CN111137886A - Method for preparing electrode material by aquatic plant - Google Patents
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- CN111137886A CN111137886A CN201911131785.5A CN201911131785A CN111137886A CN 111137886 A CN111137886 A CN 111137886A CN 201911131785 A CN201911131785 A CN 201911131785A CN 111137886 A CN111137886 A CN 111137886A
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Abstract
一种水生植物制备电极材料的方法，按照所述方法，将慈姑收获后的茎叶用去离子水洗净并烘干，碾成碎末；将碎末与KOH溶液按一定质量比充分混合并常温搅拌，获得混合物；将混合物放入反应釜中通入氨气加热并搅拌，反应结束后，通水冷却并过滤分离得到固体产物；将固体产物脱水干燥后与L–谷胱甘肽按一定质量比混合研磨均匀，放入管式炉中，通入N2，分段加热、保温、反应结束，通过HCl和去离子水冲洗，并脱水干燥得到慈姑基电极材料。本发明利用慈姑废物具有丰富的N、P杂原子结构，进一步掺杂氮原子使交联反应更加充分，资源利用率较高，有机结合分段活化方法以及活化过程中氮气气氛，有效提高了产物的电化学性能，应用前景广阔。A method for preparing electrode materials from aquatic plants. According to the method, the harvested stems and leaves of Cigu are washed with deionized water, dried, and ground into powder; the powder and KOH solution are fully mixed according to a certain mass ratio and Stir at room temperature to obtain a mixture; put the mixture into the reactor and feed it with ammonia to heat and stir, after the reaction is completed, cool with water and filter and separate to obtain a solid product; dehydrate the solid product and dry it with L-glutathione according to a certain amount. The mass ratio was mixed and ground evenly, put into a tube furnace, fed with N 2 , heated in stages, kept warm, the reaction was completed, rinsed with HCl and deionized water, and dehydrated and dried to obtain a cystein-based electrode material. The present invention utilizes the rich N and P heteroatomic structure of cigu waste, further doped nitrogen atoms to make the cross-linking reaction more sufficient, the resource utilization rate is higher, and the organic combination of the staged activation method and the nitrogen atmosphere in the activation process effectively improves the product quality. The electrochemical performance is broad and the application prospect is broad.
Description
Technical Field
The invention belongs to the field of preparation of biomass energy materials, and particularly relates to a method for preparing an electrode material by using aquatic plants.
Background
Biomass is the only renewable carbon source in the nature, and has wide distribution and environmental friendliness. China is a big agricultural country, biomass resources are rich, the yield of crop straws is about 7.2 hundred million tons every year, and the forestry residue resources are as high as 3 hundred million tons. The method develops an efficient biomass resource utilization technology, realizes the clean conversion and reasonable utilization of biomass energy, and has important significance for improving the energy structure of China, controlling the pollutant emission level and promoting the coordinated development of economy, society and environment.
The hydrothermal carbonization of biomass is one of the current ways for effectively utilizing biomass, can achieve the purposes of carbon fixation and biomass energy utilization, and is rapidly developed in recent years. The biomass is quickly converted into the carbon-rich solid water hot coke by using hot water at a certain temperature, and the carbon-rich solid water hot coke can be used as fuel and energy materials, can also be used as raw materials for pyrolysis and gasification, soil conditioners, and can also be used as adsorbing materials for heavy metals and organic pesticides in soil and water bodies.
Compared with other biomass treatment technologies such as pyrolysis, gasification and the like, the hydrothermal carbonization technology has the advantages of simple process, low cost, high carbon content of solid products and wide application field, and has great development potential and application value for dealing with energy shortage and environmental pollution. Through a series of researches, the biomass is subjected to hydrolysis, dehydration, decarboxylation, polycondensation and aromatization reactions in the hydrothermal carbonization process, and finally forms hydrothermal coke as a solid product, a partial liquid-phase product and a small amount of gas. The series of simultaneous chemical reaction paths are closely related to reaction conditions and raw material characteristics, and how to match the product application with operation parameters and raw material characteristics is always the key for popularization and application of the technology.
