CN112010404A - Organic small molecule cracking carbon, preparation method thereof, capacitive deionization unit and system - Google Patents
Organic small molecule cracking carbon, preparation method thereof, capacitive deionization unit and system Download PDFInfo
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Abstract
The invention discloses organic small molecule cracking carbon, a preparation method thereof, a capacitive deionization unit and a capacitive deionization system, wherein the preparation method comprises the following steps: mixing and grinding transition metal salt and organic micromolecules to obtain mixed powder; and sintering, grinding and acid washing the mixed powder to obtain the organic micromolecule cracking carbon. According to the invention, organic micromolecules are used as precursors for preparing the carbon electrode material, the thermal stability of the organic micromolecules is improved through the coordination of transition metal salt and the organic micromolecules, and the organic micromolecule cracking carbon with rich pore diameter structure can be obtained by performing double pore-forming through Lewis acid hydrolysis and carbon thermal reduction reaction of the transition metal salt in the sintering process; the appearance, graphitization degree and pore structure of the electrode material can be regulated and controlled by changing various parameters in the reaction process, so that the desalting performance of the capacitive deionization electrode consisting of organic micromolecular cracking carbon is improved, the preparation method is simple and rapid, and the capacitive deionization electrode can be applied to actual production in a large scale.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to organic small molecule cracking carbon, a preparation method thereof, a capacitive deionization unit and a capacitive deionization system.
Background
The global fresh water resources are increasingly deficient, and the recycling of high-salinity wastewater and sewage and the desalination of seawater and brackish water are important ways for solving the problem. The traditional common seawater desalination (desalination) technology mainly comprises multi-stage flash evaporation, reverse osmosis, membrane distillation and the like, and the methods can desalinate brine on a large scale, but the methods have high energy consumption, large equipment investment and complex membrane regeneration process, so that the development of desalination technology with lower energy consumption is urgently needed, and the brine treatment cost is reduced.
The Capacitive Deionization (CDI) technology is a novel low-cost, high-efficiency and environment-friendly desalination technology developed in recent years. Similar to the super capacitor energy storage technology, the working principle of CDI is based on the charge adsorption on the surface of the electrode material: when the brine passes through the parallel electrodes with positive and negative charges respectively, the positive and negative ions in the solution are adsorbed to the surfaces of the electrodes with opposite charges under the action of the electrostatic field, so that the ions in the solution are removed, and the water purification is realized. Compared with the traditional desalination technology, the CDI technology has the advantages of low energy consumption, simple electrode regeneration process and no secondary pollution, and is a novel desalination technology with great application potential. The core component of the CDI technology is an electrode, and controllable and macro-preparation of the electrode material with high adsorption capacity is the key of popularization and application of the technology. Therefore, the CDI electrode material which is green and environment-friendly, low in price and excellent in performance is developed, the requirement for the increasing development of CDI devices is met, and the CDI electrode material has important scientific significance and wide application prospect.
Carbon materials are an ideal class of CDI electrode materials due to their high specific surface area, good electrical conductivity, and chemical stability. Currently, carbon-based electrode materials which are commercially applied in a large scale are mainly activated carbons prepared from non-renewable petroleum resources such as asphalt through pyrolysis, however, in the carbonization-pore-forming process, the raw materials with high molecular weight involve complex molecular chain breakage and rearrangement, so that the microstructure of the obtained carbon material is difficult to control. Moreover, the process of preparing the porous carbon material by using the synthetic polymer as a raw material is complex, and the large-scale production is not easy. The development of a simple, cheap and controllable method for massively preparing the porous carbon material with excellent comprehensive performance still faces huge challenges.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The invention aims to solve the technical problems that the organic micromolecule cracking carbon and the preparation method thereof are provided for overcoming the defects in the prior art, and the problems that the process for preparing the electrode material by taking the synthetic polymer as the raw material is complex, the large-scale production is difficult, and the microstructure of the obtained carbon material is difficult to control are solved.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of organic small molecule cracked carbon comprises the following steps:
mixing and grinding transition metal salt and organic micromolecules to obtain mixed powder;
and sintering, grinding and acid washing the mixed powder to obtain the organic micromolecule cracking carbon.
