CN109942056B - Method for desalting biomass carbon electrode derived from sphagnum - Google Patents
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Abstract
本发明公开了海水淡化领域的一种用泥炭藓衍生的生物质碳电极除盐的方法，本方法具体步骤如下：步骤一，将泥炭藓进行碳化，得到碳化的生物碳后均匀研磨成粉末状；步骤二，将生物质碳、碳黑和PTFE按比例配制，随后将混合物质搅拌均匀；步骤三，将混合物质均匀涂抹在石墨纸表面，制成电极片，随后将电极片进行加热干燥；步骤四，将干燥后的电极片作为正极和负极，将两电极放入电除盐反应器中，利用蠕动泵将盐水泵入反应器并循环，电极两端施加电压进行除盐测试。本专利首次采用泥炭藓作为初始材料经过碳化过程制备了生物质衍生碳，利用这种生物质碳材料作为活性物质制备的CDI电极拥有大的比表面积，合理的孔结构以及优异的电导率和耐水性等优点。
The invention discloses a method for desalination by using sphagnum moss-derived biomass carbon electrodes in the field of seawater desalination. The specific steps of the method are as follows: step 1, carbonizing the sphagnum moss to obtain carbonized biological carbon and then evenly grinding it into powder. ; Step 2, prepare the biomass carbon, carbon black and PTFE in proportion, and then stir the mixed substance evenly; Step 3, spread the mixed substance evenly on the surface of the graphite paper to make an electrode sheet, and then heat and dry the electrode sheet; Step 4: Use the dried electrode sheet as the positive electrode and the negative electrode, put the two electrodes into the electro-demineralization reactor, use the peristaltic pump to pump the brine into the reactor and circulate, and apply a voltage to both ends of the electrodes to perform the demineralization test. This patent is the first time to use peat moss as the initial material to prepare biomass-derived carbon through the carbonization process. The CDI electrode prepared by using this biomass carbon material as the active material has a large specific surface area, a reasonable pore structure, and excellent electrical conductivity and water resistance. Sex and other advantages.
Description
Technical Field
The invention belongs to the field of seawater desalination, and particularly relates to a method for desalting by using a biomass carbon electrode derived from sphagnum moss.
Background
The shortage of water resources is one of the problems to be solved in the world, and seawater desalination is an effective way to alleviate the problem. Compared with traditional desalination technologies such as distillation, reverse osmosis and electrodialysis, Capacitive Deionization (CDI) technology has attracted attention in recent years due to its characteristics of low cost, low energy consumption and environmental friendliness. The working principle of the CDI is based on a double-electrode theory, and in the charging process, anions and cations in brine are respectively adsorbed on a positive electrode and a negative electrode; during the discharge, the adsorbed salt ions desorb back into the salt solution.
In general, the properties of CDI are closely related to the physical and structural properties of the electrode material. The ideal electrode material should have a large surface area, high conductivity and a suitable pore size distribution. Carbon materials are ideal electrode materials for CDI, and various forms of carbon materials such as activated carbon, carbon aerogel, ordered mesoporous carbon, carbon nanotubes, graphene, etc. have been widely studied and applied to CDI desalination to improve the desalination performance thereof. However, the materials have high cost and low yield, and a large amount of toxic and harmful reagents are used in the preparation process, so that secondary pollution is caused to the environment, and the wide application of the materials in CDI is limited.
In addition to the high performance of the electrode material, cost, sustainability, environmental friendliness, resource versatility, and simplicity of manufacture should all be considerations in the manufacturing process. The biomass has the characteristics of rich resources and low cost. The carbon material extracted from the biomass is widely applied to the fields of pollutant adsorption, fuel cells, electrochemical energy storage, sensors, hydrogen storage and the like, and makes an important contribution to the sustainable development of the environment. Thus, the use of sustainable biomass-derived carbon materials as CDI electrodes is also a viable approach.
