CN208082233U - A kind of film filter of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary - Google Patents
A kind of film filter of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary Download PDFInfo
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- CN208082233U CN208082233U CN201820022440.0U CN201820022440U CN208082233U CN 208082233 U CN208082233 U CN 208082233U CN 201820022440 U CN201820022440 U CN 201820022440U CN 208082233 U CN208082233 U CN 208082233U
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Abstract
The utility model discloses a kind of film filters of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary, which includes ultrasonic wave added membrane filtration recirculating still, pH detectors, feed pump and storage tank；Ultrasonic wave added membrane filtration recirculating still includes the membrane support cavity pipe fitting being located in autoclave body, membrane material component, tube sheet, waterstop, ultrasonic vibration source group in situ and conducting wire；Kettle nozzle III and kettle nozzle IV are equipped on the upside of autoclave body, downside is equipped with kettle nozzle I and kettle nozzle II；Ultrasonic wave added membrane filtration recirculating still is connected through kettle nozzle IV with pH detectors；PH detectors are connected through valve II, storage tank, feed pump with kettle nozzle II, and pH detectors are connected with valve I, and storage tank is connected with inlet valve.The cleaning energy consumption of film filter described in the utility model is about the 1/10 of the prior art, and realizes the preparation of excellent pattern graphene.
Description
Technical field
The utility model is related to a kind of film filters of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary.
Background technology
Graphene is proposed from the seminar of the A.K. Geim leaders of University of Manchester in 2004（Graphene）Concept
Since, an other bright star of the graphene as carbon family has obtained the great attention of physics, chemistry and material scholar,
Therefore, graphene becomes another " universal material " (Science 2004,306 to yield unusually brilliant results after carbon nanotube:
666.).Compared with carbon nanotube, there are perfect hybrid structures for graphene, with superelevation conductivity, the electron-transport being exceedingly fast speed
Degree, high rigidity, high-specific surface area and room-temperature quantum Hall effect etc. attract attention always (Nat. Mater. 2007,6,
183；Science 2009, 324, 1530.).Up to the present, scientific research personnel has carried out extensively the preparation of graphene
Research, the preparation method in relation to graphene has more literature review both at home and abroad.But graphene can't magnanimity system at present
Standby, expensive price seriously hinders the application process of graphene.Therefore, how magnanimity prepares high quality, structure-controllable and valence
The cheap graphene of lattice has become the main bottleneck and urgent problem in terms of current graphene application and development.
Stankovich in 2006 etc. is prepared for graphene oxide by the way that graphite is carried out oxidation, and using hydrazine reduction removing
Oxygen-containing group on graphene oxide, has finally obtained grapheme material.Since this method raw material is cheap, equipment requirement is low, behaviour
Make simply, the graphene number of plies of preparation is few, and quality is high, prepared by the graphene to become most application potential and development prospect
Method.Therefore, mass prepares graphene oxide, becomes graphene and produces the committed step strided forward towards industrial process.Oxygen
Change graphite oxide solution prepared by reduction method, due to hydrophilic functional groups such as enrichment hydroxyl, carboxyl and epoxy groups, shows strong
Hydrophily, with going deep into for purification, graphene oxide forms water-setting with water（It is molten）Glue, no matter using the skill for filtering or centrifuging
Art is all difficult to detach graphite oxide solution, constrains the output of graphene oxide, hinders graphene batch production.It is real at present
It tests room and mostly uses macromolecule dialysis membrane and graphene oxide is purified.This method is that impurity small molecule is allowed to pass through membrane diffusion of dialysing
Into water, under the action of molecular dynamics, using concentration difference as motive force, the exchange of solute molecule is carried out, utilizes dialysis fenestra
The size of diameter retains sample, through impurity molecule, to achieve the purpose that separating-purifying.This method equipment investment is few, can be only
Graphene oxide stripping and graphene reduction work independent operation are stood on, there is the production of very important industrialization continuous batch
Value.However, graphene oxide layer structure is frivolous, surface functional group is abundant, extremely strong dispersed and easily adherent feature,
It causes in membrane filtration processes, blocking pipeline is serious, and to cause membrane filtration, time-consuming, and film is replaced frequent equal very serious
Production cost problem.In addition, commercially available ceramics cross-flow filtration film, ceramic membrane, the complicated solid in fenestra road easily block,
And conventional backwash liquid all can not etching oxidation graphene, graphene oxide can only by sintering and ultrasound removal surface,
Vltrasonic device is not thorough enough to the graphene oxide removal in drilling fenestra road, and ceramic membrane sintering number is limited, this is all system
What the film dialysis of about graphene oxide purified.Therefore, in order to realize graphene oxide mass purification, it is necessary to search out one kind
The continuously and automatically film filter that can be applied to graphene oxide dialysis, can just be expected to take in terms of macroscopic preparation of graphene
Obtain breakthrough progress.
