CN116726703A - Method for concentrating water-soluble graphene slurry based on ceramic membrane method - Google Patents
Method for concentrating water-soluble graphene slurry based on ceramic membrane method Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 60
- 239000002002 slurry Substances 0.000 title claims abstract description 56
- 239000012528 membrane Substances 0.000 title claims abstract description 53
- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 238000005406 washing Methods 0.000 claims abstract description 21
- 230000004907 flux Effects 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000012141 concentrate Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000003921 particle size analysis Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009295 crossflow filtration Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/28—Solid content in solvents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Water Supply & Treatment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a method for concentrating water-soluble graphene slurry based on a ceramic membrane method. The method provided by the invention effectively reduces the process energy consumption of the concentrated water-soluble graphene slurry, improves the production efficiency, further reduces the production cost, widens the application market of graphene products, and is suitable for industrial and continuous production. Meanwhile, the SiC ceramic membrane polluted in the concentration process can be completely recovered in flux through acid washing, and can stably run for a long time.
Description
Technical Field
The invention belongs to the technical field of graphene material preparation, and particularly relates to a method for concentrating water-soluble graphene slurry based on a ceramic membrane method.
Background
Graphene has excellent conductivity, strong mechanical properties and excellent light transmittance, and is widely applied to the electronic and energy industries. At present, the domestic graphene production technology is mainly an oxidation-reduction method, the production cost of the method is high, the quality of the prepared graphene product is low, and the quality is difficult to control; and the aqueous phase physical stripping method can be used for producing graphene products in a large scale and at low cost. However, the graphene slurry prepared by the method has the problem of low solid content, so that the concentration of the slurry product cannot be further improved, the production period of the subsequent powder product is long, and the energy consumption is high. On the other hand, graphene does not have oxygen-containing functional groups, so that the graphene is difficult to dissolve and disperse in water, and the water-soluble graphene takes pure water as a dispersing solvent, so that the difficulty of dispersing and concentrating is further increased. The traditional slurry solid-liquid separation technology such as a vacuum leaf filtration technology and a diaphragm filter pressing technology has the problems of low solid-liquid separation efficiency, low automation degree, repeated loading, unloading and cleaning, serious powder loss and the like. Therefore, the selection of a new process is important for efficient concentration of graphene in the liquid phase.
The ceramic membrane is a membrane which is paid attention to at present and has application prospect, has high hydrophilicity and stable property, and simultaneously has the characteristics of high temperature resistance, acid and alkali corrosion resistance, microbial corrosion resistance and the like. When the ceramic membrane is used for concentrating and washing the powder, a filter cake is not formed, and the production efficiency is high. In addition, the inorganic ceramic film has the following advantages: (1) cross-flow filtration, continuous concentration and large flux; (2) The pore diameter of the membrane is asymmetrically distributed, the attenuation is slow, and the long-term stable high-flux filtration can be maintained; (3) The membrane material and the auxiliary equipment material are pollution-free materials, and are resistant to microbial corrosion and high temperature; (4) the membrane element has excellent acid and alkali resistance and long service life; (5) Full-automatic control, simple operation, easy cleaning and maintenance.
Therefore, the method for concentrating the water-soluble graphene slurry based on the ceramic membrane method can efficiently obtain stable concentrated graphene slurry taking pure water as a solvent through a simple process, and has positive significance in further promoting the development of the graphene industry.
Disclosure of Invention
(one) solving the technical problems
The graphene slurry prepared by stripping by the existing pure water phase method has the key problems of difficult solid-liquid separation, concentration and dehydration, low production efficiency and high energy consumption of the follow-up slurry product and the follow-up dried powder product, and therefore, the ceramic membrane method is adopted, and the advantages of the method are applied: the SiC ceramic membrane material and the technology have the advantages of selectable pore diameter, selectable configuration, high mechanical strength and pollution resistance, so as to solve the technical problems.
(II) technical scheme
The invention aims to provide a method for concentrating water-soluble graphene slurry based on a ceramic membrane method, which can efficiently obtain stable concentrated graphene slurry taking pure water as a solvent through a simple process.
The method comprises the following steps that a feeding pump pumps low-concentration water-soluble graphene slurry into ceramic membrane equipment in a pressure driving mode, and then solid-liquid separation is carried out on the low-concentration water-soluble graphene slurry, so that high-concentration water-soluble graphene slurry is obtained; and finally, the flux of the polluted SiC ceramic membrane is completely recovered by acid washing, and the polluted SiC ceramic membrane can be recycled.
The low-concentration water-soluble graphene slurry is prepared by stripping the graphene slurry by a pure water phase method, and the concentration of the slurry after homogenization is 0.5wt%.
The ceramic membrane adopts a multichannel tubular SiC ceramic membrane, the average pore diameter is adjustable between 100 and 500nm, and the length is 1200mm.
The acid washing solution is 0.5 to 1 percent of citric acid aqueous solution or 0.5 to 1 percent of HNO 3 An aqueous solution.