Disclosure of Invention
In order to solve the above problems, the present invention has an object to use a carbon material extracted from biomass for CDI technology.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for desalting by using a peat moss derived biomass carbon electrode comprises the following steps,
firstly, pretreating sphagnum, soaking the sphagnum in ultrapure water for 24 hours to absorb enough water, and then freeze-drying the material by adopting a liquid nitrogen freeze-drying technology; carbonizing sphagnum to obtain carbonized biochar, and uniformly grinding into powder; the carbonization temperature of the step is 750-850 ℃, the reaction time is 2-3 hours, the atmosphere is nitrogen, and the heating rate is 3-4 ℃/min;
step two, mixing and preparing the biomass carbon, the carbon black and the PTFE, and then uniformly stirring the mixed substances, wherein the specific operation mode is as follows: firstly, mixing and uniformly stirring powdered biomass carbon and carbon black, then dispersing PTFE in ultrapure water, and finally pouring PTFE into uniformly mixed solid powder and mechanically stirring for 10-15 minutes;
uniformly coating the mixed substance on the surface of graphite paper to prepare an electrode plate, and then heating and drying the electrode plate, wherein the adopted heating device is a programming heating plate, the set temperature is 70-80 ℃, and the drying time is 3-4 hours; the specification of the graphite paper is 3cmx10cm, and the coating area of a slurry mixture formed by biomass carbon, carbon black and PTFE is 3cmx4 cm;
and step four, taking the dried electrode slices as a positive electrode and a negative electrode, putting the two electrodes into an electric desalting reactor, pumping saline water into the reactor by using a peristaltic pump and circulating, and applying voltage to the two ends of the electrodes to perform a desalting test.
After the scheme is adopted, the following beneficial effects are realized: 1. compared with a desalting electrode made of a common carbon material, the invention adopts carbonized peat moss as an electrode active material, is inspired by the biological water absorption characteristic of the peat moss (the peat moss can absorb water by 10-25 times of the weight of the peat moss), researches the biological water absorption characteristic of the peat moss to be the combined action of the pore structure and the specific surface area of the peat moss, and prepares the biomass carbon electrode according to the characteristic, which has larger specific surface area and proper pore diameter, thereby increasing the adsorption sites, shortening the ion transmission path and adsorbing more ions.
2. Compared with biomass carbon electrodes prepared by other characteristics, the biomass carbon derived from sphagnum has strong hydrophilicity, and the contact area of the biomass carbon electrode and seawater is increased; the ordered and densely distributed pore structure improves the transmission and diffusion capacity of ions, and meanwhile, the pore structure is convenient for the absorption and desorption of ions, so that the desalting efficiency is improved.
3. Compared with the prior art adopting other materials, the technical scheme utilizes carbon black as a conductive medium and PTFE (polytetrafluoroethylene) as an adhesive, so that the conductivity of the material is enhanced and the water resistance is improved.
4. Compared with the prior art of introducing toxic and harmful chemical reagents to manufacture electrodes, the biomass carbon electrode prepared by adopting the physical method in the technical scheme improves the environmental protection property and provides a reasonable and effective way for preparing green and low-cost carbon materials.
5. Compared with directly carbonized sphagnum moss, the cyclic voltammetry curve of the freeze-dried carbonized biomass carbon electrode is closer to a rectangle, which shows that the freeze-dried carbonized biomass carbon has more ideal double-electric-layer capacitance. And its specific capacitance is greater than that of the directly carbonized biomass carbon.
6. Compared with directly carbonized sphagnum, the freeze-dried carbonized biomass carbon electrode has smaller internal resistance and charge transfer resistance, and improves the conductivity.
7. Compared with directly carbonized sphagnum moss, the conductivity of the salt solution of the freeze-dried carbonized biomass carbon electrode is reduced faster than that of the directly carbonized biomass carbon in the desalting process, so that the biomass carbon electrode has a faster ion adsorption rate and higher desalting capability.
Further, in the step two, according to biomass carbon: carbon black: the ratio of PTFE was 8:1: 1.
Further, the circulation speed of the brine in the fourth step is 20-25mL min-1And the voltage applied to the two ends of the electrode is 1.2-1.5V during the desalting test.