The arrowhead is a perennial herbaceous plant, most aquatic vegetables are eaten at the roots, the edible roots are removed in the harvest season, other parts are discarded as waste, and the arrowhead is rich in heteroatoms such as N, P due to the fact that abundant organic matters are needed for growth of the arrowhead, if the arrowhead is combined with hydrothermal reaction conditions, the arrowhead waste is effectively treated, the arrowhead waste is promoted to be effectively converted into a carbon material with abundant pore structures and electrochemical properties, and the arrowhead has wide application prospects and social and environmental benefits.
Disclosure of Invention
The invention aims to provide a method for preparing an electrode material by using aquatic plants, which realizes high-value utilization by utilizing the characteristic of rich N, P atoms. The prepared carbon material has a porous structure and good electrochemical performance.
The technical scheme of the invention is as follows: a method for preparing electrode material by aquatic plants comprises the following steps:
(1) cleaning harvested stems and leaves of arrowhead, drying and crushing to obtain minced stems and leaves of arrowhead;
(2) fully mixing the minced stem and leaf of the arrowhead obtained in the step (1) with KOH solution, and stirring at normal temperature to obtain a mixture;
(3) putting the mixture obtained in the step (2) into a reaction kettle, sealing the kettle body, introducing ammonia gas into the reaction kettle, starting magnetic stirring, heating to enable the mixture to generate aromatization reaction, immediately cooling by cooling water after the reaction is finished, filtering and separating the hydrothermal product to obtain a solid product, and dehydrating and drying;
(4) mixing and grinding the solid product dried in the step (3) and L-glutathione uniformly to obtain a mixture;
(5) putting the mixture obtained in the step (4) into a tube furnace, and introducing N2And after the step of heating, heat preservation and reaction, washing by HCl and deionized water, and dehydrating and drying to obtain the electrode material.
The concentration of the KOH solution in the step (2) is 1-2 mol/L, and the mass ratio of the KOH solution to the arrowhead powder is 1-3: 1.
And (3) introducing ammonia gas into the reaction kettle in the step (3) at a pressure of 20-25 MPa in the reaction kettle, and rotating speed of the magnetic stirrer of 2000-3000 r/min.
The heating temperature in the step (3) is 220-250 ℃, and the retention time is 45-90 minutes.
And (4) drying the solid product in the step (3) at the temperature of 85-95 ℃ for 10-12 hours.
The mass ratio of the solid product to the L-glutathione in the step (4) is 1: 1-2.
The step (5) of heating the tube-type furnace in a segmented mode is two-stage heating, the first stage heating temperature is 800 ℃, and the residence time is 10 minutes; the second stage heating temperature is 950 ℃, the retention time is 150 minutes, N2The mass flow is 50mL/min, and the heating rate is 15-20 ℃/min.
In the step (5), the HCl concentration is 0.5-1 mol/L, and the deionized water is washed to be neutral.
Advantageous effects
(1) The invention provides a method for preparing an electrode material by using aquatic plants, wherein a carbon material prepared by the method has a porous structure, and the charge and discharge test shows that when the current density is 5A/g, the specific capacitance is still kept above 230F/g after 1000 cycles.
(2) The raw material arrowhead selected by the invention belongs to aquatic plants, has high water content, adopts a hydrothermal carbonization technology, does not need extra drying and has low energy consumption.
(3) According to the invention, ammonia gas is introduced in the hydrothermal carbonization process and L-glutathione is doped before activation, so that organic combination of nitrogen supply and the process is realized, and higher specific capacity of the pseudo capacitor is provided.
(4) The raw material arrowhead of the invention contains rich nitrogen and phosphorus (the N, P content is respectively about 3 percent and 0.14 percent), and the mass specific capacitance is improved by 12 percent compared with that of arrowhead which does not adopt the process by organically combining a segmented activation method and a nitrogen atmosphere in the activation process.
