KR20170012843A - Graphene filter was manufactured by the manufacturing method and applies graphene and graphene filter water purifier filter - Google Patents

Graphene filter was manufactured by the manufacturing method and applies graphene and graphene filter water purifier filter Download PDF

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KR20170012843A
KR20170012843A KR1020150105335A KR20150105335A KR20170012843A KR 20170012843 A KR20170012843 A KR 20170012843A KR 1020150105335 A KR1020150105335 A KR 1020150105335A KR 20150105335 A KR20150105335 A KR 20150105335A KR 20170012843 A KR20170012843 A KR 20170012843A
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graphene
filter
substrate
housing
graphene filter
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KR1020150105335A
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Korean (ko)
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KR101753969B1 (en
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윤석구
안성필
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고려대학교 산학협력단
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055—Carbonaceous material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • 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
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0471—Surface coating material
    • B01D2239/0478—Surface coating material on a layer of the filter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
    • B01D2239/0604—Arrangement of the fibres in the filtering material
    • B01D2239/0631—Electro-spun
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10—Filtering material manufacturing

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geology (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The present invention relates to a method for manufacturing a graphene filter for cleaning wastewater which can produce a graphene filter quickly and inexpensively without depending on a chemical vapor deposition method or a mechanical stripping method and has excellent water purification ability and a graphene filter and a graphene filter To a water purification apparatus. A method for manufacturing a graphene filter for purifying sewage water according to the present invention comprises the steps of: electrospinning an intervening layer, which comprises electrospinning a solution of a polymer dissolved in a surface of a substrate on which meshes are formed by crossing a steel string to form an intervening layer; And an outermost layer coating step of coating the back graphene on the surface of the intervening layer to form an outermost layer. The method of manufacturing a graphene filter for purifying sewage water according to the present invention comprises the steps of electrospinning a polymer on the surface of a substrate and coating the surface of the coated polymer with graphene to thereby produce a graphene filter quickly and inexpensively In addition, coated graphene is not easily removed, and a high-quality graphene filter can be manufactured.

Description

TECHNICAL FIELD The present invention relates to a graphene filter and a graphene filter, and to a graphene filter and a graphene filter,

The present invention relates to a method for manufacturing a graphene filter for cleaning wastewater which can produce a graphene filter quickly and inexpensively without depending on a chemical vapor deposition method or a mechanical stripping method and has excellent water purification ability and a graphene filter and a graphene filter To a water purification apparatus.

In recent years, separation materials that remove contaminated materials have been attracting attention as environmental problems have become more prominent. Demand is increasing due to diversification of active research and use fields for high performance of separation material functions and applications.

In particular, water pollution caused by municipal waste and food waste causes mixing of excessive organic matter into water, which accelerates the eutrophication of rivers, oceans, and reservoirs, and causes severe damage to the aquatic ecosystem.

Therefore, various studies have been made to separate organic matters contained in water, and researches on filters using organic matter adsorption of graphene are actively under way.

In addition, Graphene is a honeycomb-like two-dimensional planar structure interconnected in the form of hexagons. Graphene is thin, transparent, chemically stable carbon that is not visible to the naked eye. It has excellent electrical conductivity, excellent mechanical properties, and excellent organic adsorption properties.

In order to produce a filter for purifying water by using graphene, a mono-layer having a width of not less than 1 micrometer and not more than 10 centimeters by a chemical vapor deposition method (CVD) , A bi-layer or a triple-layer structure. However, both the chemical vapor deposition method and the mechanical peeling method are expensive and time consuming to manufacture the filter. There is a problem that the substrate to be used is limited.

In addition, when the graphene filter is manufactured by the chemical vapor deposition method, there is a problem that the graphene does not stably adhere to the base material (substrate), and it is difficult to control the thickness of the graphene formed on the surface of the base material, There is a problem that it is difficult to implement various types of filters because there are many restrictions on the shape and the shape of the base material.

Korean Patent Publication No. 10-2012-0022164 (Apr. 24, 2014)

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to manufacture a graphene filter for cleaning sewage water quickly and at low cost without using a chemical vapor deposition method or a mechanical peeling method.

It is an object of the present invention to provide a graphene filter capable of stably attaching graphene to a substrate having a net-like shape to prevent graphene from falling off during use of the filter.

It is another object of the present invention to produce a graphene filter for the purification of sewage water without being limited by the thickness and shape of the graphene-coated substrate.

It is also an object of the present invention to provide a graphene filter for purification of wastewater, which is equipped with the graphene filter for purification of sewage water and the graphene filter manufactured by the above-described method and has excellent water purification performance.

According to an aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: an intervening layer electrospinning step of electrospinning a surface of a substrate on which a mesh is formed, And an outermost layer coating step of coating the surface of the intervening layer with graphene after the electrospinning step to form an outermost layer.

Here, it is preferable that the substrate has a plate shape.

In addition, the interposition layer electrospinning step may include: an embedding step of embedding the substrate on the stage; a precursor storing step of storing the polymer solution; a precursor supplying step of supplying a polymer solution to the injection nozzle facing the stage; And an intervening layer coating step of injecting the precursor into the aerosol state onto the substrate by charging the polymer solution supplied to the intervening layer.

In addition, it is preferable that the intervening layer coating step is such that the injection nozzle moves in a lateral direction or a longitudinal direction of the substrate and injects the polymer solution onto the substrate.

In addition, it is preferable that the interposition layer coating step rotates the stage.

Further, it is preferable that the substrate is rolled into a cylindrical shape.

