CN112340728B - Chestnut shell-based biomass carbon material and preparation method and application thereof - Google Patents
Chestnut shell-based biomass carbon material and preparation method and application thereof Download PDFInfo
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- CN112340728B CN112340728B CN202011168996.9A CN202011168996A CN112340728B CN 112340728 B CN112340728 B CN 112340728B CN 202011168996 A CN202011168996 A CN 202011168996A CN 112340728 B CN112340728 B CN 112340728B
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- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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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
Abstract
The invention provides a chestnut shell-based biomass carbon material and a preparation method and application thereof, belonging to the technical field of carbon materials. Firstly, reacting chestnut shell powder with organic acid by a hydrothermal method to obtain a hydrothermal carbon material; then placing the hydrothermal carbon material in an alkaline solution, fully stirring, standing, filtering, and freeze-drying to obtain a dried carbon material; then reacting the carbon material in an inert atmosphere to obtain a pre-product; and finally, soaking the pre-product with strong inorganic acid, and washing the pre-product with water to be neutral to obtain the chestnut shell-based biomass carbon material. The chestnut shell-based biomass carbon material has good pore structure and capacitance performance, is applied to an electrode material of a capacitance deionization technology to remove toxic heavy metals, and can effectively improve the removal rate.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and particularly relates to a chestnut shell-based biomass carbon material and a preparation method and application thereof.
Background
In recent years, with the development of economic society, particularly the rapid development of mining industry, metallurgical industry, foundry industry and chemical industry, heavy metal wastewater is discharged in large quantity, and on one hand, the heavy metal wastewater enters a water environment to cause water resource pollution and ecological environment destruction; on the other hand, china is a country with relative shortage of fresh water resources, the per capita water resources are only 1/4 of the world level, and the waste water discharged in large amount is the waste of resources. The capacitive deionization technology has the advantages of low energy consumption, in-situ regeneration, no secondary pollution to the environment and the like, and has great application potential and wide application prospect in the field of water treatment.
The key point of the capacitive deionization technology for removing heavy metal pollutants is the electrode material. The development and research of high-performance electrode materials are core links for improving the separation efficiency and the practical degree of the capacitive deionization technology and reducing the process energy consumption. Carbon materials have attracted much attention from researchers because of their high stability, high specific surface area, and good electrical conductivity. Compared with the traditional method for preparing the carbon material, the method for preparing the carbon material by directly using the biomass as the precursor has the advantages of rich raw materials, environmental friendliness, low cost, sustainability and the like, and meets the current social requirements. Therefore, the preparation of carbon materials by using biomass is a trend in the development of the current society.
China is a big agricultural country, a large amount of biomass resources such as straws, shells and the like can be generated every year, but due to the limitation of storage and conversion technologies, a lot of biomass resources are wasted seriously, most biomass resources are directly incinerated and used by livestock or buried as garbage, and the treatment modes not only pollute the environment, but also cause the waste of resources. If the low-value biomass is converted into a useful carbon material by a carbonization technology for a capacitive deionization technology, the unity of social benefit, economic benefit and environmental benefit can be realized.
Disclosure of Invention
The invention aims to provide a chestnut shell-based biomass carbon material, and a preparation method and application thereof.
The invention firstly provides a preparation method of a chestnut shell based biomass carbon material, which comprises the following steps:
the method comprises the following steps: reacting chestnut shell powder with organic acid by adopting a hydrothermal method to obtain a hydrothermal carbon material;
step two: placing the hydrothermal carbon material obtained in the first step in an alkaline solution, fully stirring, standing, filtering, and freeze-drying to obtain a dried carbon material;
step three: reacting the carbon material obtained in the second step in an inert atmosphere to obtain a pre-product;
step four: and (4) soaking the pre-product obtained in the step three with inorganic strong acid, and washing with water to be neutral to obtain the chestnut shell-based biomass carbon material.
Further, the organic acid in the first step is one or more selected from citric acid, salicylic acid and tartaric acid, and the concentration is 0.1-0.3 mol/L.
Further, the reaction temperature of the first step is 180-200 ℃, and the time is 6-8 h.
Further, the weight g of the chestnut shell powder is as follows: the volume mL of organic acid is preferably (5-8): 70.