Detailed Description
In order to better understand the present invention, the following examples further illustrate the present invention in detail.
A method for preparing electrode material by aquatic plants comprises the following steps:
(1) washing harvested stems and leaves of arrowheads with deionized water, drying for 14 hours at 80 ℃ by using a blast drier, and crushing into powder with the diameter of less than 5 mm;
(2) fully mixing the minced stem and leaf of the arrowhead obtained in the step (1) and KOH solution according to a certain mass ratio, and stirring for 30-60 minutes at normal temperature to obtain a mixture;
(3) putting the mixture obtained in the step (2) into a reaction kettle, sealing the kettle body, introducing ammonia gas into the reaction kettle, starting magnetic stirring, heating to enable the mixture to generate aromatization reaction, immediately cooling by cooling water after the reaction is finished, filtering and separating the hydrothermal product to obtain a solid product, and dehydrating and drying;
(4) mixing and uniformly grinding the solid product dried in the step (3) and L-glutathione according to a certain mass ratio to obtain a mixture;
(5) putting the mixture obtained in the step (4) into a tube furnace, and introducing N2And after the step of heating, heat preservation and reaction, washing by HCl and deionized water, and dehydrating and drying to obtain the electrode material.
The concentration of the KOH solution in the step (2) is 1-2 mol/L, and the mass ratio of the KOH solution to the arrowhead powder is 1-3: 1.
And (3) introducing ammonia gas into the reaction kettle in the step (3) at a pressure of 20-25 MPa in the reaction kettle, and rotating speed of the magnetic stirrer of 2000-3000 r/min.
The heating temperature in the step (3) is 220-250 ℃, and the retention time is 45-90 minutes.
And (4) drying the solid product in the step (3) at the temperature of 85-95 ℃ for 10-12 hours.
The mass ratio of the solid product to the L-glutathione in the step (4) is 1: 1-2.
The step (5) of heating the tube-type furnace in a segmented mode is two-stage heating, the first stage heating temperature is 800 ℃, and the residence time is 10 minutes; the second stage heating temperature is 950 ℃, the retention time is 150 minutes, N2The mass flow is 50mL/min, and the heating rate is 15-20 ℃/min.
In the step (5), the HCl concentration is 0.5-1 mol/L, and the deionized water is washed to be neutral.
The arrowhead-based electrode material has good electrochemical performance and can be applied as an electrode material.
The first embodiment is as follows:
washing 10 g of harvested stem leaves of sagittaria sagittifolia with deionized water, putting the cleaned stem leaves into a forced air drier, drying the stem leaves for 14 hours at the temperature of 80 ℃, and crushing the stem leaves into powder with the diameter of less than 5 mm; fully mixing the powder with 1mol/L KOH solution according to the mass ratio of 1:1, and stirring for 30 minutes at normal temperature to obtain a mixture; putting the mixture into a reaction kettle, sealing the kettle body, introducing ammonia gas to make the pressure reach 20MPa, starting magnetic stirring, and controlling the rotating speed at 2000 revolutions per minute; heat to 220 ℃ and incubate for 45 minutes. After the reaction is finished, cooling by cooling water, filtering and separating the hydrothermal product to obtain a solid product, and drying the solid product at 85 ℃ for 10 hours; mixing and grinding the dried solid product and L-glutathione powder uniformly according to the mass ratio of 1:1 to obtain a mixture; placing the mixture into a tube furnace and introducing N2The mass flow is 50mL/min, then the heating is carried out in sections, the first section heating temperature is 800 ℃, and the temperature is kept for 10 minutes; the second stage heating temperature is 950 ℃ and the temperature is kept for 150 minutes, and the heating rate is 15 ℃/min. After the reaction is finished, washing the electrode material by using HCL solution with the concentration of 0.5mol/L, then washing the electrode material to be neutral by using deionized water, and dehydrating and drying the electrode material to obtain the arrowhead-based electrode material.