In this case, the interposition layer electrospinning step may include: an embedding step of rotating the substrate by rotating the substrate on a spindle chuck; a precursor storing step of storing the polymer solution; a precursor supplying step of supplying a polymer solution to an injection nozzle facing the substrate; And an intervening layer coating step in which the polymer solution supplied to the injection nozzle is charged to spray the polymer solution in an aerosol state onto the substrate.

In the interlayer coating step, the injection nozzle reciprocates in the axial direction of the spindle chuck and injects the polymer solution onto the substrate.

The polymer is preferably nylon 6.

In addition, the solution is preferably a formic acid.

Further, it is preferable that the polymer solution is a solution obtained by mixing nylon 6 with 15 wt% of a formic solution seed.

In the outermost layer coating step, the substrate on which the intervening layer is formed is preferably immersed in a solution containing graphene to coat the surface of the intervening layer with graphene.

At this time, it is preferable that the outermost layer coating step spray a solution containing graphene on the substrate having the intervening layer formed thereon in an aerosol state.

The graphene-containing solution is preferably a solution in which graphene is mixed with ethanol in an amount of 0.05 wt%.

According to another aspect of the present invention, there is provided a graphene filter for purifying sewage, which is manufactured by the manufacturing method described above.

According to another aspect of the present invention, there is provided a graphene filter manufactured by the manufacturing method described above, and a housing part for housing the graphene filter, A filter housing having an inlet and an outlet, and a pipe connected to an inlet and an outlet of the filter housing, respectively.

The filter housing has a housing part in which a graphene filter is mounted, a housing body in which an upper surface is opened to communicate with the housing part and an outlet is formed in the rear of the housing part, A protrusion protruding toward the inside of the housing body is formed on a lower surface of the cover so that the protrusion presses the rim of the graphene filter when the cover is coupled to the housing body .

Preferably, the outer diameter of the protrusion formed on the lower surface of the cover and the inner diameter of the housing body are threaded, respectively, so that the protrusion and the housing body are threadedly engaged.

In addition, it is preferable that o-rings are provided on the upper part and the lower part of the graphene filter mounted on the storage part, respectively.

The filter housing has a housing portion in which a graphene filter is mounted, a housing body having an inlet port and a discharge port formed on an upper surface and a lower surface of the housing portion, respectively, and a housing body formed on a side surface of the housing body, And a cover installed on a side surface of the housing body to open and close the slot.

It is also preferable that the graphene filter has an uneven protrusion formed on a rim of the graphene filter so that the graphene filter can be mounted on the receiving portion, and the uneven groove corresponding to the uneven protrusion is formed on the receiving portion.

In addition, the graphene filter water purifier may be provided in a pipe connected to an inlet of the filter housing to supply wastewater to the filter housing, and a pipe connected to the outlet of the filter housing, A detection unit which is provided in a pipe connecting the filter housing and the filtrate water storage tank to measure the degree of filtration of water having passed through the graphene filter, And a control unit for controlling a flow rate valve provided in a pipe connecting the housing and the waste water storage tank.

Preferably, the controller receives the measured data from the detection unit, and controls the water supply pump installed in the pipe connecting the waste water storage tank and the flow rate valve.

The graphene filter water purifier includes a bypass valve installed in a pipe connecting the outlet of the filter housing and the filtered water storage tank for controlling the flow of water supplied to the filtered water storage tank, And a bypass pump for supplying the water supplied to the bypass pipe to the waste water storage tank.

It is preferable that the graphene filter water purifier further includes a high voltage application unit for applying a high voltage to the graphene filter so as to remove contaminants adhered to the graphene filter.

The method of manufacturing a graphene filter for purifying sewage water according to the present invention comprises the steps of electrospinning a polymer on the surface of a substrate and coating the surface of the coated polymer with graphene to thereby produce a graphene filter quickly and inexpensively In addition, coated graphene is not easily removed, and a high-quality graphene filter can be manufactured.

In addition, since the polymer is electrospun and the graphene is coated on the polymer as described above, various types of substrates can be used without being limited by the thickness and shape of the substrate.

In addition, since the polymer and graphene coated on the substrate can be variously patterned, the graphene filter can be manufactured in accordance with the characteristics of the water treatment equipment in which the graphene filter is installed, thereby maximizing the purification capability of the graphene filter.

In addition, the graphene filter water purifier of the present invention can stably support the graphene filter to exhibit excellent water purification ability, and is easy to use because of easy mounting and separation of the graphene filter.

Further, the graphene filter water purifying device of the present invention is provided with a detection unit for measuring the degree of filtration of water having passed through the graphene filter, so that the degree of filtration of water passing through the graphene filter can be checked at all times, Is not filtered to a desired level, it can be filtered again through a graphene filter to maximize the hydrostatic capacity of the graphene filter.

1 is a flowchart showing a method of manufacturing a graphene filter for purifying sewage according to the present invention.
Fig. 2 is a flow chart showing an interlayer electrospinning step in the manufacturing method according to the present invention.
3 is a schematic view schematically showing an intervening layer electrospinning step of the present invention.
4 is a flow chart showing another embodiment of the interposition layer electrospinning step in the manufacturing method according to the present invention.
5 is a schematic view schematically showing another embodiment of the interposing layer electrospinning step.
6 is a cross-sectional view showing a graphene filter manufactured by the manufacturing method of the present invention.
FIG. 7 shows an experimental example of fabricating a graphene filter using the method of manufacturing a graphene filter according to the present invention.
FIG. 8 shows the results of confirming the ability to remove contaminants from graphene loading of the graphene filter manufactured by the experimental example.
9 is a graph showing the results of confirming the ability to remove contaminants according to the contaminant filtration rate of the graphene filter manufactured by the experimental example.
FIG. 10 is a graph showing the contaminant removal capability and the contaminant removal capability according to the contaminant filtration rate according to the graphene content of the graphene filter manufactured according to the experimental example.
11 is a sectional view showing a graphene filter purification apparatus equipped with a graphene filter manufactured by the manufacturing method of the present invention.
12 is a cross-sectional view showing another embodiment of the filter housing of the graphene filter purification apparatus of the present invention.
13 is a cross-sectional view showing another embodiment of the filter housing of the graphene filter purification apparatus of the present invention.
14 is a schematic diagram showing another embodiment of the graphene filter purification apparatus according to the present invention.
FIG. 15 shows the results of comparing the case where the high voltage is not applied and the case where the high voltage is applied according to the number of pollution filtration of the graphene filter manufactured by the experiment example.

The terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary meanings and the inventor may properly define the concept of the term to describe its invention in the best possible way And should be construed in accordance with the principles and meanings and concepts consistent with the technical idea of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

1 is a flowchart showing a method of manufacturing a graphene filter for purifying sewage according to the present invention. A method of manufacturing a graphene filter for purifying sewage water according to the present invention includes the steps of: forming an intervening layer 120 by electrospinning a solution in which a polymer is melted on a surface of a substrate 110 on which meshes are formed, After the intervening layer electrospinning step S100 and the intervening layer electrospinning step S100, the outermost layer 130 is formed by coating the surface of the intervening layer 120 with graphene, The filter 100 is fabricated.

According to this manufacturing method, since the intervening layer 120 made of polymer is formed on the surface of the substrate 110 and the graphene is attached to the surface of the intervening layer 120, The thickness of the intervening layer 120 can be controlled by the electrostatic spraying method when forming the graphene filter 120, and the desired shape of the graphene filter 100 can be quickly manufactured.

In addition, when the graphene filter 100 manufactured by the above manufacturing method is installed on a channel or a channel of a water treatment facility, organic matter suspended in the wastewater is adsorbed by the graphene filter 100 to obtain clean water from which organic matter has been removed .

In addition, the present invention can realize an intervening layer electrospinning step S100 suitable for the shape of a substrate, so that there is no limitation to the substrate 110, and the intervening layer 120 can be uniformly and stably formed on the surface of the substrate 110 So that a high-quality sewage purifying filter can be manufactured.

In addition, the substrate 110 on which the intervening layer 120 is coated is made of a conductive material such as a metal. The metal strips in the transverse direction are arranged in diagonal lines, and the longitudinal direction of the metal strips is diagonal And is formed in a planar shape in which meshes are formed by intersecting the longitudinal direction steel wires and the longitudinal direction steel wires to form a skeleton capable of supporting the interposition layer 120 and the outermost layer 130. [

Particularly, the substrate 110 is formed so as to intersect the longitudinal direction steel strips and the longitudinal direction stripes, thereby forming a gap through which water can permeate between the longitudinal direction stripes and the longitudinal direction stripes. The overall shape of the substrate 110 may be rectangular or rectangular as shown in FIG. 3. However, the substrate 110 may be variously modified.

For example, the substrate 110 in the form of a plate may have a circular or polygonal shape, and the shape of the substrate 110 may have various shapes depending on a water treatment facility in which the graphene filter of the present invention is installed.

Meanwhile, as described above, when the substrate 110 has a flat shape, an intervening layer electrospinning step S100 is performed in which the substrate 110 is placed on the stage and the polymer is coated on the surface of the substrate.

Intervening layer  Electrospinning 1st Example

Figs. 2 and 3 are a sequence diagram and a schematic diagram showing an intervening layer electrospinning step in the case where the substrate has a flat shape.

3, when the substrate 110 has the shape of a plate as shown in FIG. 3, a step S110a of placing the substrate 110 on the stage 10, a step S110a of storing a precursor A precursor supplying step S130a for supplying the polymer solution to the injection nozzle 210 toward the stage 10; a step for charging the polymer solution supplied to the injection nozzle 210 by spraying the polymer solution in an aerosol state (S100) consisting of an intervening layer coating step (S140a) for spraying the intervening layer onto the substrate (110).

The interlayer layer electrospinning step S100 in which the polymer is coated on the surface of the substrate 110 is performed in the electrostatic spraying apparatus 200 as shown in FIG. The electrostatic spraying apparatus 200 includes a stage 10 on which a substrate 110 is placed, a spray nozzle 210 for spraying the polymer solution onto the substrate, a precursor supply device 220 for supplying the polymer solution to the spray nozzle, And a high voltage application device 230 for charging the battery.

Here, the electrostatic spraying apparatus 200 supplies the polymer solution to the injection nozzle 210 at a flow rate of about 10 ml / hr through the precursor supply device 220, and the polymer solution passes through the injection nozzle 210, The charged polymer is injected toward the substrate 110 placed on the stage 10 in a state of being charged by the charging unit 230 and the charged polymer is atomized by the electrostatic attraction between the injection nozzle 210 and the substrate 110, 110).

The placing step S110a is a step of putting the substrate 110 to be the skeleton of the graphene filter 100 on the stage 10 and fixing the substrate 110 on the stage 10 on which the flat surface is formed do. At this time, a separate holder may be further provided on the stage 10 to prevent the substrate 110 from moving.

The precursor storage step S120a is a step of storing the polymer solution to form the intervening layer 120. The polymer solution is stored in the precursor supply device 220 connected to the injection nozzle 210 through a flow path. The precursor supply device 220 is formed in the form of a container for storing the polymer solution, and a supply hose is formed on one side so that the polymer solution can be supplied to the injection nozzle 210.

The precursor supplying step S130a supplies the polymer solution to the injection nozzle 210 directed to the stage 10 and then the polymer solution supplied to the injection nozzle 210 through the intervening layer coating step S140a is charged So that the polymer solution is sprayed onto the substrate 110 in an aerosol state.

