CN114132916A - Method for preparing metal ion battery negative electrode material by using livestock and poultry manure organic fertilizer - Google Patents
Method for preparing metal ion battery negative electrode material by using livestock and poultry manure organic fertilizer Download PDFInfo
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- 239000007773 negative electrode material Substances 0.000 title claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 48
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- 150000002500 ions Chemical class 0.000 abstract description 5
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- 239000011574 phosphorus Substances 0.000 abstract description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 3
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for preparing a metal ion battery cathode material by using livestock and poultry manure organic fertilizer, belonging to the field of new energy ion batteries. Carrying out solid-liquid separation on the livestock manure, drying, cleaning, drying again and crushing; adding strong acid/strong base solution into the powder particles for ultrasonic mixing, drying the mixture, and then carrying out high-temperature carbonization treatment on the dried product in an inert atmosphere; and finally neutralizing the product to be neutral, cleaning, drying, grinding and sieving to obtain the cathode material which can be used for metal ion batteries. According to the invention, the agricultural organic fertilizer is recycled, the diffusion and transfer of lithium, potassium, sodium and the like are enhanced by the prepared porous carbon material sites, the cycle and rate capability of the negative electrode material are effectively improved, and the electrochemical performance of the material can be improved by the trace nitrogen and phosphorus elements contained in the porous carbon material sites. The preparation method has the advantages of green and environment-friendly raw materials, simple process, easily-controlled process, low energy consumption, no toxicity and no pollution in the production process, and belongs to an environment-friendly green process.
Description
Technical Field
The invention belongs to the field of new energy ion batteries, and particularly relates to a method for preparing a metal ion battery cathode material by using livestock and poultry manure organic fertilizer.
Background
The livestock and poultry manure contains protein, fat, organic acid, cellulose, hemicellulose, inorganic salt and the like, wherein the organic matter is 15-25.5%, and the livestock and poultry manure also contains 0.5-1.63% of abundant nitrogen, 0.5-1.54% of phosphorus, 0.35-0.85% of potassium and 11% of carbohydrate. Although the livestock manure can effectively improve the fertility of soil, the hidden danger of the manure cannot be ignored, such as the manure which is not decomposed, particularly the poultry manure has heavy salt content and is easy to salinize the soil; more germs, worm eggs, weed seeds and the like in the excrement of the livestock and the poultry are easy to bring adverse effects to plants, and cause plant diseases and insect pests; contains heavy metals, antibiotics and the like, can poison plants and influence the safety of agricultural products. The conventional treatment method of the livestock and poultry manure is to directly discharge the livestock and poultry manure into a soil field, and no treatment method with high added value exists at present.
Many carbonaceous ion battery negative electrode materials having various structures, such as heteroatom-doped carbonaceous materials, hard carbon, graphene and carbon fibers, have been studied. Among these materials, the three-dimensional hierarchical porous carbon material has a large specific surface area, high conductivity, good chemical stability and low cost, and is a very promising candidate material for commercial ion batteries, and has high ion battery capacity and excellent cycling stability.
In the traditional method, a biomass raw material is often adopted to prepare the porous carbon anode material, but the content of trace elements is very low, and a nitrogen source and a phosphorus source material are required to be additionally added. Few reports exist at present for preparing agricultural organic fertilizers into battery materials.
Disclosure of Invention
According to the needs and the defects in the field, the invention provides a method for preparing a metal ion battery anode material by using an animal manure organic fertilizer.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a metal ion battery cathode material by using livestock and poultry manure organic fertilizer comprises the following steps:
(1) carrying out solid-liquid separation on livestock manure collected from a farm, outputting dry solid, drying, cleaning, drying again, and crushing the dry solid into powder particles of 50-80 meshes;
(2) adding strong acid or strong base solution into the powder particles for ultrasonic mixing, putting the obtained mixture into an oven for drying, putting the obtained dried substance into heating equipment, and carrying out high-temperature carbonization treatment in an inert atmosphere;
(3) neutralizing the product with acidic solution or alkaline solution to neutrality, cleaning, drying, grinding and sieving to obtain the negative electrode material for the related metal ion battery.
In the step (1), the solid-liquid separation method is one of a decantation method, a filtration method, a centrifugal separation method and a gravity settling method; the drying method of the dry solid is a mechanical dehydration method, a heating drying method, a chemical dehumidification method and the like.
In the step (1), the drying equipment is a dehumidifying dryer, a rotary wheel type dryer, a low-pressure dryer, a vacuum dryer, a compressed air dryer and the like; the drying temperature is 100 ℃ and 150 ℃, and the moisture content is less than 2 percent.
In the step (1), the solid cleaning is carried out by using clean water, and the process of drying again is the same as the first time; the crushing equipment is a tooth type crusher, a hammer type crusher, a knife type crusher, a turbine type crusher, a press grinding type crusher, milling type crushing, a ball mill and the like; the grinding time is 1-2 hours.