Further, in the second step, the alkali solution is one or more selected from sodium carbonate, sodium hydroxide, potassium carbonate and potassium hydroxide, and the concentration is 3-5 mol/L.
Further, the reaction of the third step is that the temperature is raised to 350 ℃ from room temperature, the temperature raising rate is 5 ℃/min, and the reaction is kept for 1h; then raising the temperature from 350 ℃ to 600-800 ℃, wherein the heating rate is 5 ℃/min, and finally, naturally cooling to the room temperature after keeping for 2 hours.
Further, the inorganic strong acid in the fourth step is selected from one of hydrochloric acid, sulfuric acid and nitric acid, and the concentration of the inorganic strong acid is 1 mol/L-3 mol/L.
The invention also provides the chestnut shell-based biomass carbon material prepared by the preparation method.
The invention also provides application of the chestnut shell-based biomass carbon material as an active material in a capacitive deionization module unit in water treatment.
The invention has the advantages of
The invention provides a chestnut shell-based biomass carbon material and a preparation method and application thereof, wherein the method comprises the steps of firstly reacting chestnut shell powder with organic acid by a hydrothermal method to obtain a hydrothermal carbon material; the method comprises the steps of adopting organic acid as a catalyst for reaction, aiming at promoting the hydrolysis of cellulose, then placing a hydrothermal carbon material in an alkali solution, reacting the carbon material in an inert atmosphere, activating the carbon material, enabling metal and metal salt generated by the reaction of the alkali and the carbon to permeate into a carbon matrix to increase the lattice spacing of the carbon, finally soaking the carbon matrix in inorganic strong acid, and washing the carbon matrix with water to be neutral to obtain the chestnut shell based biomass carbon material. Compared with the prior art, the chestnut shell-based biomass carbon material obtained by the invention has a three-dimensional honeycomb porous structure, and a good pore channel structure, so that the diffusion and transmission of ions on the surface of an electrode can be promoted, and the ion adsorption rate and the ion adsorption capacity of the electrode can be improved.
The chestnut shell-based biomass carbon material is used as an active material for removing toxic heavy metals from an electrode material of a capacitive deionization technology, can effectively improve the removal rate, and has a good application prospect. Meanwhile, the carbon material is prepared by directly using the chestnut shells as the precursor, so that the method has the advantages of wide and cheap raw material sources, environment-friendly preparation process and the like, not only can the requirements of low price and large-scale production be met, but also the problem of environmental pollution caused by burning a large amount of waste biomass is relieved.
Drawings
FIG. 1 is an SEM photograph of a chestnut shell-based biomass carbon material prepared in example 2 of the present invention.
FIG. 2 shows the chestnut shell-based biomass carbon material pair Cr prepared in example 3 of the present invention 6+ Graph of the removal rate change of (2).
Detailed Description
The invention firstly provides a preparation method of a chestnut shell based biomass carbon material, which comprises the following steps:
the method comprises the following steps: reacting the chestnut shell powder with organic acid by a hydrothermal method, and particularly preferably:
weighing chestnut shell powder, adding organic acid, placing the chestnut shell powder in a polytetrafluoroethylene lining, and reacting in an oven at the reaction temperature of preferably 180-200 ℃ for 6-8 hours to obtain a hydrothermal carbon material; the organic acid is preferably selected from one or more of citric acid, salicylic acid and tartaric acid, and the concentration is preferably 0.1-0.3 mol/L; the weight g of the chestnut shell powder is as follows: the volume mL of organic acid is preferably (5-8): 70; before the chestnut shell powder is used, preferably, the waste chestnut shells are washed by distilled water for 4 to 6 times, crushed and dried in a constant-temperature drying box.