The injection nozzle 210 receives the polymer solution from the precursor supplying device 220 and injects the polymer solution into the substrate 110 placed on the stage 10 in an aerosol state. And a nozzle block coupled to one end of the nozzle case.

At the end of the nozzle block, a fine nozzle hole is formed, through which the polymer solution is injected. The nozzle block may be formed in a cone shape or in various other shapes.

In addition, when the polymer solution is injected onto the substrate 110 through the injection nozzle 210 in the intervening layer coating step S140a, the injection nozzle 210 is moved in the lateral direction or the longitudinal direction of the substrate 110 to be jetted , The polymer may be uniformly sprayed over the entire surface of the substrate 110, or an intervening layer 120 of a polymer having a specific pattern may be formed.

In some cases, the polymer may be attached to the substrate 110 in a curved pattern by spraying a polymer solution onto the rotating substrate 110 by rotating the stage 10 on which the substrate 110 is placed .

A rotary shaft 12 is integrally formed with the stage 10 at a lower portion of the stage 10 and the rotary shaft 12 is mechanically connected to a driving motor so that the stage 10, The polymer solution is sprayed onto the substrate 110 while the substrate 110 rotates.

As the substrate 110 rotates and the polymer solution is injected while the injection nozzle 210 moves in the transverse direction or longitudinal direction of the substrate 110, the polymer is intensively coated on any part of the substrate 110 The thickness of the intervening layer 120 can be controlled, and the graphene filter 100 can be manufactured in accordance with the characteristics of the water treatment facility.

For example, in order to manufacture a graphene filter having a thicker thickness toward the outer side of the substrate 110, the injection nozzle 210 repeatedly moves along the outer edge of the substrate 110, The thickness of the interlayer 120 may be increased toward the outside of the interlayer 120.

The polymer solution injected from the injection nozzle 210 is applied in the form of a thin film on the surface of the substrate 110. The polymer solution is injected through the high voltage application device 230 during the injection through the injection nozzle 210 And the substrate 110 is configured to be grounded via a separate ground terminal 240 so that the charged polymer is adhered to the substrate 110 by an electrostatic attracting force.

At this time, since the substrate 110 is grounded through the ground terminal 240, the charged polymer is easily attached to the surface of the substrate 110 by the electrostatic attracting force. For example, when the polymer is charged to the positive (+) side by the high voltage application device 230, the substrate connected to the ground terminal 240 acts as the negative (-), so that the positively charged polymer is electrostatically Is attached to the surface of the substrate (110) by attraction, and the charge charged on the polymer after it is attached is entirely discharged through the ground terminal (240).

Intervening layer  Electrospinning Second Example

On the other hand, if the substrate 110 has a cylindrical shape, the intervening layer electrospinning step S100 is performed while the substrate 110 is rotated by the spindle chuck 250. [ Figs. 4 and 5 are a sequence diagram and a schematic diagram showing an intervening layer electrospinning step in the case where the substrate has a shape in which the substrate is rolled in the shape of a cylinder.

5, in the case where the substrate 110 has a shape of a cylindrical shape as shown in FIG. 5, the positioning step S110b for rotating the substrate 110 by the spindle chuck 250, A precursor storing step S120b for storing the solution, a precursor supplying step S130b for supplying the polymer solution to the injection nozzle 210 facing the substrate 110, a step of charging the polymer solution supplied to the injection nozzle to form a polymer solution in an aerosol state And an intervening layer coating step (S140b) for spraying the intervening layer onto the substrate is carried out.

5, the intervening layer electrospinning step S100, in which the polymer is coated on the substrate 110 having a cylindrical shape in the shape of a cylinder, is performed by the electrostatic spraying apparatus 200 provided with the spindle chuck 250, Lt; / RTI >

The electrostatic spraying apparatus 200 used in the second embodiment of the interlayer electrospinning step S100 is similar to the electrostatic spraying apparatus of the first embodiment of the intervening layer electrospinning step described above, but instead of the stage 10, 110 are rotated by the spindle chuck 250 and the precursor storage step S 120 b and the precursor supply step S 130 b are performed in this state.

After the precursor supply step (S130b), an intervening layer coating step (S140b) is performed in which the polymer solution supplied to the injection nozzle (210) is charged to spray the polymer solution in an aerosol state onto the substrate (110).

At this time, the interlayer coating step (S140b) preferably uniformly injects the polymer over the entire surface of the substrate 110 by spraying the polymer solution onto the substrate, and the injection nozzle 210 is preferably reciprocated in the axial direction of the spindle chuck 250 Or an intervening layer 120 made of a polymer having a specific pattern can be formed.

Meanwhile, the polymer solution used in the first and second embodiments of the above-described interposition layer electrospinning step (S100) is a solution prepared by mixing 15 wt% of nylon 6 with formic acid.

Accordingly, the polymer solution injected onto the substrate 110 through the injection nozzle 210 easily transports the nylon 6 from the precursor supply device 220 to the injection nozzle 210 due to the physical properties of the formic liquid seed, In the course of spraying the solution from the injection nozzle 210 onto the substrate 110, the formic solution seed is volatilized and the nylon 6 is attached to the surface of the substrate.

After the intervening layer electrospinning step S100 of forming the intervening layer 120 of polymer on the surface of the substrate 110 is performed as described above, the outermost layer 130 of graphene is formed on the surface of the intervening layer 120 The outermost layer coating step S200 is performed.

The outermost layer 130 formed on the surface of the intervening layer 120 is made of graphene. The graphene is a material having a honeycomb-like two-dimensional planar structure, Is very thin and transparent, has excellent electrical conductivity and strength equivalent to 200 times that of steel.