In the step (2), the acid is hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, oxalic acid, carbonic acid and the like; the alkali is lithium hydroxide, sodium hydroxide, potassium hydroxide, ammonia water, etc.; the concentration of the acid or the alkali is 90-99%.
In the step (2), the mass ratio of the acid (or alkali) to the powder particles is (1-20): 100, respectively; the ultrasonic mixing time is 1-3 hours; the drying is carried out by adopting an air-blast drying oven, the temperature of the air-blast drying oven is 100-120 ℃, and the drying time is 12 hours.
In the step (2), the inert atmosphere is nitrogen or argon, the heating equipment is a microwave oven, a muffle furnace, a tube furnace and the like, the heating rate is 5-10 ℃/min, the heating temperature is 1000-1500 ℃, and the heat preservation time is 0.5-2 h.
In the step (3), the acidic solution is selected from one of dilute hydrochloric acid, dilute sulfuric acid and dilute nitric acid; the alkaline solution is one of sodium hydroxide, potassium hydroxide and ammonia water solution; the concentration of the acidic solution or the alkaline solution is less than 0.8%; the cleaning solution is pure water, ultrapure water, deionized water, distilled water and the like; the pH value is between 6 and 7.
In the step (3), the drying is performed by adopting a vacuum drying oven, the drying temperature is 100 ℃ and 120 ℃, and the drying time is 12 hours; grinding for 1-2h, and sieving to obtain particles with size of more than 200 meshes; the metal ion battery is a lithium ion battery, a sodium ion battery, a potassium ion battery and the like.
According to the invention, the agricultural organic fertilizer is effectively recycled, the diffusion and transfer of lithium, potassium, sodium and the like are enhanced by the prepared porous carbon material sites, the cycle and rate capability of the negative electrode material are effectively improved, and the electrochemical performance of the material can be improved by the trace nitrogen and phosphorus elements contained in the porous carbon material sites. The preparation method has the advantages of green and environment-friendly raw materials, simple process, easily-controlled process, low energy consumption, no toxicity and no pollution in the production process, belongs to an environment-friendly green process, and is easy for large-scale production and popularization.
Drawings
FIG. 1 is a topographical map of a porous carbon material prepared in example 1 of the present invention.
Fig. 2 is reported data for specific surface area and pore volume of porous carbon prepared in example 1 of the present invention.
FIG. 3 is charge and discharge data of the composite material prepared in example 1 of the present invention.
Detailed Description
In the following examples, the solid-liquid separation method is one of decantation, filtration, centrifugal separation and gravity settling; the drying method of the dry solid is a mechanical dehydration method, a heating drying method, a chemical dehumidification method and the like. The drying equipment is a dehumidifying dryer, a rotary wheel dryer, a low-pressure dryer, a vacuum dryer, a compressed air dryer and the like. The crushing equipment adopts a tooth type crusher, a hammer type crusher, a knife type crusher, a turbine type crusher, a press grinding type crusher, milling type crushing, a ball mill and the like.
Example 1
Method for preparing metal ion battery negative electrode material by using livestock and poultry manure organic fertilizer
The livestock manure collected from a farm is subjected to solid-liquid separation by adopting a filtration method, dry solid is output by heating and drying, the dry solid is dried at 150 ℃ until the moisture content is less than 2%, and then the dry solid is cleaned, dried again, ground for 2 hours by a ball mill and crushed into 50-mesh powder particles. Adding a hydrochloric acid solution with the concentration of 99% into the powder particles according to the mass ratio of 20: 100 (acid: powder) for ultrasonic mixing for 3h, putting the mixture into a 120 ℃ oven for drying, putting the dried material into a tubular furnace, performing high-temperature carbonization treatment in an inert atmosphere, wherein the heating rate is 2 ℃/min, the heating temperature is 1000 ℃, and the heat preservation time is 2 h. And finally neutralizing the product with acid and alkali to be neutral, washing with deionized water, drying at 120 ℃, grinding for 2h, and sieving to select particles with the size of more than 200 meshes to obtain the sodium-ion battery cathode material.
Fig. 2 is reported data of the specific surface area and pore volume of the porous carbon prepared in example 1, and shows that the negative electrode material of the sodium-ion battery prepared in the example has a large amount of mesopores and a large specific surface area, and can promote the transmission of metal ions, so that the electrochemical performance of the material can be improved. Example 2
Method for preparing metal ion battery negative electrode material by using livestock and poultry manure organic fertilizer
The livestock manure collected from a farm is subjected to solid-liquid separation by adopting a filtration method, dry solid is output by heating and drying, the dry solid is dried at 150 ℃ until the moisture content is less than 2%, and then the dry solid is cleaned, dried again and ground for 1 hour by a ball mill to be crushed into 80-mesh powder particles. Adding 99% sodium hydroxide solution into the powder particles according to the mass ratio of 10: 100 (alkali: powder) for ultrasonic mixing for 2h, putting the mixture into a 120 ℃ oven for drying, putting the dried material into a tubular furnace, and performing high-temperature carbonization treatment under the inert atmosphere, wherein the heating rate is 5 ℃/min, the heating temperature is 800 ℃, and the heat preservation time is 2 h. Neutralizing the product with acid and alkali to neutrality, washing with deionized water, drying at 120 deg.C, grinding for 2 hr, and sieving to obtain particles of 200 meshes.