Step two: placing the hydrothermal carbon material obtained in the first step into an alkaline solution, wherein the alkaline solution is preferably one or more selected from sodium carbonate, sodium hydroxide, potassium carbonate and potassium hydroxide, the concentration is preferably 3-5 mol/L, fully stirring, standing, filtering and freeze-drying, and the freeze-drying time is preferably 8-48 h to obtain a dried carbon material;
step three: reacting the carbon material obtained in the second step in an inert atmosphere, preferably raising the temperature from room temperature to 350 ℃, wherein the temperature raising rate is 5 ℃/min, and keeping for 1h; then raising the temperature from 350 ℃ to 600-800 ℃, wherein the raising rate is 5 ℃/min, and finally, naturally lowering the temperature to room temperature after keeping for 2 hours to obtain a pre-product;
step four: and (4) soaking the pre-product obtained in the third step by using inorganic strong acid, and washing the pre-product by using water until the pre-product is neutral to obtain the chestnut shell based biomass carbon material, wherein the inorganic strong acid is preferably selected from one of hydrochloric acid, sulfuric acid and nitric acid, and the concentration of the inorganic strong acid is preferably 1-3 mol/L.
The invention also provides the chestnut shell-based biomass carbon material prepared by the preparation method.
The invention also provides application of the chestnut shell-based biomass carbon material as an active material in a capacitive deionization module unit in water treatment.
According to the invention, the chestnut shell-based biomass carbon material is used as an active material for assembling a capacitive deionization module unit. The method specifically comprises the following steps: the deionization module comprises 1 or more symmetrical electrode pairs consisting of chestnut shell-based biomass carbon materials, two electrodes of the same electrode pair are separated by a plastic net to form a fluid channel, and the outermost electrode is in contact with a current collector and is connected with a direct current power supply.
The capacitive deionization module is applied to the fields of water treatment and resource recycling and is used for removing heavy metals in water. The heavy metal is preferably Pb 2+ 、Cr 6+ 、Cd 2+ 。
The technical solutions of the present invention are further described below with reference to specific examples, but these are specific methods and descriptions used in the examples and do not limit the scope of the present invention.
Example 1
1) Washing the waste chestnut shells with distilled water for 4-6 times, crushing, drying in a constant-temperature drying oven at 100 ℃, and storing for later use.
2) Weighing 6g of chestnut shell powder, adding 70mL of 0.1mol/L salicylic acid solution, placing the chestnut shell powder in a polytetrafluoroethylene lining, and reacting in an oven at 180 ℃ for 6 hours to obtain a hydrothermal carbon material;
3) Putting the material obtained in the step 2) into a 3mol/L sodium carbonate solution, fully stirring, standing, filtering, and freeze-drying for 36 hours to obtain a dried carbon material;
4) Heating the freeze-dried sample to 350 ℃ in an inert atmosphere at a heating rate of 5 ℃/min, calcining for 1h, heating to 800 ℃ at a heating rate of 5 ℃/min, and carrying out constant heat treatment for 2h to obtain a pre-product.
5) Using 1mol/L HNO to the pre-product 3 Soaking, and washing with water to neutrality to obtain the chestnut shell-based biomass carbon material.
The obtained chestnut shell-based biomass carbon material is used as an active material, acetylene black and PTFE are mixed with the raw materials according to the mass ratio of 8. At a temperature of 25 ℃, cr 6+ The heavy metal removal experiment was carried out at an initial concentration of 30mg/L and a voltage of 1.0V. The experimental results show that: the chestnut shell-based biomass carbon material can effectively remove heavy metal Cr 6+ The removal rate can reach 88.5 percent.
Example 2
1) Washing the waste chestnut shells with distilled water for 4-6 times, crushing, drying in a constant-temperature drying oven at 100 ℃, and storing for later use.
2) Weighing 7.5g of chestnut shell powder, adding 70mL of 0.1mol/L citric acid solution, placing the chestnut shell powder in a polytetrafluoroethylene lining, and reacting in an oven at 200 ℃ for 6 hours to obtain a hydrothermal carbon material;
3) Putting the material obtained in the step 2) into a 4mol/L potassium hydroxide solution, fully stirring, standing, filtering, and freeze-drying for 48 hours to obtain a dried carbon material;
4) Heating the freeze-dried sample to 350 ℃ in an inert atmosphere at the heating rate of 5 ℃/min, calcining for 1h, heating to 700 ℃ at the heating rate of 5 ℃/min, and carrying out constant heat treatment for 2h to obtain a pre-product.
5) And soaking the pre-product by using 1mol/L HCl, and washing the pre-product by using water until the pre-product is neutral to obtain the chestnut shell based biomass carbon material.
The SEM image of the obtained chestnut shell-based biomass carbon material is shown in fig. 1, which illustrates that the chestnut shell-based biomass carbon material prepared by the method of the present invention has a three-dimensional honeycomb porous structure.