The cyclic voltammetry test shows that under the current density of 5A/g, the mass specific capacitance can be maintained at 240F/g after 1000 cycles of charging and discharging.
Example two:
washing 10 g of harvested stem leaves of sagittaria sagittifolia with deionized water, putting the cleaned stem leaves into a forced air drier, drying the stem leaves for 14 hours at the temperature of 80 ℃, and crushing the stem leaves into powder with the diameter of less than 5 mm; fully mixing the powder with 2mol/L KOH solution according to the mass ratio of 1:1, and stirring for 30 minutes at normal temperature to obtain a mixture; putting the mixture into a reaction kettle, sealing the kettle body, introducing ammonia gas to make the pressure reach 20MPa, starting magnetic stirring, and controlling the rotating speed at 2000 revolutions per minute; heat to 220 ℃ and incubate for 45 minutes. After the reaction is finished, cooling by cooling water, filtering and separating the hydrothermal product to obtain a solid product, and drying the solid product at 85 ℃ for 10 hours; mixing and grinding the dried solid product and L-glutathione powder uniformly according to the mass ratio of 1:1 to obtain a mixture; placing the mixture into a tube furnace and introducing N2Mass flow rate of 50mLMin, then heating in a sectional way, wherein the first-stage heating temperature is 800 ℃ and keeping the temperature for 10 minutes; the second stage heating temperature is 950 ℃ and the temperature is kept for 150 minutes, and the heating rate is 15 ℃/min. After the reaction is finished, washing the electrode material by using HCL solution with the concentration of 0.5mol/L, then washing the electrode material to be neutral by using deionized water, and dehydrating and drying the electrode material to obtain the arrowhead-based electrode material.
The cyclic voltammetry test shows that the mass specific capacitance can be still maintained at 241F/g after 1000 cycles of charging and discharging under the current density of 5A/g.
Example three:
washing 10 g of harvested stem leaves of sagittaria sagittifolia with deionized water, putting the cleaned stem leaves into a forced air drier, drying the stem leaves for 14 hours at the temperature of 80 ℃, and crushing the stem leaves into powder with the diameter of less than 5 mm; fully mixing the powder with 1.5mol/L KOH solution according to the mass ratio of 1:3, and stirring for 30 minutes at normal temperature to obtain a mixture; putting the mixture into a reaction kettle, sealing the kettle body, introducing ammonia gas to make the pressure reach 22MPa, starting magnetic stirring, and rotating at 2500 rpm; heat to 220 ℃ and incubate for 90 minutes. After the reaction is finished, cooling by cooling water, filtering and separating the hydrothermal product to obtain a solid product, and drying the solid product at 85 ℃ for 10 hours; mixing and grinding the dried solid product and L-glutathione powder uniformly according to the mass ratio of 1:2 to obtain a mixture; placing the mixture into a tube furnace and introducing N2The mass flow is 50mL/min, then the heating is carried out in sections, the first section heating temperature is 800 ℃, and the temperature is kept for 10 minutes; the second stage heating temperature is 950 ℃ and the temperature is kept for 150 minutes, and the heating rate is 15 ℃/min. After the reaction is finished, washing the electrode material by using HCL solution with the concentration of 0.5mol/L, then washing the electrode material to be neutral by using deionized water, and dehydrating and drying the electrode material to obtain the arrowhead-based electrode material.
The cyclic voltammetry test shows that the mass specific capacitance can be maintained at 236F/g after 1000 cycles of charging and discharging under the current density of 5A/g.