The method for concentrating the water-soluble graphene slurry based on the ceramic membrane method specifically comprises the following steps of:
1) Adding the homogenized low-concentration water-soluble graphene slurry into a feed tank;
2) Starting a feed valve, starting a feed pump, pumping low-concentration water-soluble graphene slurry into ceramic membrane equipment, and adjusting the membrane-entering pressure and the operating temperature;
3) When the membrane filtration reaches a preset concentration multiple, closing a feed pump, and opening a valve to obtain high-concentration water-soluble graphene slurry;
4) And adding an acid washing solution into the feed tank, starting the feed pump, carrying out acid washing, controlling the washing time and the washing temperature, discharging the cleaning liquid after the end, adding pure water to wash until the pH value is neutral, and closing the feed pump.
Further, the homogenized low-concentration graphene slurry in the step 1) is 30-50 kg.
Further, the film-entering pressure in the step 2) is 0.05-0.15 MPa of normal operation pressure, and the operation temperature is 20-25 ℃.
Further, the acid washing solution in the step 4) is 1% citric acid aqueous solution, the dosage is 10-30L, the washing time is 20-40 min, and the washing temperature is 60-80 ℃.
(III) beneficial effects
The method for concentrating the water-soluble graphene slurry based on the ceramic membrane method has the advantages that the core of dehydration concentration of the graphene slurry is solid-liquid separation, and compared with the traditional slurry solid-liquid separation process, the method adopts the ceramic membrane method, has high degree of automation, is simple to operate and can be repeatedly used, a filter cake is not formed when the ceramic membrane is used for concentrating and washing the powder, the production efficiency is high, and the efficiency and the energy consumption performance of a water-soluble graphene slurry concentrating link are greatly improved.
According to the method for concentrating the water-soluble graphene slurry based on the ceramic membrane method, according to the calculation of 2000 tons of water-soluble graphene slurry produced in one year, the production cost of enterprises is expected to be reduced by 20 ten thousand yuan/year, the income is increased by 150 ten thousand yuan/year, and new power is injected for the development of the graphene industry.
Drawings
FIG. 1 is a schematic flow chart of a method for concentrating water-soluble graphene slurry based on a ceramic membrane method;
fig. 2 is a graph showing the concentration effect of the graphene slurry obtained in example 1 of the present invention;
FIG. 3 is a graph showing the particle size distribution of graphene obtained in example 1 of the present invention;
fig. 4 is a scanning electron microscope image of graphene obtained in embodiment 1 of the present invention;
FIG. 5 is a transmission electron microscope image of graphene obtained in example 1 of the present invention;
fig. 6 is an atomic force microscope image of graphene obtained in example 1 of the present invention, where (a) is a 2D image and (b) is a 3D image.
Detailed Description
The following examples are illustrative of the invention and are not intended to limit the scope of the invention. The reagents used were not manufacturer-noted and were all conventional products available for purchase by regular channel suppliers.
Example 1
As shown in fig. 1, the method for concentrating the water-soluble graphene slurry based on the ceramic membrane method comprises the following specific steps:
concentrating graphene slurry by adopting a SiC ceramic membrane, wherein the SiC ceramic membrane is the outer diameterThe 12-channel tubular membrane of (2) has a length L=1200mm, an average pore diameter of about 100nm, and a pure water flux of about 1700 L.m -2 ·h -1 . Concentrating 30kg of water-soluble graphene slurry with solid content of 0.5wt%, controlling the operating pressure to be 0.05MPa, the operating temperature to be 22 ℃, and testing flux to be 1600 L.m -2 ·h -1 . After 45min concentration, the flux was stabilized at 1580L.m -2 ·h -1 About 13.6kg of concentrate, 1.1wt% of solid content, 2.2 times of concentrate. Then, the SiC ceramic membrane is subjected to acid washing treatment for 30min by using 20L of 1% citric acid aqueous solution, and then is washed by clean water until the pH value is neutral, and the pure water flux of the SiC ceramic membrane is recovered to 1700 L.m -2 ·h -1 Left and right.
As shown in fig. 2, the concentration effect of the water-soluble graphene slurry is shown, and it can be seen that the concentration degree of the method is high and the interception effect is remarkable.
As shown in fig. 3, the particle size analysis chart of graphene in the concentrated solution shows that the graphene peak is narrow and the average particle size is 16.7 μm.
The micro-morphology detection of graphene in the concentrate is performed, wherein the micro-morphology detection is shown in fig. 4: a Scanning Electron Microscope (SEM) of the graphene can find that the graphene has a sheet diameter of 10-20 mu m, a large number of intrinsic folds exist on a sheet layer, and the graphene has a thinner thickness; as described by fig. 5: transmission Electron Microscopy (TEM) provides greater magnification and surface wrinkles can be more clearly observed.
As shown in FIG. 6, the thickness of the lamellar layer was about 4.7nm, which is an Atomic Force Microscope (AFM) image of graphene in the concentrated solution.