Example 3
Method for preparing metal ion battery negative electrode material by using livestock and poultry manure organic fertilizer
The livestock manure collected from a farm is subjected to solid-liquid separation by adopting a filtration method, dried solid is output by heating and drying, and is dried at 100 ℃, the moisture content is less than 3%, and the dried solid is cleaned, dried again, ground for 2 hours by a ball mill and crushed into 60-mesh powder particles. Adding a hydrochloric acid solution with the concentration of 98% into the powder particles according to the mass ratio of 15: 100 (acid: powder) for ultrasonic mixing for 3h, putting the mixture into a 120 ℃ oven for drying for 3, putting the dried material into a tubular furnace, performing high-temperature carbonization treatment under the inert atmosphere, wherein the heating rate is 5 ℃/min, the heating temperature is 1500 ℃, and the heat preservation time is 2 h. Neutralizing the product with acid and alkali to neutrality, washing with deionized water, drying at 120 deg.C, grinding for 2 hr, sieving to obtain particles of 300 mesh size, and making into potassium ion battery negative electrode material.
Claims (10)
1. A method for preparing a metal ion battery cathode material by using livestock and poultry manure organic fertilizer is characterized by comprising the following steps:
(1) carrying out solid-liquid separation on livestock manure collected from a farm, outputting dry solid, drying, cleaning, drying again, and crushing the dry solid into powder particles of 50-80 meshes;
(2) adding strong acid or strong base solution into the powder particles for ultrasonic mixing, putting the obtained mixture into an oven for drying, putting the obtained dried substance into heating equipment, and carrying out high-temperature carbonization treatment in an inert atmosphere;
(3) neutralizing the product with an acidic solution or an alkaline solution to be neutral, cleaning, drying, grinding and sieving to obtain the cathode material.
2. The method for preparing the metal ion battery anode material from the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (1), the solid-liquid separation method is one of decantation, filtration, centrifugal separation and gravity settling; the drying method of the dry solid is a mechanical dehydration method, a heating drying method or a chemical dehumidification method.
3. The method for preparing the metal ion battery anode material by using the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (1), the drying equipment is a dehumidifying dryer, a rotary wheel dryer, a low-pressure dryer, a vacuum dryer or a compressed air dryer, etc.; the drying temperature is 100 ℃ and 150 ℃, and the drying is carried out until the moisture content of the material is less than 2 percent.
4. The method for preparing the metal ion battery negative electrode material from the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (1), the crushing equipment is a tooth type crusher, a hammer type crusher, a knife type crusher, a turbine type crusher, a press grinding type crusher, a milling type crusher or a ball mill.
5. The method for preparing the metal ion battery anode material from the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (2), the acid is hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, oxalic acid or carbonic acid; the alkali is lithium hydroxide, sodium hydroxide, potassium hydroxide or ammonia water; the concentration of the acid or the alkali is 90-99%.
6. The method for preparing the metal ion battery anode material from the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (2), the mass ratio of the acid or alkali to the powder particles is 1-20: 100, respectively; the ultrasonic mixing time is 1-3 hours; the drying is carried out by adopting an air-blast drying oven, the temperature of the air-blast drying oven is 100-120 ℃, and the drying time is 12 hours.
7. The method for preparing the metal ion battery negative electrode material from the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (2), the inert atmosphere is nitrogen or argon, the heating equipment is a microwave oven, a muffle furnace or a tubular furnace, the heating rate is 5-10 ℃/min, the heating temperature is 1000-1500 ℃, and the heat preservation time is 0.5-2 h.
8. The method for preparing the metal ion battery anode material from the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (3), the acid solution is one of dilute hydrochloric acid, dilute sulfuric acid and dilute nitric acid; the alkaline solution is one of sodium hydroxide, potassium hydroxide and ammonia water solution; the concentration of the acidic solution or the alkaline solution is less than 0.8%; the cleaning solution is pure water, ultrapure water, deionized water or distilled water.
9. The method for preparing the metal ion battery anode material by using the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein in the step (3), the drying is performed by using a vacuum drying oven, the drying temperature is 100 ℃ and 120 ℃, and the drying time is 12 hours; grinding for 1-2h, and sieving to obtain granules with size of more than 200 meshes.
10. The method for preparing the metal ion battery anode material from the livestock and poultry manure organic fertilizer as claimed in claim 1, wherein the anode material is used for preparing a metal ion battery, and the metal ion battery is a lithium ion battery, a sodium ion battery or a potassium ion battery.
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