Further, since the graphene has excellent permeability to water, if the outermost layer 130 and the interstitial layer 120 made of graphene and polymer are formed on the surface of the substrate, the organic matter contained in the wastewater is quickly adsorbed, The organic matter contained therein can be quickly removed and purified.

At this time, the outermost layer coating step (S200) may include coating the surface of the intervening layer 120 with graphene by immersing the substrate 110 having the intervening layer 120 formed thereon in the solution containing graphene, A solution containing graphene is sprayed on the substrate 110 in the form of an aerosol to coat the graphene. Here, the solution containing graphene may be a solution obtained by mixing 0.05 wt% of graphene with ethanol.

In the graphene coating by immersion, the graphene-containing solution is filled in a container such as a water tank, the substrate 110 on which the intervening layer 120 is formed is immersed in the solution, and graphening is performed on the surface of the intervening layer 120 . The graphene coating due to such immersion can uniformly distribute the graphenes over the entire surface of the intervening layer 120.

The precursor supplying device 220 may be filled with a solution containing graphene and may be injected through the injection nozzle 210 into the intervening layer 120 And the outermost layer 130 is formed.

The graphene coating by this spraying is not only enhanced by the graphening of the graphene layer 120 due to the jetting speed of graphene, but also the adhesion of graphene to a specific region of the interlayer 120, The coating thickness of the fin can be controlled.

Accordingly, when the outermost layer coating step S200 is completed as described above, the graphene filter 100 as shown in FIG. 6 can be manufactured.

Grapina  Manufacture of filters Experimental Example

FIG. 7 shows an experimental example of fabricating a graphene filter using the method of manufacturing a graphene filter according to the present invention.

Specifically, in the experimental example shown in FIG. 7, an electrospinning step is carried out by using a polymer solution prepared by mixing 15 wt% of nylon 6 with a formic solution seed, as shown in FIGS. 2 and 3, Layer was formed, and then a solution of 0.05 wt% of graphene in ethanol was coated to form the outermost layer. When graphene mixed solution is coated on the intercalation layer, graphene is impregnated between the nylon 6 nanofibers.

Fig. 7 (b) shows the change in diameter of the electrospun nylon 6, and d shows the Raman spectrum analysis result of the produced graphene filter. Referring to the graph shown in FIG. 11D, D, G and 2D peaks in which graphene is commonly found can be confirmed.

FIG. 8 shows the results of confirming the ability to remove contaminants from graphene loading of the graphene filter manufactured by the experimental example. Here, the MB (methylene blue) solution was used as a contaminant, and the concentration of the MB solution was 1 ppm and the filtration rate was 1.0 mL / min. The decontamination ability of the graphene filter was confirmed by the absorbance value of the filtered MB solution. That is, the lower the absorbance, the higher the ability to remove contaminants.

8, the graphene content was 0.388 mg / cm < 2 > , It is possible to confirm that the pollutant removing ability of 100% is exhibited.

9 is a graph showing the results of confirming the ability to remove contaminants according to the contaminant filtration rate of the graphene filter manufactured by the experimental example. Here, the graphene content of the graphene filter was fixed at 0.388 mg / cm 2 .

The results of FIG. 9 show that the filtration rate of the MB solution showed 100% contaminant removal ability at 1.0 mL / min, but that the contaminant removal capability was lowered after 1.5 filtration rate.

8 and 9, it is necessary to set the graphene content of the graphene filter to 0.388 mg / cm 2 or more and the contaminant filtration rate to be 1.0 mL / min in order for the graphene filter to exhibit the best contaminant removing ability .

FIG. 10 is a graph showing the contaminant removal capability and the contaminant removal capability according to the contaminant filtration rate according to the graphene content of the graphene filter manufactured according to the experimental example.

Meanwhile, the graphene filter 100 manufactured by the above-described manufacturing method is installed on a channel or a channel of a water treatment facility. To this end, the graphene filter 100 of the present invention is installed in a graphene filter water purifier and exhibits excellent water purification performance. Such graphene filter purification apparatus will be described with reference to Figs. 11 to 14. Fig.

11 is a sectional view showing a graphene filter purification apparatus equipped with a graphene filter manufactured by the manufacturing method of the present invention. Referring to the drawings, the graphene filter water purifier according to the present invention includes a graphene filter 100 manufactured by the manufacturing method described above, a filter housing 300 to which the graphene filter 100 is mounted, And a pipe 400 for guiding to the housing 300 and draining purified water.

The filter housing 300 has a shape of a hollow tube and a housing part 301 in which the graphene filter 100 is mounted is formed inside the filter housing 300. The housing part 301 is formed in the filter housing 300, The graphene filter 100 is positioned on the filter housing 300 and all the wastewater passing through the flow path of the filter housing 300 is formed in a recessed shape along the inner circumference of the filter housing 300 so as to pass through the graphene filter 100, The graphene filter 100 having a size that fits the diameter of the storage portion 301 is mounted on the storage portion 301.

An inlet port 302 through which wastewater flows is formed at one side of the filter housing 300 with respect to the storage section 301 and an outlet port 303 for discharging the filtered water through the graphene filter 100 Is formed. A pipe 400 is formed in the inlet 302 and the outlet 303 of the filter housing 300 so that the wastewater is purified through the graphene filter 100 and drained. At this time, the inlet 302 and the outlet 303 are connected to the pipe 400 by flange connection, respectively.

Meanwhile, since the filter housing 300 on which the graphene filter 100 is mounted is separated, the mounting of the graphene filter 100 can be performed more conveniently. This will be described with reference to FIG.