Drawings
FIG. 1 is a schematic diagram of the operation of a prior art CDI;
FIG. 2 is a flowchart of a first embodiment;
FIG. 3 is a flowchart of the second embodiment;
FIG. 4 is a structural diagram of a scanning electron microscope of lyophilized carbonized sphagnum moss;
FIG. 5 is a structural diagram of a transmission electron microscope of freeze-dried carbonized sphagnum moss;
FIG. 6 is a cyclic voltammogram of a lyophilized carbonized biomass carbon electrode at different sweep rates;
FIG. 7 shows the scanning rate of 20mV s for the direct carbonization and the freeze-dried carbonization of biomass carbon electrode in 1.0M NaCl aqueous solution-1Cyclic voltammogram;
FIG. 8 is a plot of specific capacitance versus scan rate for direct carbonized and freeze dried carbonized biomass carbon electrodes;
FIG. 9 is an impedance curve of a direct carbonized and freeze-dried carbonized biomass carbon electrode in a 1.0M NaCl aqueous solution;
FIG. 10 is a plot of conductivity versus time in the desalting test for direct and freeze-dried carbonized biomass carbon electrodes;
FIG. 11 is a Kim-Yoon plot of the desalting test for the direct carbonized and freeze dried carbonized biomass carbon electrodes.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: salt solution 1, cleaning solution 2, anion 3, cation 4, positive electrode 5 and negative electrode 6.
The prior art is as follows:
as shown in the attached figure 1, the electric desalting principle mainly comprises two processes:
an adsorption process: an external electric field is applied to a pair of parallel electrodes, the salt solution 1 passes through the electrodes, and under the electrostatic action, anions 3 migrate to a positive electrode 5, and cations 4 migrate to a negative electrode 6. Finally, the concentration of the salt solution is continuously reduced to achieve the aim of desalting.
A desorption process: after the electrode is saturated, the electric field is removed, or the positive electrode 5 and the negative electrode 6 are interconnected, ions adsorbed on the electrode are released into the cleaning solution 2 due to the action of the lost electrostatic force, and the electrode is regenerated.
The first embodiment is as follows:
the embodiment is basically as shown in the attached figure 2: a method for desalting by using a peat moss derived biomass carbon electrode comprises the following steps:
firstly, material selection and instrument manufacturing: fresh sphagnum moss is selected as a basic material, and saline (NaCl aqueous solution, 250mg L) is used for the test-1) The auxiliary materials are ultrapure water, a nitrogen tank, graphite paper, carbon black and PTFE (polytetrafluoroethylene), and selected instruments are a tube furnace, a mortar, a programming heating plate, an electronic balance, a mechanical stirring tool, scissors, a medicine spoon, a beaker and a power supply.
Secondly, a carbonization stage: putting the sphagnum into a tubular furnace in a vacuum state, continuously introducing nitrogen into the tubular furnace by an operator to enable the nitrogen to serve as an atmosphere, then, presetting the heating rate of the tubular furnace to be 3 ℃/min by the operator, and carbonizing the sphagnum for two hours at the temperature of 800 ℃.
Thirdly, grinding and mixing stage: the operating personnel utilize electronic balance to weigh biomass carbon, carbon black and PTFE, biomass carbon: carbon black: the mass ratio of PTFE is 8:1:1, then the PTFE is dispersed in ultrapure water by an operator, the biomass carbon is ground by the other operators, then carbon black is mixed and stirred uniformly, finally the PTFE is poured into the uniformly mixed solid powder by the operator, and a slurry-shaped mixture is formed by stirring for 10 minutes by a mechanical stirring tool.
Fourthly, manufacturing the electrode: the operator lays the graphite paper flat on a table and cuts the graphite paper to a specification of 3cmx10cm, and then the operator uses a medicine spoon to evenly smear slurry mixture formed by mixing biomass carbon, carbon black and PTFE on the surface of the cut graphite paper, wherein the coating area of the slurry mixture is 3cmx4 cm. After the coating is finished, the graphite paper coated with the slurry mixture is placed on a programming heating plate for drying, the set temperature is 80 ℃, and the drying time is 3 hours.
And fifthly, desalting, namely taking the dried electrode plates as a positive electrode and a negative electrode, placing the two electrodes in an electric desalting reactor, pumping the saline water into the reactor by using a peristaltic pump, and circulating (the circulation speed is 25mL min)-1) A voltage (1.5V) was applied across the electrodes for salt removal testing.
