CN111087054A - Simple preparation method for synthesizing electro-adsorption desalination electrode by carbonizing reed straw - Google Patents
Simple preparation method for synthesizing electro-adsorption desalination electrode by carbonizing reed straw Download PDFInfo
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- 239000010902 straw Substances 0.000 title claims abstract description 29
- 235000014676 Phragmites communis Nutrition 0.000 title claims abstract description 24
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000010612 desalination reaction Methods 0.000 title claims abstract description 12
- 238000010000 carbonizing Methods 0.000 title abstract description 4
- 230000002194 synthesizing effect Effects 0.000 title description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000002028 Biomass Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000003575 carbonaceous material Substances 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
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- 239000012258 stirred mixture Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 238000003763 carbonization Methods 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 11
- 238000002242 deionisation method Methods 0.000 abstract description 9
- 238000009835 boiling Methods 0.000 abstract description 3
- 239000003610 charcoal Substances 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 3
- 238000004140 cleaning Methods 0.000 abstract 1
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- 238000012360 testing method Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 230000008929 regeneration Effects 0.000 description 6
- 238000011069 regeneration method Methods 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 239000002149 hierarchical pore Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
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- 238000005406 washing Methods 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000011033 desalting Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 239000003513 alkali Substances 0.000 description 1
- 239000010796 biological waste Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 238000003795 desorption Methods 0.000 description 1
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- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- 239000013535 sea water Substances 0.000 description 1
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- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
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Abstract
The invention discloses an electro-adsorption desalination electrode synthesized by carbonizing reed straws and a preparation method thereof. And then drying to obtain a dry mixture, placing the dry mixture in a tubular heating furnace, preserving the heat at 600 ℃, 700 ℃ and 800 ℃ for 1 hour, adding a proper amount of hydrochloric acid solution into the obtained biomass carbon powder, and neutralizing and cleaning to obtain the final biomass carbon powder. Mixing absolute ethyl alcohol, polytetrafluoroethylene and final biomass carbon powder, heating in a water bath, stirring, pressing the obtained mixture into a paste body on a stainless steel net by using a hot press, boiling the pressed electrode slice, and drying. And preparing the biomass charcoal electrode plate for capacitive deionization. (1) The electrode prepared by the invention has small internal resistance, high capacitance and good adsorption performance, and (2) the preparation method and the preparation process are simple, the production cost is low, the resource utilization of waste is realized, and the environment is protected.
Description
Technical Field
The invention relates to the field of capacitive deionization, in particular to a capacitive deionization adsorption electrode and a preparation method thereof.
Background
The earth has rich water resources, wherein the fresh water resources only account for 2.7 percent, and most of the fresh water is glacier water which is difficult to utilize, the fresh water resources are not only deficient, but also have the problems of serious uneven distribution and the like, bitter water can not be used, and the difficulty of regenerating domestic and industrial sewage treatment is increased, which is the most important problem for hindering the rapid and continuous development of the society, and the traditional seawater desalination technologies, such as membrane distillation, ion exchange resin, reverse osmosis and electrodialysis, are energy-intensive and expensive, and comprise regeneration in an environment-unfriendly way, such as using acid or alkali solution; therefore, a new water desalination technology, Capacitive Deionization (CDI), is rapidly developing due to its excellent properties, which include high energy efficiency and water recovery as well as low energy consumption and pollution; capacitive Deionization (CDI) is a water desalination technique based on the removal of ions by an electro-adsorption process; the electrode material is a key factor influencing the deionization effect of the capacitor, and the biomass material has the characteristics of low cost and rich resources, so that the biomass material is widely applied to the fields of supercapacitors, microbial fuel cells and the like, but the biomass material applied to electric adsorption is less, the reed is a common aquatic plant and is widely distributed, and a large amount of reed is accumulated and blocks a river channel after drying up in autumn and winter; the adsorbent is used for preparing the adsorbent, so that double effects of purifying water and comprehensively utilizing resources can be achieved; therefore, the invention takes reed straws as an adsorbent material, researches the adsorption effect and influence factors of the adsorbent material on NaCl in a water body, and prepares the porous carbon material by using the reed straws as a raw material and KOH as an activating agent, so the porous carbon material is called as a reed straw porous carbon material (RSPC); the prepared material has a mutually connected hierarchical pore structure, the hierarchical pore structure has great advantages in the electric adsorption process, and the unique through hole structure of the RSPC causes large specific surface area; the gap between the hierarchical pore structure and the upper wall layer facilitates rapid charge movement; in addition, due to their three-dimensional hierarchical pore structure, RSPCs can form bilayers at the interface with the electrolyte to store large amounts of charge, resulting in high specific capacitance and excellent rate performance, which demonstrates the potential use of RSPCs as electrode materials in capacitive deionization.