Example four:
washing 10 g of harvested stem leaves of sagittaria sagittifolia with deionized water, putting the cleaned stem leaves into a forced air drier, drying the stem leaves for 14 hours at the temperature of 80 ℃, and crushing the stem leaves into powder with the diameter of less than 5 mm; fully mixing the powder with 2mol/L KOH solution according to the mass ratio of 1:2Mixing, and stirring for 40 minutes at normal temperature to obtain a mixture; putting the mixture into a reaction kettle, sealing the kettle body, introducing ammonia gas to make the pressure reach 25MPa, starting magnetic stirring, and rotating at 3000 r/min; heat to 230 ℃ and incubate for 60 minutes. After the reaction is finished, cooling by cooling water, filtering and separating the hydrothermal product to obtain a solid product, and drying the solid product at 85 ℃ for 10 hours; mixing and grinding the dried solid product and L-glutathione powder uniformly according to the mass ratio of 1:1 to obtain a mixture; placing the mixture into a tube furnace and introducing N2The mass flow is 50mL/min, then the heating is carried out in sections, the first section heating temperature is 800 ℃, and the temperature is kept for 10 minutes; the second stage heating temperature is 950 ℃ and the temperature is kept for 150 minutes, and the heating rate is 20 ℃/min. After the reaction is finished, washing the electrode material by using HCL solution with the concentration of 0.5mol/L, then washing the electrode material to be neutral by using deionized water, and dehydrating and drying the electrode material to obtain the arrowhead-based electrode material.
The cyclic voltammetry test shows that under the current density of 5A/g, the mass specific capacitance can still be maintained at 242F/g after 1000 cycles of charging and discharging.
Example five:
washing 10 g of harvested stem leaves of sagittaria sagittifolia with deionized water, putting the cleaned stem leaves into a forced air drier, drying the stem leaves for 14 hours at the temperature of 80 ℃, and crushing the stem leaves into powder with the diameter of less than 5 mm; fully mixing the powder with 1.8mol/L KOH solution according to the mass ratio of 1:3, and stirring for 40 minutes at normal temperature to obtain a mixture; putting the mixture into a reaction kettle, sealing the kettle body, introducing ammonia gas to make the pressure reach 23MPa, starting magnetic stirring, and making the rotating speed be 3500 rpm; heat to 240 ℃ and incubate for 60 minutes. After the reaction is finished, cooling by cooling water, filtering and separating the hydrothermal product to obtain a solid product, and drying the solid product at 85 ℃ for 10 hours; mixing and grinding the dried solid product and L-glutathione powder uniformly according to the mass ratio of 1:1.2 to obtain a mixture; placing the mixture into a tube furnace and introducing N2The mass flow is 50mL/min, then the heating is carried out in sections, the first section heating temperature is 800 ℃, and the temperature is kept for 10 minutes; the second stage heating temperature is 950 ℃ and the temperature is kept for 150 minutes, and the heating rate is 15 ℃/min. After the reaction is finished, washing with HCL solution with the concentration of 0.8mol/L, and then washing with HCL solutionWashing the electrode material with deionized water to be neutral, dehydrating and drying to obtain the arrowhead-based electrode material.
The cyclic voltammetry test shows that the mass specific capacitance can be still maintained at 241F/g after 1000 cycles of charging and discharging under the current density of 5A/g.
Example six:
washing 10 g of harvested stem leaves of sagittaria sagittifolia with deionized water, putting the cleaned stem leaves into a forced air drier, drying the stem leaves for 14 hours at the temperature of 80 ℃, and crushing the stem leaves into powder with the diameter of less than 5 mm; fully mixing the powder with 1.7mol/L KOH solution according to the mass ratio of 1:1, and stirring for 50 minutes at normal temperature to obtain a mixture; putting the mixture into a reaction kettle, sealing the kettle body, introducing ammonia gas to make the pressure reach 23MPa, starting magnetic stirring, and controlling the rotating speed at 4000 revolutions per minute; heat to 250 ℃ and incubate for 70 minutes. After the reaction is finished, cooling by cooling water, filtering and separating the hydrothermal product to obtain a solid product, and drying the solid product at 85 ℃ for 10 hours; mixing and grinding the dried solid product and L-glutathione powder uniformly according to the mass ratio of 1:2 to obtain a mixture; placing the mixture into a tube furnace and introducing N2The mass flow is 50mL/min, then the heating is carried out in sections, the first section heating temperature is 800 ℃, and the temperature is kept for 10 minutes; the second stage heating temperature is 950 ℃ and the temperature is kept for 150 minutes, and the heating rate is 15 ℃/min. After the reaction is finished, washing the electrode material by using HCL solution with the concentration of 1mol/L, then washing the electrode material to be neutral by using deionized water, and dehydrating and drying the electrode material to obtain the arrowhead-based electrode material.