The preparation method of the organic micromolecule cracking carbon comprises the following steps of (1) preparing transition metal salt, wherein the transition metal salt is one or more of ferric chloride, cobalt chloride, nickel chloride and copper chloride; the organic micromolecules are one or more of 1, 10-phenanthroline, aspartic acid, dopamine hydrochloride and melamine.
The preparation method of the organic micromolecule cracking carbon comprises the following steps of (0.5-16): 1.
the preparation method of the organic small molecule cracking carbon comprises the following steps of sintering, grinding and acid washing the mixed powder to obtain the organic small molecule cracking carbon:
sintering the mixed powder in inert gas, cooling to room temperature, grinding, and screening by a 200-400-mesh sample sieve to obtain a sintered product;
and stirring the sintered product in an acid solution for 5-8 hours, washing with deionized water and drying to obtain the organic micromolecular cracking carbon.
The preparation method of the organic small molecule cracking carbon comprises the following steps: heating to 600-1000 ℃ at a heating rate of 4-6 ℃/min and preserving heat for 1-3 h.
The preparation method of the organic micromolecule cracking carbon comprises the step of preparing an acid solution, wherein the acid solution is a hydrochloric acid solution with the concentration of 1-3 mol/L.
The organic small molecule cracking carbon is prepared by the preparation method.
A capacitive deionization unit comprising a capacitive deionization electrode, wherein the capacitive deionization electrode comprises the small organic molecule cleavage carbon.
The capacitive deionization unit, wherein the capacitive deionization electrode further comprises conductive carbon black and a binder; the mass ratio of the organic micromolecule cracking carbon to the conductive carbon black to the binder is 6-8: 2-1.
A capacitive deionization system comprises the capacitive deionization unit.
Has the advantages that: according to the invention, organic micromolecules are used as precursors for preparing the carbon electrode material, the thermal stability of the organic micromolecules is improved through the coordination of transition metal salt and the organic micromolecules, and the organic micromolecule cracking carbon with rich pore diameter structure can be obtained by performing double pore-forming through Lewis acid hydrolysis and carbon thermal reduction reaction of the transition metal salt in the sintering process; the appearance, graphitization degree and pore structure of the electrode material can be regulated and controlled by changing various parameters in the reaction process, so that the desalting performance of the capacitive deionization electrode consisting of organic micromolecular cracking carbon is improved, the preparation method is simple and rapid, and the capacitive deionization electrode can be applied to actual production in a large scale.
Drawings
FIG. 1 is a scanning electron microscope photograph of a melamine organic small molecule cracked carbon prepared in example 1 of the present invention;
FIG. 2 is a graph showing isothermal adsorption and desorption curves of the cracked carbon of melamine organic small molecules prepared in example 1 of the present invention;
FIG. 3 is a graph showing the distribution of the pore diameters of the small organic melamine molecular cracking carbons prepared in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern of a small organic melamine molecular cracking carbon prepared in example 1 of the present invention;
FIG. 5 is a plot of cyclic voltammetry for a capacitive deionization electrode composed of the small melamine organic molecule cleaved carbon prepared in example 1 of the present invention;
FIG. 6 is a graph of constant current charging and discharging of a capacitive deionization electrode composed of the melamine organic small molecule cracked carbon prepared in example 1 of the present invention;
FIG. 7 is a schematic structural diagram of a capacitive deionization unit according to an embodiment of the present invention;
FIG. 8 is a graph showing the change of conductivity with time of a capacitive deionization electrode composed of a small organic melamine molecular cracking carbon prepared in example 1 of the present invention, which was subjected to a desalting performance test;
FIG. 9 is a graph showing the change of the salt adsorption amount with time when a capacitive deionization electrode composed of a melamine organic small molecule cracked carbon prepared in example 1 of the present invention was subjected to a desalting performance test;
FIG. 10 is a plot of cyclic voltammetry for a capacitive deionization electrode composed of 1,10 phenanthroline small organic molecule cleaved carbon prepared in example 2 of the present invention;
FIG. 11 is a graph showing constant current charging and discharging curves of a capacitive deionization electrode composed of 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention;
FIG. 12 is a graph showing the change of conductivity with time when a desalting performance test was performed on a capacitive deionization electrode composed of 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention;
FIG. 13 is a graph showing the change of the amount of salt adsorbed with time when a desalting performance test was performed on a capacitive deionization electrode composed of 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention;
FIG. 14 is a plot of cyclic voltammetry for a capacitive deionization electrode composed of dopamine hydrochloride small organic molecule cleaving carbon prepared in example 3 of the present invention;
fig. 15 is a constant current charge and discharge curve diagram of a capacitive deionization electrode composed of dopamine hydrochloride small organic molecule cracked carbon prepared in example 3 of the present invention.
