106750296A (en) * | 2017-03-20 | 2017-05-31 | 西北工业大学 | A kind of modified graphene/polyimides heat-conductive composite material and preparation method thereof |
| CN207016517U (en) * | 2017-04-24 | 2018-02-16 | 东华大学 | A kind of new type solar energy photo-thermal seawater evaporator |
| CN108043242A (en) * | 2017-11-30 | 2018-05-18 | 商丘师范学院 | A kind of preparation method of the adjustable graphene oxide membrane of surface wettability energy |
| CN108176247A (en) * | 2018-02-28 | 2018-06-19 | 长沙理工大学 | Nano composite filtering membrane for brine separation and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109910418A (en) * | 2019-03-22 | 2019-06-21 | 四川大学 | Thermally conductive polytetrafluoroethylene film with porous structure and preparation method thereof |
| CN109910418B (en) * | 2019-03-22 | 2021-02-23 | 四川大学 | Heat-conducting polytetrafluoroethylene film with porous structure and preparation method thereof |
| WO2020248017A1 (en) * | 2019-06-12 | 2020-12-17 | Newsouth Innovations Pty Limited | Filtration membrane and method of production thereof |
| CN114144253A (en) * | 2019-06-12 | 2022-03-04 | 新南创新私人有限公司 | Filter membrane and method for producing same |
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