CN115779861A - Preparation method and application of carboxylic acid functionalized hydrothermal carbon adsorption material - Google Patents
Preparation method and application of carboxylic acid functionalized hydrothermal carbon adsorption material Download PDFInfo
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a preparation method and application of a carboxylic acid functionalized hydrothermal carbon adsorption material, wherein the preparation method comprises the following steps: (1) Adding bamboo powder and a dilute hydrochloric acid solution into a reaction kettle, carbonizing by adopting a hydrothermal carbonization method, cooling, performing suction filtration and washing after the reaction is finished, adding a sodium hydroxide solution, stirring, performing suction filtration, washing and drying after the reaction is finished, and obtaining hydrothermal bamboo charcoal; (2) And adding itaconic acid, ammonium persulfate and sodium hydroxide solid into the hydrothermal bamboo charcoal, grinding until the mixture is uniformly mixed, putting the mixture into a reaction kettle, introducing nitrogen, heating for reaction, cooling after the reaction is finished, performing suction filtration, washing and drying to obtain the adsorbent. The adsorbent prepared by the invention can effectively adsorb cationic pollutants, the adsorption capacity of the adsorbent on methylene blue can reach 1032.95mg/g at room temperature, the adsorption capacity on lead ions can reach 285.16mg/g, and the adsorbent has a good application prospect in the field of water pollution treatment.
Description
Technical Field
The invention belongs to the field of water pollution treatment, and particularly relates to a preparation method and application of a carboxylic acid functionalized hydrothermal carbon adsorption material.
Background
The main pollution sources of water body pollution are from industrial dyes, heavy metals, pharmaceutical wastewater and other organic pollutants, and even at the lowest concentration, the pollutants can cause biogenetic problems and physiological defects of organisms. Although a large number of adsorbents such as MOFs, hydrogel, mesoporous materials, activated carbon and the like are applied to wastewater treatment, the adsorbents still have the defects of low stability, high price, low adsorption capacity, poor regeneration capacity and the like. Therefore, it is important to develop and utilize convenient, economic and environment-friendly materials to remove the pollution sources in the water environmental system. The hydrothermal carbonization method is a green, environment-friendly and simple carbon material preparation method, agricultural and forestry wastes can be converted into carbon-rich materials under mild conditions, and the prepared hydrothermal carbon has small specific surface area and limited pollutant adsorption capacity due to lack of specific binding sites on the surface. The adsorption capacity of the hydrothermal carbon can be enhanced by increasing the content of high-activity groups such as carboxylate radicals on the surface of the hydrothermal carbon, but the currently used carboxylic anhydride modification method has the problems of higher price, limited number of grafted carboxylic acid functional groups and the like.
Bamboo is a good renewable resource, has short growth cycle, high yield and wide distribution range, and can effectively relieve the problems of wood resource reduction and the like. The bamboo charcoal is a product obtained by carbonizing bamboo, has a special microporous structure and a higher specific surface area, and has a good application prospect in an adsorbent. The free radical polymerization method is a common surface modification method, and can endow the material with new physical and chemical properties. Itaconic acid is a nontoxic monomer, can be prepared from renewable non-petroleum resources through microbial fermentation, contains a double bond and two carboxylic acid groups, and the double bond and the carboxylic acid generate a conjugated effect, has higher polymerization capacity, and is expected to improve the adsorption capacity of hydrothermal carbon through free radical copolymerization modified hydrothermal carbon. In addition, no organic solvent is used in the solid phase reaction process, so that the method is a green and environment-friendly synthesis method.
Disclosure of Invention
The invention aims to: the invention aims to provide a preparation method of a carboxylic acid functionalized hydrothermal carbon adsorption material, which adopts a free radical polymerization method to synthesize the hydrothermal carbon adsorption material in a solid phase manner, does not need to use an organic solvent in the solid phase reaction process, and is simple and environment-friendly; the invention also aims to provide the application of the carboxylic acid functionalized hydrothermal carbon adsorption material prepared by the method in the adsorption of methylene blue and heavy metal lead ions, and the adsorption material has a stable structure and can be recycled.
The technical scheme is as follows: the preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material comprises the following steps:
(1) Adding bamboo powder and a dilute hydrochloric acid solution into a hydrothermal reaction kettle, carbonizing by adopting a hydrothermal carbonization method, cooling after the reaction is finished, performing suction filtration, washing with a solvent, adding a sodium hydroxide solution, stirring, performing suction filtration after the reaction is finished, washing with the solvent until the filtrate is neutral, and drying to obtain the hydrothermal bamboo charcoal.
(2) Taking the hydrothermal bamboo charcoal, adding itaconic acid, ammonium persulfate and sodium hydroxide solid, grinding until the mixture is uniformly mixed, putting the mixture into a reaction kettle, introducing nitrogen, carrying out heating reaction, cooling after the reaction is finished, carrying out suction filtration, washing with a solvent until the filtrate is neutral, and drying to obtain a target compound, namely the carboxylic acid functionalized hydrothermal carbon.
Further, the concentration of the dilute hydrochloric acid solution in the step (1) is 0.5-1.0mol/L, and the adding proportion of the bamboo powder to the dilute hydrochloric acid solution is 40-50g:160-180mL, the adding proportion of the bamboo powder and the sodium hydroxide solution is 40-50g:400-500mL; the carbonization temperature is 200-220 ℃, and the reaction time is 12-24h; the concentration of the sodium hydroxide solution is 0.2-0.25mol/L, and the stirring time is 1-4h; the washing solvent is deionized water.