Disclosure of Invention
In conclusion, the invention aims to develop a low-cost reed straw electro-adsorption desalination electrode and a preparation method thereof, and the electrode material can be applied to the field of capacitive deionization due to the characteristics of small internal resistance, high capacitance and good adsorption performance;
in order to achieve the above purpose, the technical scheme adopted by the invention comprises the following specific steps:
a. preparing reed straw pulp: firstly, washing reed straws with deionized water, drying and crushing the reed straws into powder; adding straw powder and KOH into a conical flask according to a certain proportion, adding a proper amount of deionized water, heating in a water bath and stirring;
b. activation of reed straw pulp: then, the mixture is placed in an oven to be dried for 5 hours at the temperature of 100 ℃, the straws are subjected to heat treatment under the protection of high-purity nitrogen, and then the straws are cooled to room temperature under the atmosphere of nitrogen;
c. washing to be neutral: grinding the calcined product in a mortar; after grinding, adding 20mL of deionized water and a proper amount of concentrated hydrochloric acid into a beaker, stirring for 12 hours by using a magnetic stirrer, and centrifuging the stirred mixture until the pH value of the solution is neutral; finally, putting the residues into an oven, and drying for 12 hours at 120 ℃ to obtain a porous biomass charcoal material;
d. pressing an electrode plate: 0.6g of RSPC, 1.8g of absolute ethanol and 1.8g of polytetrafluoroethylene (10% PTFE) were continuously mixed and stirred in a water bath at 65 ℃ until the water evaporated to form a paste; then, the mixture is quickly taken out, and the paste is pressed on a stainless steel net (4cm multiplied by 6cm) by a hot press; and finally, boiling the pressed electrode slice in water for 30min to stabilize the electrode slice, and drying the electrode slice in a drying oven at 40 ℃ for later use to prepare the reed straw electro-adsorption desalination electrode slice.
The invention has the beneficial effects that:
(1) the invention adopts natural reed straw as raw material, realizes the resource and effective utilization of biological waste, changes waste into valuable, and has environment-friendly preparation process;
(2) the RSPC material prepared by the invention has small internal resistance, rich pore channel structure, higher specific surface area (specific number) and excellent electrochemical performance;
(3) the RSPC material prepared by the invention has the characteristics of high electrode desalting capacity, high current efficiency, low energy consumption (1.2V low voltage is selected), strong electrode adsorption capacity, simple process, low cost and the like, so that the RSPC material can be used for a capacitance deionization experiment and is easy for large-scale production.
Drawings
FIG. 1 shows the conductivity of five samples as a function of time.
FIG. 2 is a scanning electron microscope image of a sample with an activation temperature of 700 ℃ and an activation ratio of 3: 1.
Detailed Description
The specific implementation method comprises the following steps: in order to avoid repetition, first, technical parameters related to this embodiment are uniformly described as follows, and no further description is given in the embodiments, and first, the RSPC electrode is prepared:
an electro-adsorption desalination electrode synthesized by carbonizing reed straws and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
firstly, washing reed straws with deionized water for 3-5 times, drying at 60 ℃ for 5 hours, crushing into powder, and screening by using a 200-mesh screen; adding 5 straw powder and 5KOH powder (mass ratio is 1:1) into a conical flask, adding 100mL of deionized water, heating in a water bath at 75 ℃, and stirring for 4 hours;
secondly, placing the mixture in an oven to be dried for 5h at 100 ℃, taking out the mixture in a completely dried state, placing the mixture in a mortar to be ground, placing the mixture powder in a porcelain boat, and placing the porcelain boat in a high-purity nitrogen protective atmosphere at 5 ℃ for min-1Heating to 700 ℃ at the heating rate, keeping the temperature for 1h, and then cooling to room temperature in the nitrogen atmosphere;
thirdly, grinding the calcined product in a mortar, adding 20mL of deionized water and concentrated hydrochloric acid into the beaker after grinding, stirring for 12 hours by using a magnetic stirrer, and centrifuging the stirred mixture until the pH value of the solution is neutral; finally, putting the residues into an oven, and drying for 12 hours at 120 ℃ to obtain a porous biomass charcoal material;
fourthly, 0.6g of RSPC, 1.8g of absolute ethyl alcohol and 1.8g of polytetrafluoroethylene (10 percent PTFE) are continuously mixed and stirred in a water bath at 65 ℃ until water is evaporated to form paste;
fifthly, quickly taking out the mixture, and pressing the paste on a stainless steel net (4cm multiplied by 6cm) by a hot press; and finally, boiling the pressed electrode slice in water for 30min to stabilize the electrode slice, and drying the electrode slice in a drying oven at 40 ℃ for later use to prepare the reed straw electro-adsorption desalination electrode slice.