12 is a cross-sectional view showing another embodiment of the filter housing of the graphene filter purification apparatus of the present invention. Referring to the drawings, the filter housing 300 according to another embodiment includes a filter housing 300 in a separated structure so that the graphene filter 100 can be easily attached or detached.

The filter housing 300 is formed of a housing body 310 and a cover 320. The housing body 310 has a receiving portion 301 in which a graphene filter 100 is mounted And the discharge port 303 is formed in the rear of the storage unit 301. The discharge port 303 is connected to the discharge port 301,

The cover 320 is formed on the upper surface of the housing body 310 and has an inlet 302 formed on the upper surface thereof. Particularly, the cover 320 has a protrusion 321 protruding toward the inside of the housing body 310. When the cover 320 is coupled to the housing body 310, the protrusion 321 is connected to the graphene filter 100 are clamped to fix the graphene filter 100.

Although it has been described in the foregoing description that the discharge port 303 is formed at the rear of the housing body 310 and the inlet port 302 is formed at the cover 320, the inlet port 302 may be formed at the rear of the housing body 310 302 may be formed on the cover 320 and a discharge port 303 may be formed on the cover 320.

The outer diameter of the protrusion 321 formed on the cover 320 and the inner diameter of the upper surface of the housing body 310 are threaded so that the protrusion 321 and the housing body 310 are thread- And the housing body 310 are convenient. An o-ring (not shown) is interposed between the protrusion 321 and the housing body 310 to prevent leakage of water from the contact surface between the cover 320 and the housing body 310 when the protrusion 321 and the housing body 310 are coupled by a thread.

When the cover 320 and the housing body 310 are combined with each other, the gap between the cover 320 and the housing body 310 is filled with the protrusion 321 so that the protrusion 321 can suppress the graphene filter 100 An O-ring 330 is interposed between the upper part and the lower part of the graphene filter 100 mounted on the storage part 301 to prevent leakage of water to the filter housing 300.

A slot 304 may be formed in the filter housing 300 so that the graphene filter 100 can be easily attached and detached from the receiving portion 301 of the filter housing 300. This will be described with reference to FIG.

13 is a cross-sectional view showing another embodiment of the filter housing of the graphene filter purification apparatus of the present invention. The filter housing 300 according to another embodiment of the present invention includes a housing part 301 in which a graphene filter 100 is mounted, And a slot 304 formed in a side surface of the housing body 310 and communicating with the housing part 301 to receive and receive the graphene filter 100. The housing body 310 has an inlet 302 and an outlet 303, .

A lid 305 is provided on the side surface of the housing body 310 to open and close the slot 304. The lid 305 is fastened to the housing body 310 by bolts to tighten or loosen the bolts, The lid 305 is detached from the body 310 and then the graphene filter 100 is attached to or detached from the storage unit 301.

At this time, a sealing member (not shown) such as a gasket is provided between the lid 305 and the housing body 310 to prevent leakage from the contact surface between the lid 305 and the housing body 310.

As described above, when the slot 304 communicating with the housing part 301 is formed on the side surface of the housing body 310 and the slot 304 is closed by the lid 305, the lid 305 The graphene filter 100 can be easily attached and detached.

Meanwhile, as described above, the degree of filtration of the filtered water passing through the filter housing 300 to which the graphene filter 100 is attached is measured, and the filter housing 300 The detection unit 700 may be installed in the pipe 400 connected to the detection unit 700. This will be described with reference to FIG.

14 is a schematic diagram showing another embodiment of the graphene filter purification apparatus according to the present invention. The graphene filter water purifier installed with the detection unit 700 includes a wastewater storage tank 500 for storing wastewater and supplying the wastewater to the filter housing 300, water purified through the filter housing 300, A detection unit 700 for detecting the degree of filtration of water that has passed through the graphene filter 100 of the filter housing 300 and a sensor unit 700 for receiving data measured from the detection unit 700, A control unit 800 for controlling the flow rate of the wastewater to be supplied to the graphene filter 300, and a high voltage applying unit 900 for applying a high voltage to the graphene filter 100.

In addition, the waste water storage tank 500 is provided in the pipe 400 connected to the inlet of the filter housing 300 to supply the filter housing 300 with wastewater. A flow valve 410 for controlling the flow rate of the wastewater to be supplied to the filter housing 300 is installed in the pipe 400 connecting the wastewater storage tank 500 and the filter housing 300.

The filtered water storage tank 600 is connected to a pipe 400 connected to the discharge port 303 of the filter housing 300 and stores purified water through the graphene filter 100 installed in the filter housing 300 do.

A detection unit 700 for measuring the degree of filtration of water having passed through the graphene filter 100 is installed in the pipe 400 connecting the filtration water storage tank 600 and the filter housing 300. 700 are configured to measure the degree of inclusion of organic matter per unit area of water passing through the pipe 400 connecting the filter housing 300 and the filtered water storage tank 600.

The detection unit 700 is a device for quantitatively analyzing and irradiating light to the inside of the pipe 400 connecting the filter housing 300 and the filtering water storage tank 600, Lt; / RTI >

The detection unit 700 for measuring the degree of filtration of water that has passed through the graphene filter 100 of the filter housing 300 includes a pipe 400 connecting the wastewater storage tank 500 and the filter housing 300, And the data measured from the detection unit 700 are provided to the control unit 800 and are electrically connected to the filter housing 800 in the waste water storage tank 500 according to the measured result. The flow rate of the wastewater to be supplied to the discharge pipe 300 is controlled.

The control unit 800 may further include a storage unit for storing the data measured by the detection unit 700 in units of time. The storage unit may process the data measured by the detection unit 700 and provide the data to the control unit 800 It is possible to know the change in the water purification ability of the graphene filter 100 with time and predict the replacement time of the graphene filter 100 or the like.