FIG. 16 is a graph showing the change of conductivity with time of a capacitive deionization electrode composed of dopamine hydrochloride small organic molecule cracked carbon prepared in example 3 of the present invention, which was subjected to a desalting performance test;
FIG. 17 is a graph showing the change of salt adsorption with time when a capacitive deionization electrode composed of dopamine hydrochloride small organic molecule cracked carbon prepared in example 3 of the present invention was subjected to a desalting performance test.
Detailed Description
The invention provides an organic small molecule cracking carbon, a preparation method thereof, a capacitance deionization unit and a system, and the invention is further described in detail below in order to make the purposes, technical schemes and advantages of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Specifically, the preparation method of the small organic molecule cracking carbon comprises the following steps:
and S1, mixing and grinding the transition metal salt and the organic micromolecules to obtain mixed powder.
In specific implementation, the method aims to solve the problems that the existing process for preparing the electrode material by taking the synthetic polymer as the raw material is complex, large-scale production is not easy, and the microstructure of the obtained carbon material is difficult to control. In the embodiment, organic small molecules are used as precursors for preparing the carbon electrode material, the organic small molecules are easily decomposed into gas at high temperature and escape, the organic small molecules are directly carbonized to obtain a solid product, and before the organic small molecules are carbonized, the transition metal salt and the organic small molecules are mixed and ground to obtain mixed powder. In the subsequent sintering process, the transition metal ions and the organic micromolecules improve the thermal stability of the organic micromolecules through coordination, and the organic micromolecules are prevented from being decomposed into gas, so that the organic micromolecule cracking carbon is obtained.
Detailed description of the inventionWhen the transition metal salt is ferric chloride (FeCl)3) Cobalt chloride (CoCl)2) Nickel chloride (NiCl)2) Copper chloride (CuCl)2) The organic small molecule is 1, 10-phenanthroline (C)12H8N2·H2O), aspartic acid (C)4H7NO4) Dopamine hydrochloride (C)8H11NO2HCl) and melamine (C)3H6N6) One or more of (a). During sintering, the transition metal ion, i.e. Fe3+、Co2+、Ni2+Or Cu2+Can coordinate with nitrogen functional groups on the surface of the organic micromolecule, thereby improving the thermal stability of the organic micromolecule. In one embodiment, the mole ratio of the small organic molecule to the transition metal salt is (0.5-16): 1.
and S2, sintering, grinding and acid washing the mixed powder to obtain the organic micromolecule cracking carbon.
In specific implementation, after mixed powder of the transition metal salt and the small organic molecule is obtained, the mixed powder is further sintered, ground and acid-washed to obtain the small organic molecule cracking carbon. In the high-temperature sintering process, the transition metal salt can be coordinated with a functional group on the organic micromolecule to improve the thermal stability of the organic micromolecule, and Lewis acid hydrolysis and carbon thermal reduction reaction can also be carried out, so that double pore forming is carried out on the organic micromolecule cracking carbon, and the prepared organic micromolecule cracking carbon has a rich porous structure. In the embodiment, the appearance, graphitization degree and pore structure of the prepared organic micromolecule cracking carbon can be regulated and controlled by changing factors such as the boiling point, metal activity (electronegativity), metal salt crystal structure, heteroatom type and proportion in the organic micromolecule, and the like of the transition metal salt, so that the desalting performance of the capacitive deionization electrode consisting of the organic micromolecule cracking carbon is improved, the preparation method is simple and rapid, and the capacitive deionization electrode can be applied to actual production in a large scale.