Utility model content
The purpose of this utility model is to provide a kind of membrane filtrations of inexpensive mass cleaning that realizing graphene oxide
Device.
The cleaning energy consumption of film filter described in the utility model is about the 1/10 of the prior art, and realizes excellent pattern
The preparation of graphene.
The film filter of the continuous automatic cleaning graphene oxide of a kind of ultrasonic wave auxiliary, it is characterised in that the device includes
Ultrasonic wave added membrane filtration recirculating still, pH detectors, feed pump and storage tank；The ultrasonic wave added membrane filtration recirculating still includes being located at kettle
Internal membrane support cavity pipe fitting, membrane material component, tube sheet, waterstop, ultrasonic vibration source group in situ and conducting wire；The membrane support chamber
Body pipe fitting is the porous hollow type structure in intermediate position, by tube sheet fixed cast inside autoclave body；The membrane material component selection
Flexible membrane material is simultaneously fastened on membrane support cavity pipe fitting, and seals upper and lower port by waterstop, and membrane material component is logical
Lower flange is crossed to be replaced；The ultrasonic vibration source group in situ is made of multigroup ultrasonic vibrator, and is hung on using conducting wire series connection
Membrane support cavity inside pipe fitting, conducting wire are drawn by upper flange in kettle Ligation in vitro power supply；Kettle nozzle is equipped on the upside of the autoclave body
III and kettle nozzle IV, downside is equipped with kettle nozzle I and kettle nozzle II；The ultrasonic wave added membrane filtration recirculating still is through kettle nozzle IV and pH
Detector is connected；The pH detectors are connected through valve II, storage tank, feed pump with kettle nozzle II, pH detectors and valve I phases
Even, storage tank is connected with inlet valve.
The material of the membrane support cavity pipe fitting is PVC（Polyvinyl chloride）,PC（Makrolon）,PS（Polystyrene）Or
PTFE（Polytetrafluoroethylene (PTFE)）.Material price used is cheap and corrosion resistance is preferable, and being designed as porous hollow type structure can increase
The contact area of graphene oxide and filter membrane material, to accelerated filtration efficiency.
The membrane material component is organic polymer synthetic fabrics, such as nylon fabric, nylon fabric, polypropylene fibre knits
Object, polyvinyl fabric or dacron.The membrane material component be it is a kind of it is flexible load and unload replaceable, encapsulation is in membrane support chamber
On body, can the size according to graphene oxide sheet diameter and the corrosion factor with cleaning solution, select unlike material different pore size
Flexible membrane.
Total ultrasonic power of the ultrasonic vibration source group in situ is 20 ~ 80W, and frequency is 25 ~ 40KHZ, and vibration source part is corrosion resistant
Lose stainless steel.Ultrasound vibration source group in situ can realize that the concussion to membranous wall bur removes in entire filtering circulating device
And the ultrasonic disperse to circulating liquid.