Example two
As shown in fig. 3, the present embodiment is different from the first embodiment in that liquid nitrogen and tweezers are added to the selected apparatus, and the second embodiment is to pre-treat sphagnum before carbonization, soak the sphagnum in ultra-pure water for 24 hours to absorb enough moisture, and then freeze-dry the material by liquid nitrogen freeze-drying technology.
As shown in fig. 4, the lyophilized carbonized peat moss was observed under a scanning electron microscope. The surface of the sphagnum moss after absorbing the ultrapure water is completely unfolded, the pore size distribution is orderly, the structure is not collapsed, and the surface of the sphagnum moss has no obvious cracks under the quick-freezing effect of the liquid nitrogen.
The operator then observed the lyophilized carbonized peat moss under a transmission electron microscope to obtain a structural map as shown in fig. 5. The carbonized sphagnum has rich and ordered pore size distribution under high multiplying power.
As shown in fig. 6, the freeze-dried carbonized biomass carbon electrode is subjected to cyclic voltammetry tests at different sweep rates, so that cyclic voltammetry curves of the biomass carbon electrode at different sweep rates are shown, and the capacitance and energy storage effect of the biomass carbon are tested.
As shown in FIG. 7, the scanning rate of a direct carbonization/freeze-drying carbonization biomass carbon electrode in a 1.0M NaCl aqueous solution was 20mV s-1Cyclic voltammetry curve of (a). It can be clearly seen that the freeze-dried carbonized biomass carbon electrode curve is closer to a rectangle than the direct carbonization, indicating an ideal double layer capacitance phenomenon, and possessing a larger specific capacitance.
As shown in fig. 8, the specific capacitance of the biomass carbon electrode subjected to direct carbonization and freeze-drying carbonization varies with the scanning rate, and it can be seen from the specific capacitance of different biomass carbon electrodes varying with the scanning rate that the specific capacitance of the biomass carbon electrode subjected to freeze-drying carbonization is larger than that of the biomass carbon electrode subjected to direct carbonization at any scanning rate. Proves that compared with the biomass carbon directly carbonized, the biomass carbon freeze-dried and carbonized has better capacitance performance. More particularly at 2mV s-1The specific capacitance of freeze-drying carbonization can reach 192F g-1。
As shown in fig. 9, the impedance curves of the biomass carbon electrode subjected to direct carbonization and freeze-drying carbonization in the 1M NaCl solution are shown, the impedance graph is composed of a semicircle in the high-frequency region and a straight line in the low-frequency region, the semicircle in the high-frequency region of the freeze-drying carbonization is smaller, the slope of the inclined straight line in the low-frequency region is larger, and the intercept with the horizontal axis is smaller, which indicates that the biomass carbon electrode subjected to freeze-drying carbonization has smaller internal resistance and charge transfer resistance of the electrode, and the conductivity is good.
As shown in fig. 10, the NaCl solution conductivity curves during desalination for the direct carbonization and freeze-drying carbonization biomass carbon electrodes, and during the electric desalination, the conductivity of the NaCl solution decreases faster and more by freeze-drying carbonization biomass carbon electrodes. The freeze-dried carbonized biomass carbon electrode has a faster ion adsorption rate and higher desalting capability.
As shown in fig. 11, in the electric desalting, Kim-Yoon curve is used to describe the desalting capability of the electrode, and it can be seen that the freeze-dried carbonized biomass carbon electrode is located at the upper and lower positions compared with the curve of the directly carbonized electrode, indicating that the freeze-dried carbonized biomass carbon electrode has stronger desalting capability than the directly carbonized biomass carbon.
The sphagnum has strong water absorption capacity and can absorb water 10-25 times of the weight of the sphagnum. The biomass derived carbon is prepared by taking sphagnum as an initial material through a carbonization process for the first time, the biomass carbon material is used as an active substance, carbon black is used as a conductive agent, Polytetrafluoroethylene (PTFE) is used as a binder, the mixture is uniformly mixed and then coated on graphite paper, and a CDI electrode is obtained through a drying process. The prepared CDI electrode has the advantages of large specific surface area, reasonable pore structure, excellent conductivity and water resistance and the like.