The obtained chestnut shell-based biomass carbon material is used as an active material, acetylene black and PTFE are mixed with the raw materials according to the mass ratio of 8. At a temperature of 25 ℃, pb 2+ The heavy metal removal experiment was carried out at an initial concentration of 20mg/L and a voltage of 1.0V. The experimental results show that: the chestnut shell-based biomass carbon material can effectively remove heavy metal Pb 2+ The removal rate can reach 95.8%.
Example 3
1) Washing the waste chestnut shells with distilled water for 4-6 times, crushing, drying in a constant-temperature drying oven at 100 ℃, and storing for later use.
2) Weighing 7g of chestnut shell powder, adding 70mL of 0.1mol/L citric acid solution, placing the chestnut shell powder in a polytetrafluoroethylene lining, and reacting in an oven at 200 ℃ for 8 hours to obtain a hydrothermal carbon material;
3) Placing the material obtained in the step 2) in a 4mol/L sodium hydroxide solution, fully stirring, standing, filtering, and freeze-drying for 36 hours to obtain a dried carbon material;
4) Heating the freeze-dried sample to 350 ℃ in an inert atmosphere at the heating rate of 5 ℃/min, calcining for 1h, heating to 700 ℃ at the heating rate of 5 ℃/min, and carrying out constant heat treatment for 2h to obtain a pre-product.
5) And soaking the pre-product by using 1mol/L HCl, and washing the pre-product by using water until the pre-product is neutral to obtain the chestnut shell based biomass carbon material.
The obtained chestnut shell-based biomass carbon material is used as an active material, acetylene black and PTFE are mixed with the raw materials according to the mass ratio of 8. At a temperature of 25 ℃, cr 6+ The heavy metal removal experiment was carried out at an initial concentration of 30mg/L and a voltage of 1.0V.
Example 3 chestnut shell-based Biomass carbon Material pair Cr prepared 6+ The removal rate change curve of (2) is shown in fig. 2. FIG. 2 illustrates the combination of chestnut shell-based biomass carbon material with Cr 6+ The removal rate of (a) is 90.1%,can effectively remove heavy metal Cr 6+ And has good application prospect.
Claims (6)
1. The application of the chestnut shell-based biomass carbon material as an active material in the aspect of water treatment of capacitive deionization module units is characterized in that the preparation method of the chestnut shell-based biomass carbon material comprises the following steps:
the method comprises the following steps: reacting chestnut shell powder with organic acid by a hydrothermal method to obtain a hydrothermal carbon material;
step two: placing the hydrothermal carbon material obtained in the first step in an alkaline solution, fully stirring, standing, filtering, and freeze-drying to obtain a dried carbon material;
step three: reacting the carbon material obtained in the second step in an inert atmosphere to obtain a pre-product;
step four: soaking the pre-product obtained in the third step in strong inorganic acid, and washing the soaked pre-product with water to be neutral to obtain a chestnut shell-based biomass carbon material;
the reaction in the third step is that the temperature is increased from room temperature to 350 ℃, the temperature increasing rate is 5 ℃/min, and the reaction is kept for 1h; then raising the temperature from 350 ℃ to 600-800 ℃, wherein the heating rate is 5 ℃/min, and finally, naturally cooling to the room temperature after keeping for 2 hours.
2. The use of claim 1, wherein the organic acid is one or more selected from citric acid, salicylic acid, and tartaric acid, and the concentration is 0.1mol/L to 0.3mol/L.
3. The use of claim 1, wherein the reaction temperature of step one is 180-200 ℃ and the reaction time is 6-8 h.
4. Use according to claim 1, wherein the chestnut shell powder has a mass g: the volume mL of the organic acid is preferably (5-8): 70.
5. The use of claim 1, wherein the alkali solution in the second step is one or more selected from sodium carbonate, sodium hydroxide, potassium carbonate and potassium hydroxide, and the concentration is 3mol/L to 5mol/L.
6. The use according to claim 1, wherein the strong inorganic acid in step four is selected from one of hydrochloric acid, sulfuric acid and nitric acid, and the concentration of the strong inorganic acid is 1mol/L to 3mol/L.
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