Traditional filtering cross-flow film device, uses ceramic membrane mostly, and ceramic membrane aperture structure is complex, in processing oxygen
When the floating suspension of this nanoscale twins scale of graphite alkene, it is easy to blocked, and again because of graphene oxide physical property
Stabilization is almost resistant to all chemical reagent at normal temperatures and pressures, is handled it is difficult to backwash Membrane cleaning mode by traditional washing lotion,
It causes film to block serious, can not restore, improve cost and recycle degree.It can not be complete using ultrasonic cleaning solution
Graphene oxide layer inside the embedded three-dimensional aperture of transfer, the ceramic membrane that graphene oxide blocks only are gone by high temperature sintering
Restore fenestra except graphene oxide, but since membrane support plumbing is fixed, and frequently dismantled in production process, it causes
The sealing of device sexually revises, and sintering restores to be difficult to apply in fenestra actual production.And the utility model uses flexible has
Machine Polymer Synthesizing tunica fibrosa, excellent anti-corrosion performance, thickness is low, is according to fabric mostly to which membrane aperture is simple in structure
Establishment density and the various apertures built, foreign ion motion mode in this aperture are simple, insert depth is low, is easy to de-
Go out, shortens ion motion path, and by the flange opening replacement membrane material above and below autoclave body, can ensure integral tube
Under the premise of road is not loaded and unloaded, applicable flexible membrane is sleeved on support tube, and is encapsulated using waterstop, to realize simple replace
Method.In addition, the characteristics of being easy to block aperture according to graphene oxide, the utility model is arranged in situ super in membrane support cavity
Sound accessory part, being can be while membrane filtration, and ultrasound removal in situ is blocked in the graphene oxide layer of film surface, allows
During the graphene oxide layer moment is in a kind of movement, film surface can not be rested on, and small molecular weight impurity ion can be with
Random slave hole surface abjection, achievees the purpose that purification.Even graphene oxide patch has born film surface, and ultrasonic vibration is also very
Readily then returned to liquid internal, the visible experimental result of subsequent embodiment.The ultrasonic power requirement that the process uses
It is very low.The equipment solves the critical issue that graphene oxide is cleaned with membrane filtration, while the equipment can be by amplifying and going here and there
Join component and expand scale, solves the problems, such as the cleaning of graphene oxide scale.
The utility model has the beneficial effects that：
1, the utility model is constituted by simple, cheap equipment single component and prepares graphite oxide for filtering purification
Alkene it is a kind of can scale application device.
2, the selection membrane filtration material flexible of the utility model innovation can be according to different graphene oxide liquid
Corrosivity and graphene oxide size selection and replacement membrane material and aperture, successfully solve different model graphene oxide
Cleaning problem increases the applicable range of equipment.Using membrane material flexible, it is easy to cut and is sealed into suitable for variously-shaped
Holder cavity, and fenestra road is simple in structure, and foreign ion deviates from that path is short, and ultrasonication is with obvious effects, material toughness
Height, ultrasonication is with obvious effects, avoids the wall thickness of traditional ceramic filter membrane etc., duct stereochemical structure is complicated, foreign ion
Deviate from path length, is difficult to restore and to being cleaned by ultrasonic the problems such as vibration frequency requirement restored is harsh after blocking.
3, the utility model be arranged internal in-situ sonic oscillation device, can be realized in entire filtering circulating device for
Recovery and the quick abjection for foreign ion at any time in the blocked duct of membranous wall, solving graphene oxide can not be anti-in situ
The problem of rinsing the fenestra for restoring to block.
Description of the drawings
Fig. 1 is the structural schematic diagram of the utility model.
Fig. 2 is the structural schematic diagram of ultrasonic wave added membrane filtration recirculating still described in the utility model.
Fig. 3 is the structural schematic diagram of membrane support cavity pipe fitting described in the utility model.
Fig. 4 is that nylon cloth is material surface pattern photo after setting ultrasound filtration in situ in membrane filtration material.
Fig. 5 is that nylon cloth is material surface pattern photo after not setting ultrasound filtration in situ in membrane filtration material.
Fig. 6 is the stereoscan photograph of graphene oxide design feature.
In figure：The upper lower flanges of 1-；2- kettles nozzle IV；3- autoclave bodies；4- conducting wires；5- tube sheets；6- kettles nozzle II；7- membrane support chambers
Body pipe fitting；8- kettles nozzle III；9- ultrasonic vibration source groups in situ；10- membrane material components；11- waterstops；12- kettles nozzle I；13- is stored up
Tank；14- feed pumps；15- ultrasonic wave added membrane filtration recirculating stills；16- power supplys；17- valves I；18- valves II；19-pH detectors；
20- inlet valves.