In a specific embodiment, the step S2 specifically includes:
s21, sintering the mixed powder in inert gas, cooling to room temperature, grinding, and screening by a 200-400-mesh sample sieve to obtain a sintered product;
and S22, stirring the sintered product in an acid solution for 5-8 hours, washing with deionized water and drying to obtain the organic small molecule cracking carbon.
In specific implementation, after the mixed powder is obtained, sintering the mixed powder in an inert atmosphere to crack and carbonize organic small molecules in the mixed powder, cooling to room temperature, grinding the product, and sieving with a 200-400-mesh sample sieve to obtain a sintered product. And then stirring the sintered product in an acid solution for 5-8 h, washing with deionized water to remove residual acid solution and transition metal salt in the sintered product, and drying to obtain the organic micromolecular cracking carbon. In a specific embodiment, the inert gas is nitrogen, argon, and the like, the sintered product is ground and then screened by a 300-mesh sample sieve to improve the particle size uniformity of the prepared small organic molecule cracked carbon, the acid solution is a hydrochloric acid solution with a concentration of 1-3 mol/L, and the stirring time is 6 hours.
Further, the sintering conditions are as follows: heating to 600-1000 ℃ at a heating rate of 4-6 ℃/min and preserving heat for 1-3 h. With the increase of the sintering temperature, the organic micromolecules undergo the pyrolysis reaction of dehydrogenation to carbon, so that the prepared organic micromolecule cracked carbon has higher carbonization degree, but the organic micromolecules are easily decomposed into gas to escape due to too high sintering temperature. In one embodiment, the temperature is raised to 800 ℃ at a heating rate of 5 ℃/min and maintained for 2 hours during sintering.
In a specific embodiment, the invention also provides small organic molecule cracking carbon, and the small organic molecule cracking carbon is prepared by the preparation method.
In one embodiment, the present invention also provides a capacitive deionization unit comprising a capacitive deionization electrode; the capacitive deionization electrode consists of a current collector and an electrode material coated on the current collector; the electrode material comprises the organic small molecule cracking carbon. As shown in fig. 7, the capacitive deionization unit includes an electrode pair composed of two capacitive deionization electrodes 1 which are the same in size and are symmetrically arranged, a hollow resin partition plate 2 for isolating the two capacitive deionization electrodes 1 on the electrode pair to serve as a fluid channel, a water inlet 3 and a water outlet 4 connected to the hollow resin partition plate 2, and a dc power supply 5 connected to the two capacitive deionization electrodes 1 of the electrode pair, and the capacitive deionization unit is sealed by glass resin and silica gel.
Further, the electrode material comprises conductive carbon black and a binder besides the organic small molecule cracking carbon. The mass ratio of the organic micromolecule cracking carbon to the conductive carbon black to the binder is 6-8: 2-1. When the capacitive deionization electrode 1 is prepared, mixing organic small molecule cracking carbon, conductive carbon black and a binder in a mass ratio of 6-8: 2-1, then dripping a small amount of ethanol, stirring and ultrasonically treating for a preset time, drying, then dripping ethanol to obtain a viscous micelle, and pressing the viscous micelle on a current collector to obtain the capacitive deionization electrode. In a specific embodiment, the binder is polytetrafluoroethylene, the mass fraction of the binder polytetrafluoroethylene is 10-60%, the stirring time is 10min, the ultrasonic time is 10min, and the current collector is one or more of a titanium sheet, a graphite sheet and a copper sheet.
In a specific embodiment, the invention further provides a capacitive deionization system, which comprises the capacitive deionization unit, a water storage tank, a peristaltic pump, an external power supply and a conductivity meter. The water storage tank is used for water inlet and outlet circulation; the peristaltic pump is used for controlling the flow rate of water; the external power supply is used for controlling the charging and discharging processes of the capacitive deionization unit; the conductivity meter is used for monitoring and recording the conductivity (namely salt concentration) condition of the water in the water storage tank.