The specific implementation method II comprises the following steps: the first difference between the implementation method and the specific implementation method is that: in the first step, RS and KOH are 2:1, and the rest is the same as the first embodiment.
The specific implementation method comprises the following steps: the first difference between the implementation method and the specific implementation method is that: in the first step, RS and KOH are 3:1, and the rest is the same as the first embodiment.
The specific implementation method four: the first difference between the implementation method and the specific implementation method is that: the activation temperature in the second step is 600 ℃, and the rest is the same as that in the first embodiment.
The concrete implementation method comprises the following steps: the first difference between the implementation method and the specific implementation method is that: the activation temperature in the second step is 800 ℃, and the rest is the same as that in the first embodiment.
The beneficial effects of the present invention were verified by the RSAC desalting performance test prepared below.
Test one, the electrode sheets with the same size (4cm × 6cm) prepared in the implementation method one are assembled into a device. RSPC material is respectively connected with the anode and the cathode of a power supply and is 1g L in 100mL-1Performing electro-adsorption test in NaCl solution, setting constant voltage mode for DC power supply voltage of 1.2V, three pairs of electrode plates with plate interval of 3mm, and flow rate of 15mL min-1The adsorption and desorption time is 30 min; the conductivity meter monitors the change of the solution concentration in real time, the experimental result is shown in figure 1 (the relationship between the conductivity and the time), and the RSPC electrode has good cyclic regeneration performance, and the adsorption quantity of the electrode per unit mass is 10.65 mg g-1。
Experiment II, the difference between the experiment example and the experiment example 1 is that the electrode slice is used in the implementation method II, the experiment result is shown in figure 1 (the relation between the conductivity and the time), and the RSPC electrode has good cycle regeneration performance, and the adsorption quantity of the electrode per unit mass is 10.94mg g-1。
Experiment III, the difference between the experiment example and the experiment example 1 is that the electrode slice is used in the implementation method III, the experimental result is shown in figure 1 (the relation between the conductivity and the time), and the RSPC electrode has good cycle regeneration performance, and the adsorption quantity of the electrode per unit mass is 13.23mg g-1。
The fourth test is different from the first test in that the electrode sheet is used in the fourth implementation method, the test result is shown in fig. 1 (the relation between the conductivity and the time), and the RSPC electrode has good cyclic regeneration performance and unit mass electrodeHas an adsorption amount of 11.89mg g-1。
The fifth test is different from the first test 1 in that the electrode sheet is used in the fifth test, the test result is shown in fig. 1 (the relationship between the conductivity and the time), and the RSPC electrode has good cycle regeneration performance and the adsorption amount per unit mass of the electrode is 12.7mg g-1。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111252866A (en) * | 2020-01-20 | 2020-06-09 | 中南大学 | CDI electrode active material and preparation and application thereof |
| CN114180573A (en) * | 2021-12-24 | 2022-03-15 | 南京师范大学 | Biomass-derived porous carbon electrode and preparation method and application thereof |
| CN114477386A (en) * | 2022-01-07 | 2022-05-13 | 中国农业大学 | Utilize bitter water desalination irrigation equipment of charcoal electrode adsorption salt ion |
| CN114920336A (en) * | 2022-03-15 | 2022-08-19 | 中国船舶重工集团公司第七一八研究所 | Preparation method of capacitive deionization electrode |
| CN117550598A (en) * | 2023-11-15 | 2024-02-13 | 昆明理工大学 | Preparation method of arundo donax biomass porous carbon and application of arundo donax biomass porous carbon in silicon-carbon negative electrode of lithium ion battery |
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| CN117550598A (en) * | 2023-11-15 | 2024-02-13 | 昆明理工大学 | Preparation method of arundo donax biomass porous carbon and application of arundo donax biomass porous carbon in silicon-carbon negative electrode of lithium ion battery |
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Application publication date: 20200501 |