A water supply pump 420 is installed in the pipe 400 connecting the wastewater storage tank 500 and the flow valve 410. The water supply pump 420 is electrically connected to the control unit 800, It is possible to control the flow rate of the wastewater fed from the filter housing 500 to the filter housing 300.

That is, even if the flow rate of the wastewater to be supplied to the filter housing 300 through the flow valve 410 is controlled to be constant, the hydrostatic capacity of the graphene filter 100 may be changed as the flow velocity is increased or decreased.

The control unit 800 controls the water pump 420 to control the flow rate of the wastewater to be supplied to the graphene filter 100 so that the graphene filter 100 ) Can be maximized.

Meanwhile, the graphene filter water purifying device according to the present invention may pass the graphene filter 100 through the graphene filter 100, and if the filtered wastewater is not filtered to a desired degree, the wastewater may be purified to an appropriate level .

For this purpose, the graphene filter water purifier is provided with a bypass valve 430, a bypass pipe 440, and a recovery pump 450. The bypass valve 430 is installed in the pipe 400 connecting the filter housing 300 and the filtered water storage tank 600 to control the flow of water supplied to the filtered water storage tank 600.

The bypass pipe 440 is branched from the bypass valve 430 and is connected to the waste water storage tank 500 to block the water that has passed through the graphene filter 100 from being supplied to the filtered water storage tank 600 The water that has passed through the graphene filter is supplied to the waste water storage tank 500. The recovery pump 450 is installed in the bypass pipe 440 connecting the bypass valve 430 and the waste water storage tank 500 to discharge the water bypassing the bypass pipe 440 to the waste water storage tank 500. [ .

At this time, the bypass valve 430 and the recovery pump 450 are electrically connected to the control unit 800 described above, and the operation of the bypass valve 430 and the recovery pump 450 is controlled by the control unit 800, It is possible to reprocess it and purify the sewage to an appropriate level.

In the graphene filter water purifier of the present invention, the organic matter contained in the wastewater is adsorbed and filtered by the graphene filter 100, so that the organic matter contained in the wastewater can be removed.

The filtered water is filtered through the graphene filter 100 and the organics are removed from the filtration unit 700. If the wastewater is not filtered to a desired level, So that the water of appropriate quality can be obtained.

In filtering the wastewater by using the graphene filter 100, the contaminant removing capability of the graphene filter 100 is lowered when the number of times of removing the pollutant increases. In order to solve such a problem, a high voltage applying unit 900 applies a high voltage to the graphene filter 100. FIG. When the high voltage application unit 900 applies a high voltage to the graphene filter 100, it is possible to remove contaminants that are trapped between the graphene filter 100, thereby increasing the number of filtration of the graphene filter 100 The contaminant removing capability of the graphene filter 100 can be restored. The operation of the high-voltage applying unit 900 is controlled by the control unit 800. [ The control unit 800 can confirm the change in the water purification capability of the graphene filter 100 from the measured data of the detection unit 700 so that the high voltage application unit 900 can apply a high voltage to the graphene filter 100 at a proper time Let's do it.

FIG. 15 shows the results of comparing the case where the high voltage is not applied and the case where the high voltage is applied according to the number of pollution filtration of the graphene filter manufactured by the experiment example.

15, when the number of contaminant filtration increases, the contaminant removal capability of the graphene filter is lowered. However, if a high voltage (HV) is applied to the graphene filter, the degree of degradation of the contaminant removal capability of the graphene filter can be reduced Able to know. This is because applying a high voltage to the graphene filter can remove pollutants that are trapped between the graphene filters, thereby recovering the ability of the graphene filter to remove contaminants to some extent.

While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. .

For example, when the graphene filter 100 mounted on the housing part 301 of the filter housing 300 is mounted on the housing part 301, the wastewater supplied through the inlet 302 of the filter housing 300 And the graphene filter 100 is mounted on the housing part 301 of the filter housing 300 so that the pattern position of the outermost layer 130 formed on the graphene filter 100 is not arbitrarily changed. May be mounted with directionality.

13, the recessed protrusions 112 are formed on the rim of the graphene filter 100 and the recessed grooves 306 are formed in the storage portion 301 to match the recessed protrusions 112 do. That is, when the graphene filter 100 is formed of a disc as shown in FIG. 13, the concave and convex protrusions 112 are formed on the four sides of the graphene filter 100.

A recessed groove 306 is formed in the inner diameter of the accommodating portion 301 so as to correspond to the recessed and protruded projections 112 of the graphene filter 100, And is mounted to the storage portion 301. Accordingly, even if the wastewater passes through the graphene filter 100, the graphene filter 100 can be prevented from being damaged even if the uneven protrusion 112 formed on the graphene filter 100 is fitted into the uneven groove 306 of the receiving portion 301. [ So that the organic matter contained in the wastewater can be stably trapped and purified.

The concavity and convexity protrusion 112 and the protrusive groove 306 are not formed only in the filter housing 300 and the graphene filter 100 of FIG. 13 in the foregoing description, As shown in FIG.