Specific implementation mode
As shown in Figure 1, 2, 3, the film filter of the continuous automatic cleaning graphene oxide of a kind of ultrasonic wave auxiliary, the device
Including ultrasonic wave added membrane filtration recirculating still 15, pH detectors 19, feed pump 14 and storage tank 13；Ultrasonic wave added membrane filtration recirculating still 15
Include membrane support cavity pipe fitting 7 in autoclave body 3, membrane material component 10, tube sheet 5, waterstop 11, ultrasonic vibration source group 9 in situ
With conducting wire 4；Membrane support cavity pipe fitting 7 is the porous hollow type structure in intermediate position, by 5 fixed cast of tube sheet inside autoclave body 3；
Membrane material component 10 selects flexible membrane material and is fastened on membrane support cavity pipe fitting 7, and by the sealing of waterstop 11
Lower port, membrane material component 10 are replaced by 1 orchid of upper laxative remedy；Ultrasound vibration source group 9 in situ is made of multigroup ultrasonic vibrator, and
It is hung on inside membrane support cavity pipe fitting 7 using the series connection of conducting wire 4, conducting wire 4 is drawn by upper flange and connects power supply outside autoclave body 3；
3 upside of autoclave body is equipped with kettle nozzle III 8 and kettle nozzle IV 2, and downside is equipped with kettle nozzle I 12 and kettle nozzle II 6；Ultrasonic wave added membrane filtration
Recirculating still 15 is connected through kettle nozzle IV 2 with pH detectors 19；PH detectors 19 are through valve II 18, storage tank 13, feed pump 14 and kettle
Nozzle II 6 is connected, and pH detectors 19 are connected with valve I17, and storage tank 13 is connected with inlet valve 20.
The material of membrane support cavity pipe fitting 7 is PVC（Polyvinyl chloride）,PC（Makrolon）,PS（Polystyrene）Or PTFE
（Polytetrafluoroethylene (PTFE)）.
Membrane material component 10 is organic polymer synthetic fabrics, such as nylon fabric, nylon fabric, polypropylene fabric,
Polyvinyl fabric or dacron.
Total ultrasonic power of ultrasound vibration source group 9 in situ is 20 ~ 80W, and frequency is 25 ~ 40KHZ, vibration source part be it is corrosion-resistant not
Rust steel material.
Embodiment 1
Graphene oxide is prepared using hummers methods, by multiple natural subsidence, graphene oxide aqueous dispersions to be washed
Inlet valve 20 is opened in pH=1.5 referring to Fig.1, into sample storage tank 13, opens feed pump 14 by graphene oxide water to be cleaned
Dispersion liquid squeezes into ultrasonic wave added membrane filtration recirculating still 15, wherein the power supply 16 of ultrasonic vibration source component is arranged outside autoclave body, for auxiliary
The graphene oxide liquid to be cleaned flowed in pipe fitting in cleaning autoclave body is helped, after filtering, graphene oxide is to be cleaned to be entered
Test sample purity in pH detectors 19, sample test is up to standard, opens valve I17 and collects storage, if sample detection is below standard
It then opens valve II18 and enters in sample storage tank 13 and continue cycling through cleaning.Recycle stream of the graphene oxide liquid to be cleaned in autoclave body
It is dynamic that with reference to Fig. 2, graphene oxide liquid to be cleaned is entered by the kettle nozzle II 6 of ultrasonic wave added membrane filtration recirculating still 15 in wall,
It is flowed in membrane tube body, membrane tube part is to be encapsulated on membrane support cavity pipe fitting 7 by the winding of membrane material component 10, and pass through waterstop
11 be sealed prevent leakage constitute, wherein membrane support cavity pipe fitting 7 is as shown in figure 3, membrane support cavity pipe fitting 7 is middle part
The structure for dividing hollow out, is conducive to the high degree in contact of liquid and membrane material, membrane tube part is to be connected and fixed to cleaning solution by tube sheet 5
On body circulation tank body 3, the parallel operation of multigroup pipe fitting is constituted, promotes working efficiency.During filtering and impurity removing, pass through original
Position ultrasound vibration source group 9 is connected on conducting wire 4, and the ultrasonic wave in situ of formation carries out quick impurity abjection to sample, and in situ extensive
The membrane aperture blocked again, realizes an efficient continuous clean cycle device, and ejected wash water enters from kettle nozzle I 12, passes through
The flow velocity and temperature for adjusting ejected wash water can speed up and control the speed of graphene oxide foreign ion abjection, after cycle
Ejected wash water flowed out from kettle nozzle III 8, carry out ion removing processing, be again introduced into autoclave body and carry out graphene oxide foreign ion
Removal.After carrying out two groups of cycles, graphene oxide aqueous dispersions pH value is detected>5, representative sample has cleaned up, and leads to
Cross lower flange 1 lay down used nylon cloth material membrane material component 10 be scanned Electronic Speculum characterization, as shown in figure 4, base
It is remained without excessive graphene oxide layer on nylon cloth in sheet, it was demonstrated that this device of structure can be good at eliminating hole plug
Problem.