When the electrode is applied to a desalting test, the biomass carbon electrode shows good desalting performance and cycling stability. The desalting amount can reach 10mg g-1. The working of the method has the advantages of abundant and easily obtained precursor materials, simple preparation, environmental protection and no use of any chemical reagent. The work provides a reasonable and effective way for preparing the green low-cost carbon material, and has great application potential in aspects of CDI, energy storage and the like.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (3)
1. A method for desalting by using a peat moss derived biomass carbon electrode, which is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
firstly, pretreating sphagnum, soaking the sphagnum in ultrapure water for 24 hours to absorb enough water, and then freeze-drying the material by adopting a liquid nitrogen freeze-drying technology; carbonizing sphagnum to obtain carbonized biochar, and uniformly grinding into powder; the carbonization temperature of the step is 750-850 ℃, the reaction time is 2-3 hours, the atmosphere is nitrogen, and the heating rate is 3-4 ℃/min;
step two, mixing and preparing the biomass carbon, the carbon black and the PTFE, and then uniformly stirring the mixed substances, wherein the specific operation mode is as follows: firstly, mixing and uniformly stirring powdered biomass carbon and carbon black, then dispersing PTFE in ultrapure water, and finally pouring PTFE into uniformly mixed solid powder and mechanically stirring for 10-15 minutes;
uniformly coating the mixed substance on the surface of graphite paper to prepare an electrode plate, and then heating and drying the electrode plate, wherein the adopted heating device is a programming heating plate, the set temperature is 70-80 ℃, and the drying time is 3-4 hours; the specification of the graphite paper is 3cmx10cm, and the coating area of a slurry mixture formed by biomass carbon, carbon black and PTFE is 3cmx4 cm;
and step four, taking the dried electrode slices as a positive electrode and a negative electrode, putting the two electrodes into an electric desalting reactor, pumping saline water into the reactor by using a peristaltic pump and circulating, and applying voltage to the two ends of the electrodes to perform a desalting test.
2. The method of claim 1, wherein the step of desalting comprises the steps of: biomass carbon in step two: carbon black: the mass ratio of PTFE is 8:1: 1.
3. The method of claim 1, wherein the step of desalting comprises the steps of:
the circulation speed of the brine in the fourth step is 20-25mL min-1And the voltage applied to the two ends of the electrode is 1.2-1.5V during the desalting test.
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| CN110526350A (en) * | 2019-09-05 | 2019-12-03 | 中南大学 | A kind of CDI multi-stage porous activated carbon electrodes and its preparation method and application using HAP cracking self-activation |
| CN111087054A (en) * | 2019-12-13 | 2020-05-01 | 黑龙江大学 | Simple preparation method for synthesizing electro-adsorption desalination electrode by carbonizing reed straw |
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| CN101343060A (en) * | 2008-08-01 | 2009-01-14 | 王德福 | Organic absorbent charcoal and preparing method |
| CN105788876A (en) * | 2016-03-09 | 2016-07-20 | 湘潭大学 | Process for preparing biomass porous nitrogen-doped carbon material and fabrication method of supercapacitor electrode |
| CN106299384A (en) * | 2016-10-14 | 2017-01-04 | 北京理工大学 | A kind of lithium sky anode electrode slice based on charcoal |
| CN108109853A (en) * | 2017-12-25 | 2018-06-01 | 武汉大学 | The preparation method and application of superelevation specific surface porous carbon biomass electrode material |
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| CN101343060A (en) * | 2008-08-01 | 2009-01-14 | 王德福 | Organic absorbent charcoal and preparing method |
| CN105788876A (en) * | 2016-03-09 | 2016-07-20 | 湘潭大学 | Process for preparing biomass porous nitrogen-doped carbon material and fabrication method of supercapacitor electrode |
| CN106299384A (en) * | 2016-10-14 | 2017-01-04 | 北京理工大学 | A kind of lithium sky anode electrode slice based on charcoal |
| CN108109853A (en) * | 2017-12-25 | 2018-06-01 | 武汉大学 | The preparation method and application of superelevation specific surface porous carbon biomass electrode material |
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