According to the invention, organic micromolecules are used as precursors for preparing the carbon electrode material, the thermal stability of the organic micromolecules is improved through the coordination of transition metal salt and the organic micromolecules, and the organic micromolecule cracking carbon with rich pore diameter structure can be obtained by performing double pore-forming through Lewis acid hydrolysis and carbon thermal reduction reaction of the transition metal salt in the sintering process; the appearance, graphitization degree and pore structure of the electrode material can be regulated and controlled by changing various parameters in the reaction process, so that the desalting performance of the capacitive deionization electrode consisting of organic micromolecular cracking carbon is improved, the preparation method is simple and rapid, and the capacitive deionization electrode can be applied to actual production in a large scale.
The invention is further illustrated by the following specific examples.
Example 1
(1) Weighing ferric trichloride hexahydrate (FeCl) with a molar ratio of 1:13·6H2O) and organic small molecule melamine (C)3H6N6) Fully grinding after mixing to obtain mixed powder;
(2) and sintering the mixed powder in a nitrogen atmosphere under the following sintering conditions: heating to 800 deg.C at a rate of 5 deg.C/min, and maintaining for 120 min; naturally cooling to room temperature after sintering, grinding, and screening by a 300-mesh sample sieve to obtain a sintered product; and placing the sintered product in a 2mol/L hydrochloric acid solution, stirring for 6h, washing with deionized water to remove residual hydrochloric acid and transition metal salt, and drying to obtain the melamine organic micromolecule cracking carbon.
Example 2
(1) Weighing ferric trichloride hexahydrate (FeCl) with a molar ratio of 1:163·6H2O) and organic small molecule 1,10 phenanthroline (C)12H8N2·H2O), fully grinding after mixing to obtain mixed powder;
(2) and sintering the mixed powder in a nitrogen atmosphere under the following sintering conditions: heating to 800 deg.C at a rate of 5 deg.C/min, and maintaining for 120 min; naturally cooling to room temperature after sintering, grinding, and screening by a 300-mesh sample sieve to obtain a sintered product; and placing the sintered product in a 2mol/L hydrochloric acid solution, stirring for 6h, washing with deionized water to remove residual hydrochloric acid and transition metal salt, and drying to obtain the 1,10 phenanthroline organic micromolecule cracking carbon.
Example 3
(1) Weighing ferric trichloride hexahydrate (FeCl) with a molar ratio of 1:13·6H2O) and organic small-molecule dopamine hydrochloride (C)8H11NO2HCl), mixed and then fully ground to obtain a mixed powder;
(2) and sintering the mixed powder in a nitrogen atmosphere under the following sintering conditions: heating to 800 deg.C at a rate of 5 deg.C/min, and maintaining for 120 min; naturally cooling to room temperature after sintering, grinding, and screening by a 300-mesh sample sieve to obtain a sintered product; and placing the sintered product in a 2mol/L hydrochloric acid solution, stirring for 6h, washing with deionized water to remove residual hydrochloric acid and transition metal salt, and drying to obtain the dopamine hydrochloride organic micromolecule cracking carbon.
Fig. 1 is a scanning electron microscope image of the melamine organic small molecule cracked carbon prepared in example 1 of the present invention, and it can be seen from fig. 1 that the melamine organic small molecule cracked carbon prepared in example 1 of the present invention has a rich porous structure and good structural stability.
Fig. 2 is a graph showing isothermal adsorption and desorption of the melamine organic small molecule cracked carbon prepared in example 1 of the present invention, and fig. 3 is a graph showing the pore size distribution of the melamine organic small molecule cracked carbon prepared in example 1 of the present invention. As can be seen from fig. 2 and fig. 3, the small organic melamine molecular cracking carbon prepared in example 1 of the present invention has a large specific surface area and a rich pore size structure.
Fig. 4 is an X-ray diffraction diagram of the cracked carbon containing small organic melamine molecules prepared in example 1 of the present invention, and it can be seen from fig. 4 that the cracked carbon containing small organic melamine molecules prepared in example 1 of the present invention has a high graphitization degree and Fe is bonded to N.
Fig. 5 is a cyclic voltammogram of a capacitive deionization electrode composed of melamine organic small molecule cracked carbon prepared in example 1 of the present invention, and it can be seen from fig. 5 that the cyclic voltammogram of the capacitive deionization electrode is rectangular, showing electric double layer capacitance characteristics.