Comparative example
Specific device such as embodiment 1 does not open the power supply 16 of ultrasonic vibration source component in cyclic process, follow for eight times
Ring detects that graphene oxide aqueous dispersions pH value has reached 2.5, and extends the time and also be difficult to promote the pH value of liquid again,
Shutdown emptying graphene oxide after washing lotion, in opening lower flange 1 lay down the membrane material component 10 of the nylon cloth material used into
Row scanning electron microscope characterizes, and such as Fig. 5, shown in 6, there are many graphene oxide layers residuals substantially on nylon cloth, substantially stifled
Whole holes has been filled in, circulating filtration inefficiency is caused.
Claims (5)
1. a kind of film filter of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary, it is characterised in that the device includes super
Sound auxiliary film filtration cycle kettle（15）, pH detectors（19）, feed pump（14）And storage tank（13）；The ultrasonic wave added membrane filtration follows
Ring kettle（15）Including being located at autoclave body（3）Interior membrane support cavity pipe fitting（7）, membrane material component（10）, tube sheet（5）, waterstop
（11）, vibration source group in situ ultrasonic（9）And conducting wire（4）；The membrane support cavity pipe fitting（7）For the porous hollow type knot in intermediate position
Structure passes through tube sheet（5）Fixed cast is in autoclave body（3）It is internal；The membrane material component（10）The flexible membrane material of selection is simultaneously wound solid
It is scheduled on membrane support cavity pipe fitting（7）On, and pass through waterstop（11）Seal upper and lower port, membrane material component（10）Pass through upper laxative remedy
（1）Orchid is replaced；The ultrasonic vibration source group in situ（9）It is made of multigroup ultrasonic vibrator, and utilizes conducting wire（4）Series connection is hung on
Membrane support cavity pipe fitting（7）Inside, conducting wire（4）It is drawn in autoclave body by upper flange（3）Outer connection power supply；The autoclave body（3）On
Side is equipped with kettle nozzle III（8）With kettle nozzle IV（2）, downside is equipped with kettle nozzle I（12）With kettle nozzle II（6）；The ultrasonic wave added
Membrane filtration recirculating still（15）Through kettle nozzle IV（2）With pH detectors（19）It is connected；The pH detectors（19）Through valve II（18）,
Storage tank（13）, feed pump（14）With kettle nozzle II（6）It is connected, pH detectors（19）With valve I（17）It is connected, storage tank（13）With into
Expect valve（20）It is connected.
2. film filter as described in claim 1, it is characterised in that the membrane support cavity pipe fitting（7）Material be PVC,
PC, PS or PTFE.
3. film filter as described in claim 1, it is characterised in that the membrane material component（10）It is closed for organic polymer
At fabric.
4. film filter as described in claim 1, it is characterised in that the membrane material component（10）For nylon fabric, polypropylene fibre
Fabric, polyvinyl fabric or dacron.
5. film filter as described in claim 1, it is characterised in that the ultrasonic vibration source group in situ（9）Total ultrasonic power
For 20 ~ 80W, frequency is 25 ~ 40KHZ, and vibration source part is corrosion-resistant stainless steel material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820022440.0U CN208082233U (en) | 2018-01-08 | 2018-01-08 | A kind of film filter of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary |
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| CN201820022440.0U CN208082233U (en) | 2018-01-08 | 2018-01-08 | A kind of film filter of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109485039A (en) * | 2018-11-19 | 2019-03-19 | 大同新成新材料股份有限公司 | A kind of purification devices and its method of graphene oxide |
| CN110013767A (en) * | 2018-01-08 | 2019-07-16 | 中国科学院兰州化学物理研究所 | A kind of film filter of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary |
| CN111346429A (en) * | 2018-12-21 | 2020-06-30 | P&I人类韩国有限公司 | Water treatment facility |
-
2018
- 2018-01-08 CN CN201820022440.0U patent/CN208082233U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110013767A (en) * | 2018-01-08 | 2019-07-16 | 中国科学院兰州化学物理研究所 | A kind of film filter of the continuous automatic cleaning graphene oxide of ultrasonic wave auxiliary |
| CN110013767B (en) * | 2018-01-08 | 2024-02-06 | 中国科学院兰州化学物理研究所 | Membrane filtration device for ultrasonic-assisted continuous automatic cleaning of graphene oxide |
| CN109485039A (en) * | 2018-11-19 | 2019-03-19 | 大同新成新材料股份有限公司 | A kind of purification devices and its method of graphene oxide |
| CN111346429A (en) * | 2018-12-21 | 2020-06-30 | P&I人类韩国有限公司 | Water treatment facility |
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