10: stage 12:
100: Graphene filter 110: substrate
112: protrusion protrusion 120:
130: Outer layer 200: Electrostatic spray device
210: injection nozzle 220: precursor supply device
230: high voltage applying device 240: ground terminal
250: spindle chuck 300: filter housing
301: storage part 302: inlet
303: Outlet 304: Slot
305: cover 306: uneven groove
310: housing body 320: cover
321: protrusion 330: O-ring
400: Piping 410: Flow valve
420: Feed water pump 430: Bypass valve
440: Bypass piping 450: Return pump
500: Wastewater storage tank 600: Filtered water storage tank
700: Detection unit 800:
900: High voltage application part

Claims (25)

An intervening layer electrospinning step of forming an intervening layer by electrospinning a solution in which a polymer is melted on a surface of a substrate on which a mesh is formed by crossing a metal strip;
And an outermost layer coating step of coating the surface of the intervening layer with graphene to form an outermost layer after the intervening layer electrospinning step. The method according to claim 1,
Wherein the substrate has a shape of a plate. 3. The method according to claim 1 or 2,
Wherein the interlayer layer electrospinning step comprises:
An anchoring step of placing the substrate on a stage;
A precursor storage step of storing the polymer solution;
A precursor supplying step of supplying a polymer solution to an injection nozzle facing the stage; And
And an intervening layer coating step of spraying the precursor on the substrate in an aerosol state by charging the polymer solution supplied to the injection nozzle. The method of claim 3,
Wherein the interlayer coating step comprises:
Wherein the spray nozzle moves in a transverse direction or a longitudinal direction of the substrate and injects the polymer solution onto the substrate. The method of claim 3,
Wherein the interlayer coating step comprises:
And the stage is rotated. The method according to claim 1,
Wherein the substrate is rolled into a cylindrical shape. 7. The method according to claim 1 or 6,
Wherein the interlayer layer electrospinning step comprises:
An anchoring step of engaging the substrate with the spindle chuck to rotate the substrate;
A precursor storage step of storing the polymer solution;
A precursor supplying step of supplying a polymer solution to an injection nozzle facing the substrate; And
And an intervening layer coating step of spraying the polymer solution on the substrate in an aerosol state by charging the polymer solution supplied to the injection nozzle. 8. The method of claim 7,
Wherein the interlayer coating step comprises:
Wherein the injection nozzle reciprocates in the axial direction of the spindle chuck and injects the polymer solution onto the substrate. The method according to claim 1,
Wherein the polymer is nylon 6. ≪ RTI ID = 0.0 > 8. < / RTI > The method according to claim 1,
Wherein the solution is a formic acid. ≪ RTI ID = 0.0 > 15. < / RTI > 11. The method according to claim 9 or 10,
Wherein the polymer solution is a solution obtained by mixing 15 wt% Nylon 6 with a formic solution seed. The method according to claim 1,
Wherein the outermost layer coating step comprises:
Wherein the substrate on which the intervening layer is formed is immersed in a solution containing graphene to coat the surface of the intervening layer with graphene. The method according to claim 1,
Wherein the outermost layer coating step comprises:
And spraying the graphene-containing solution onto the substrate having the intervening layer formed thereon in an aerosol state. The method according to any one of claims 1, 12 and 13,
Wherein the graphene-containing solution is a solution obtained by mixing 0.05wt% of graphene with ethanol. A graphene filter for sewage treatment, which is produced by at least one of claims 1 to 14. A graphene filter manufactured by at least one of claims 1 to 14;
A filter housing having a housing part for housing the graphene filter therein and having an inlet and an outlet formed around the housing part; And
And a pipe connected to an inlet and an outlet of the filter housing, respectively. 17. The method of claim 16,
The filter housing includes:
A housing body in which a housing part for mounting a graphene filter is formed, a housing body having an upper surface opened to communicate with the housing part and an outlet port formed behind the housing part; And
And a cover formed on the upper surface of the housing body and having an inlet formed on an upper surface thereof,
Wherein a protrusion protruding toward the inside of the housing body is formed on a lower surface of the cover so that the protrusion presses the rim of the graphene filter when the cover is coupled to the housing body. 18. The method of claim 17,
Wherein a thread is formed in an outer diameter of a protrusion formed on a lower surface of the cover and an inner diameter of the housing body, respectively, so that the protrusion and the housing body are threadedly engaged. The method according to claim 17 or 18,
And an o-ring is provided on an upper portion and a lower portion of the graphene filter mounted on the storage portion, respectively. 17. The method of claim 16,
The filter housing includes:
A housing body in which a housing part for mounting a graphene filter is formed, a housing body having an inlet port and an outlet port formed on an upper surface and a lower surface of the housing part, respectively;
A slot formed on a side surface of the housing body and communicating with the accommodating portion to allow the graphene filter to enter and exit; And
And a cover installed on a side surface of the housing body to open and close the slot. 21. The method according to claim 17 or 20,
Wherein the graphene filter has an uneven protrusion formed on a rim of the graphene filter so that the graphene filter can be oriented and mounted on a receiving part, Device. 17. The method of claim 16,
The graphene filter water purifier device,
A waste water storage tank provided in a pipe connected to an inlet of the filter housing to supply wastewater to the filter housing;
A filtered water storage tank provided in a pipe connected to an outlet of the filter housing and storing the filtered water through the graphene filter;
A detection unit provided in a pipe connecting the filter housing and the filtered water storage tank to measure the degree of filtration of water having passed through the graphene filter; And
And a control unit for receiving the measured data from the detection unit and controlling a flow rate valve installed in a pipe connecting the filter housing and the waste water storage tank. 23. The method of claim 22,
Wherein,
Wherein the control unit controls the water supply pump installed in the pipe for receiving the measured data from the detection unit and connecting the waste water storage tank and the flow rate valve. 23. The method of claim 22,
The graphene filter water purifier
A bypass valve installed in a pipe connecting the outlet of the filter housing and the filtered water storage tank for controlling the flow of water supplied to the filtered water storage tank;
A bypass pipe connecting the bypass valve and the waste water storage tank; And
And a bypass pump for supplying the water supplied to the bypass pipe to the waste water storage tank. 17. The method of claim 16,
Further comprising a high voltage application unit for applying a high voltage to the graphene filter so as to remove contaminants adhered to the graphene filter.
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