Fig. 6 is a constant current charging and discharging curve diagram of the capacitive deionization electrode composed of the melamine organic small molecule cracked carbon prepared in the embodiment 1 of the present invention, and it can be seen from fig. 6 that the constant current charging and discharging curve of the capacitive deionization electrode is triangular, and has good capacitance reversibility.
FIG. 7 is a schematic diagram of a capacitive deionization apparatus.
FIG. 8 is a graph showing the change of conductivity with time when a capacitive deionization electrode composed of a small organic melamine molecular cracking carbon prepared in example 1 of the present invention was subjected to a desalting performance test.
FIG. 9 is a graph showing the change of the salt adsorption amount with time when a desalting performance test is performed on a capacitive deionization electrode composed of a melamine organic small molecule cracked carbon prepared in example 1 of the present invention. As can be seen from FIG. 9, the desalting capacity of the capacitive deionization electrode composed of the melamine organic small molecule cracked carbon prepared in example 1 of the present invention reached 13 mg/g.
Fig. 10 is a cyclic voltammogram of the capacitive deionization electrode composed of 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention, and as can be seen from fig. 10, the cyclic voltammogram of the capacitive deionization electrode is rectangular, showing the electric double layer capacitance characteristics.
Fig. 11 is a constant current charging and discharging curve diagram of the capacitive deionization electrode composed of the 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention, and it can be seen from fig. 11 that the constant current charging and discharging curve of the capacitive deionization electrode is triangular, and has good capacitance reversibility.
FIG. 12 is a graph showing the change of conductivity with time when a desalting performance test was performed on a capacitive deionization electrode composed of 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention.
FIG. 13 is a graph showing the change of the salt adsorption amount with time when a desalting performance test was performed on a capacitive deionization electrode composed of 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention. As can be seen from FIG. 13, the desalting capacity of the capacitive deionization electrode composed of 1,10 phenanthroline organic small molecule cracked carbon prepared in example 2 of the present invention reaches 8 mg/g.
Fig. 14 is a cyclic voltammetry graph of a capacitive deionization electrode composed of dopamine hydrochloride organic small molecule cleavage carbon prepared in example 3 of the present invention, and it can be seen from fig. 14 that the cyclic voltammetry graph of the capacitive deionization electrode is rectangular, showing electric double layer capacitance characteristics.
Fig. 15 is a constant current charging and discharging curve diagram of the capacitive deionization electrode composed of dopamine hydrochloride organic small molecule cracked carbon prepared in example 3 of the present invention, and it can be seen from fig. 15 that the constant current charging and discharging curve of the capacitive deionization electrode is triangular and has good capacitance reversibility.
FIG. 16 is a graph showing the change of conductivity with time when a capacitive deionization electrode composed of dopamine hydrochloride small organic molecule cracked carbon prepared in example 3 of the present invention was subjected to a desalting performance test.
FIG. 17 is a graph showing the change of salt adsorption with time when a capacitive deionization electrode composed of dopamine hydrochloride small organic molecule cracked carbon prepared in example 3 of the present invention was subjected to a desalting performance test. As can be seen from FIG. 17, the desalting capacity of the capacitive deionization electrode composed of dopamine hydrochloride organic small molecule cracked carbon prepared in example 3 of the present invention reaches 18 mg/g.
In summary, the invention discloses an organic small molecule cracking carbon, a preparation method thereof, a capacitive deionization unit and a capacitive deionization system, wherein the preparation method comprises the following steps: mixing and grinding transition metal salt and organic micromolecules to obtain mixed powder; and sintering, grinding and acid washing the mixed powder to obtain the organic micromolecule cracking carbon. According to the invention, organic micromolecules are used as precursors for preparing the carbon electrode material, the thermal stability of the organic micromolecules is improved through the coordination of transition metal salt and the organic micromolecules, and the organic micromolecule cracking carbon with rich pore diameter structure can be obtained by performing double pore-forming through Lewis acid hydrolysis and carbon thermal reduction reaction of the transition metal salt in the sintering process; the appearance, graphitization degree and pore structure of the electrode material can be regulated and controlled by changing various parameters in the reaction process, so that the desalting performance of the capacitive deionization electrode consisting of organic micromolecular cracking carbon is improved, the preparation method is simple and rapid, and the capacitive deionization electrode can be applied to actual production in a large scale.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of organic small molecule cracking carbon is characterized by comprising the following steps:
mixing and grinding transition metal salt and organic micromolecules to obtain mixed powder;
and sintering, grinding and acid washing the mixed powder to obtain the organic micromolecule cracking carbon.