Comparative example 1
The difference from the above example 1 is only that the specification of the SiC ceramic film was changed to the outer diameterThe length L=1200mm, the average pore diameter is about 100nm, and the pure water flux is about 1630L.m -2 ·h -1 . Concentrating 30kg of water-soluble graphene slurry with solid content of 0.5wt%, controlling the operating pressure to be 0.05MPa, the operating temperature to be 22 ℃, and testing flux to be about 1600 L.m -2 ·h -1 . After 60min concentration, the measured flux was stabilized at 1550 L.m -2 ·h -1 About 13.3kg of the concentrate had a solids content of about 1.1wt% and was concentrated 2.2 times. Then, the SiC ceramic membrane is subjected to acid washing treatment for 30min by using 20L of 1% citric acid aqueous solution, and then is washed by clean water until the pH value is neutral, and the pure water flux of the SiC ceramic membrane is recovered to 1630 L.m -2 ·h -1 Left and right. Flux becomes smaller, concentration time becomes longer, but concentration degree is high and interception effect is remarkable. Particle size analysis and microscopic morphology detection are carried out on graphene in the concentrated solution obtained after separation, so that the morphology is not changed obviously.
Comparative example 2
The difference from the above example 1 is only that the average pore diameter of the SiC ceramic membrane was changed to 500nm, and the SiC ceramic membrane was still of the outer diameterThe length l=1200mm of the 12-channel tubular membrane of (2) and the pure water flux of about 2200l·m -2 ·h -1 . Concentrating 30kg of water-soluble graphene slurry with solid content of 0.5wt%, controlling the operating pressure to be 0.05MPa, the operating temperature to be 22 ℃, and measuring flux to be about2100L·m -2 ·h -1 . After concentration for 40min, the measured flux was stabilized at 1980 L.m -2 ·h -1 About 13.2kg of the concentrate had a solids content of about 1.1wt% and was concentrated 2.2 times. Then, the SiC ceramic membrane is subjected to acid washing treatment for 30min by using 20L of 1% citric acid aqueous solution, and then is washed by clean water until the pH value is neutral, and the pure water flux of the SiC ceramic membrane is recovered to 2200 L.m -2 ·h -1 Left and right. The flux is increased, the concentration time is shortened, but the concentration degree is high and the interception effect is obvious. Particle size analysis and microscopic morphology detection are carried out on graphene in the concentrated solution obtained after separation, so that the morphology is not changed obviously.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (7)
1. A method for concentrating water-soluble graphene slurry based on a ceramic membrane method is characterized by comprising the following steps of: pumping low-concentration water-soluble graphene slurry into ceramic membrane equipment through a feed pump, and performing solid-liquid separation on the low-concentration water-soluble graphene slurry in a pressure driving mode to obtain high-concentration water-soluble graphene slurry; finally, the flux of the polluted SiC ceramic membrane is completely recovered by acid washing, so that the SiC ceramic membrane can stably operate for a long time.
2. The method for concentrating water-soluble graphene slurry based on a ceramic membrane method according to claim 1, wherein the method comprises the following steps: the graphene slurry prepared by stripping the low-concentration water-soluble graphene slurry by a pure water phase method is homogenized, and the concentration of the slurry is 0.5wt%.
3. The method for concentrating water-soluble graphene slurry based on a ceramic membrane method according to claim 1, wherein the method comprises the following steps: the ceramic membrane is a multichannel tubular SiC ceramic membrane, the average pore diameter is adjustable between 100 and 500nm, and the length is 1200mm.
4. The method for concentrating a water-soluble graphene slurry based on a ceramic membrane method according to claim 1, comprising the steps of:
1) Adding the homogenized low-concentration water-soluble graphene slurry into a feed tank;
2) Starting a feed valve, starting a feed pump, pumping low-concentration water-soluble graphene slurry into ceramic membrane equipment, and adjusting the membrane-entering pressure and the operating temperature;
3) When the membrane filtration reaches a preset concentration multiple, closing a feed pump, and opening a valve to obtain high-concentration water-soluble graphene slurry;
4) And adding an acid washing solution into the feed tank, starting the feed pump, carrying out acid washing, controlling the washing time and the washing temperature, discharging the cleaning liquid after the end, adding pure water to wash until the pH value is neutral, and closing the feed pump.
5. The method for concentrating water-soluble graphene slurry based on a ceramic membrane method according to claim 4, wherein the method comprises the following steps: the homogenized low-concentration water-soluble graphene slurry in the step 1) is 30-50 kg.
6. The method for concentrating water-soluble graphene slurry based on a ceramic membrane method according to claim 4, wherein the method comprises the following steps: the film-entering pressure in the step 2) is 0.05-0.15 MPa of normal operation pressure, and the operation temperature is 20-25 ℃.
7. The method for concentrating water-soluble graphene slurry based on a ceramic membrane method according to claim 4, wherein the method comprises the following steps: the acid washing solution in the step 4) is 0.5 to 1 percent of citric acid aqueous solution or 0.5 to 1 percent of HNO 3 The water solution is used in an amount of 10-30L, the cleaning time is 20-40 min, and the cleaning temperature is 60-80 ℃.
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