Comparative example: and (3) putting the mixture into a tubular furnace, introducing air into the tubular furnace at the mass flow rate of 50mL/min, heating the mixture to 450 ℃ and keeping the temperature for 60 minutes under the same other reaction conditions. After the reaction is finished, washing the electrode material by using HCL solution with the concentration of 1mol/L, then washing the electrode material to be neutral by using deionized water, and dehydrating and drying the electrode material to obtain the arrowhead-based electrode material.
The cyclic voltammetry test shows that under the current density of 5A/g, the mass specific capacitance can still be kept at 245F/g after 1000 cycles of charging and discharging. The electrode material obtained in the comparative example maintained a mass specific capacitance of 215F/g under the same test conditions.
Claims (8)
1. A method for preparing electrode material by aquatic plant is characterized by comprising the following steps:
(1) cleaning harvested stems and leaves of arrowhead, drying and crushing to obtain minced stems and leaves of arrowhead;
(2) fully mixing the minced stem and leaf of the arrowhead obtained in the step (1) with KOH solution, and stirring at normal temperature to obtain a mixture;
(3) putting the mixture obtained in the step (2) into a reaction kettle, sealing the kettle body, introducing ammonia gas into the reaction kettle, starting magnetic stirring, heating to enable the mixture to generate aromatization reaction, immediately cooling by cooling water after the reaction is finished, filtering and separating the hydrothermal product to obtain a solid product, and dehydrating and drying;
(4) mixing and uniformly grinding the solid product dried in the step (3) and L-glutathione to obtain a mixture;
(5) putting the mixture obtained in the step (4) into a tube furnace, and introducing N2And after the segmented heating, heat preservation and reaction are finished, washing by HCl and deionized water, and dehydrating and drying to obtain the electrode material.
2. A method of preparing electrode material for aquatic plants according to claim 1, wherein: the concentration of the KOH solution in the step (2) is 1-2 mol/L, and the mass ratio of the KOH solution to the arrowhead powder is 1-3: 1.
3. A method of preparing electrode material for aquatic plants according to claim 1, wherein: and (3) introducing ammonia gas into the reaction kettle in the step (3) at a pressure of 20-25 MPa in the reaction kettle, and rotating speed of the magnetic stirrer of 2000-3000 r/min.
4. A method of preparing electrode material for aquatic plants according to claim 1, wherein: the heating temperature in the step (3) is 220-250 ℃, and the retention time is 45-90 minutes.
5. A method of preparing electrode material for aquatic plants according to claim 1, wherein: and (4) drying the solid product in the step (3) at the temperature of 85-95 ℃ for 10-12 hours.
6. A method of preparing electrode material for aquatic plants according to claim 1, wherein: the mass ratio of the solid product to the L-glutathione in the step (4) is 1: 1-2.
7. A method of preparing electrode material for aquatic plants according to claim 1, wherein: the step (5) of heating the tube-type furnace in a segmented mode is two-stage heating, the first stage heating temperature is 800 ℃, and the residence time is 10 minutes; the second stage heating temperature is 950 ℃, the retention time is 150 minutes, N2The mass flow is 50mL/min, and the heating rate is 15-20 ℃/min.
8. A method of preparing electrode material for aquatic plants according to claim 1, wherein: in the step (5), the HCl concentration is 0.5-1 mol/L, and the deionized water is washed to be neutral.
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