2. The method for preparing small organic molecule cracking carbon according to claim 1, wherein the transition metal salt is one or more of ferric chloride, cobalt chloride, nickel chloride and copper chloride; the organic micromolecules are one or more of 1, 10-phenanthroline, aspartic acid, dopamine hydrochloride and melamine.
3. The method for preparing small organic molecule cracking carbon according to claim 1, wherein the molar ratio of the small organic molecule to the transition metal salt is (0.5-16): 1.
4. the method for preparing small organic molecule cracked carbon according to claim 1, wherein the step of sintering, grinding and acid washing the mixed powder to obtain small organic molecule cracked carbon comprises:
sintering the mixed powder in inert gas, cooling to room temperature, grinding, and screening by a 200-400-mesh sample sieve to obtain a sintered product;
and stirring the sintered product in an acid solution for 5-8 hours, washing with deionized water and drying to obtain the organic micromolecular cracking carbon.
5. The method for producing small organic molecule cracked carbon according to claim 1, wherein the sintering conditions are: heating to 600-1000 ℃ at a heating rate of 4-6 ℃/min and preserving heat for 1-3 h.
6. The method for preparing small organic molecule cracked carbon according to claim 4, characterized in that the acid solution is hydrochloric acid solution with a concentration of 1-3 mol/L.
7. An organic small molecule cracking carbon, which is prepared by the preparation method of any one of claims 1 to 6.
8. A capacitive deionization unit comprising a capacitive deionization electrode, wherein the capacitive deionization electrode comprises the small organic molecule cleaved carbon of claim 7.
9. The capacitive deionization unit according to claim 8, wherein said capacitive deionization electrode further comprises conductive carbon black and a binder; the mass ratio of the organic micromolecule cracking carbon to the conductive carbon black to the binder is 6-8: 2-1.
10. A capacitive deionization system comprising a capacitive deionization unit according to claim 8 or 9.
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| CN106981671A (en) * | 2017-04-15 | 2017-07-25 | 佛山市利元合创科技有限公司 | A kind of three-dimensional porous nitrogen-doped graphene and its preparation method and application |
| CN107481864A (en) * | 2016-06-07 | 2017-12-15 | 中国海洋大学 | It is a kind of to prepare high surface, the method for nitrogen oxygen codope carbon material and the application in ultracapacitor by raw material of organic matter |
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2020
- 2020-08-03 CN CN202010767206.2A patent/CN112010404A/en active Pending
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| US20030086860A1 (en) * | 2000-01-31 | 2003-05-08 | Kenichi Uehara | Method for preparing porous carbon material, porous carbon material and electrical double layer capacitor using the same |
| US20120241691A1 (en) * | 2009-11-30 | 2012-09-27 | Toyo Tanso Co., Ltd. | Nitrogen-containing porous carbon material and method of producing the same, and electric double-layer capacitor using the nitrogen-containing porous carbon material |
| CN104269566A (en) * | 2014-09-22 | 2015-01-07 | 南开大学 | Preparation method and application of nitrogen-doped porous carbon nano sheet composite material |
| CN105836858A (en) * | 2016-06-03 | 2016-08-10 | 华东师范大学 | Method for preparing capacitive desalination electrode |
| CN107481864A (en) * | 2016-06-07 | 2017-12-15 | 中国海洋大学 | It is a kind of to prepare high surface, the method for nitrogen oxygen codope carbon material and the application in ultracapacitor by raw material of organic matter |
| CN106981671A (en) * | 2017-04-15 | 2017-07-25 | 佛山市利元合创科技有限公司 | A kind of three-dimensional porous nitrogen-doped graphene and its preparation method and application |
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