Further, the mass ratio of the hydrothermal carbon, the itaconic acid, the ammonium persulfate and the sodium hydroxide in the step (2) is 8-9g:16-18g:0.8-1.0g:8-9g; during grinding, hydrothermal bamboo charcoal, itaconic acid, ammonium persulfate and sodium hydroxide are added in sequence, nitrogen is introduced for 15-30min after the hydrothermal bamboo charcoal, the itaconic acid, the ammonium persulfate and the sodium hydroxide are poured into a reaction kettle, and the reaction condition is solid-phase heating reaction; the reaction temperature is 200-220 ℃, and the reaction time is 8-12h; the washing solvent is deionized water.
Further, the drying temperature of the step (1) and the drying temperature of the step (2) are both 60-80 ℃.
The carboxylic acid functionalized hydrothermal carbon adsorption material prepared by the preparation method can be applied to adsorption of methylene blue and heavy metal cations.
The invention principle is as follows: according to the invention, itaconic acid containing unsaturated double bonds is successfully grafted to the surface of the hydrothermal bamboo charcoal rich in hydroxyl groups through a free radical reaction, the itaconic acid can generate a conjugate effect, and the double bonds and carboxylic acid of the itaconic acid can generate a polymerization reaction to modify the hydrothermal bamboo charcoal, so that the content of carboxylate radicals on the surface of the hydrothermal charcoal is increased, and the adsorption capacity of the hydrothermal charcoal can be effectively improved. The carboxylic acid functionalized hydrothermal carbon can adsorb methylene blue and lead ions by utilizing the actions of ion exchange, pi-pi conjugation, electrostatic action, internal surface complexation, cation-pi, hydrogen bond and the like. The carboxylic acid functionalized hydrothermal carbon is in negative charge under the condition of lower pH value, so that the hydrothermal bamboo charcoal can adsorb cation pollutants through electrostatic interaction in a wider pH value range, and the adsorption capacity is higher.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: (1) The preparation method is simple, convenient and environment-friendly, the carboxylic acid functionalized hydrothermal carbon adsorption material is synthesized by adopting a free radical polymerization method in a solid phase, and an organic solvent is not required in the solid phase reaction process, so that the method is an environment-friendly synthesis method; (2) The adsorbent prepared by the preparation method can effectively adsorb cation pollutants, the adsorption capacity of the adsorbent to methylene blue can reach 1032.95mg/g at room temperature, the adsorption capacity to lead ions can reach 285.16mg/g, and the adsorbent material can be recycled and reused, so that the adsorbent has a good application prospect in the field of water pollution treatment.
Drawings
FIG. 1 is a) a force diagram of adsorption capacity of carboxylic acid functionalized hydrothermal carbon on methylene blue with different initial concentrations, and b) a force diagram of adsorption capacity of carboxylic acid functionalized hydrothermal carbon on lead ions with different initial concentrations;
FIG. 2 is a test chart of the recycling of methylene blue and lead ion adsorption by carboxylic acid functionalized hydrothermal carbon.
Detailed Description
Example 1
The preparation method of the carboxylic acid functionalized hydrothermal carbon comprises the following steps:
weighing 40g of waste bamboo powder, placing the waste bamboo powder into a 500mL high-pressure reaction kettle with a polytetrafluoroethylene lining, adding 160mL of hydrochloric acid solution with the concentration of 1mol/L, uniformly stirring, reacting for 24 hours at 200 ℃, cooling, performing suction filtration, cleaning with deionized water, adding 400mL of sodium hydroxide solution with the concentration of 0.25mol/L, stirring for 1 hour, performing suction filtration, cleaning with deionized water until the filtrate is neutral, performing suction filtration, and drying at 60 ℃ to obtain the hydrothermal bamboo charcoal.
Weighing 8g of hydrothermal bamboo charcoal, 16g of itaconic acid, 1g of ammonium persulfate and 8g of sodium hydroxide, placing the mixture into a mortar, grinding the mixture into uniform powder, pouring the powder into a 500mL high-pressure reaction kettle with a polytetrafluoroethylene lining, introducing nitrogen for 15min, heating the mixture at 200 ℃ for reaction for 8h, cooling the mixture to room temperature, washing the mixture with deionized water until the pH value of filtrate is neutral, and drying the mixture at 60 ℃ to obtain the carboxylic acid functionalized hydrothermal carbon.
Example 2
The preparation method of the carboxylic acid functionalized hydrothermal carbon comprises the following steps:
weighing 40g of waste bamboo powder, placing the waste bamboo powder into a 500mL high-pressure reaction kettle with a polytetrafluoroethylene lining, adding 180mL of hydrochloric acid solution with the concentration of 0.5mol/L, uniformly stirring, reacting at 220 ℃ for 12 hours, cooling, performing suction filtration, cleaning with deionized water, adding 400mL of sodium hydroxide solution with the concentration of 0.2mol/L, stirring for 4 hours, performing suction filtration, cleaning with deionized water until the filtrate is neutral, and performing suction filtration to obtain the hydrothermal bamboo charcoal.
Respectively weighing 9g of hydrothermal bamboo charcoal, 16g of itaconic acid, 0.8g of ammonium persulfate and 9g of sodium hydroxide, placing the mixture into a mortar, grinding the mixture into uniform powder, pouring the powder into a 500mL high-pressure reaction kettle with a polytetrafluoroethylene lining, introducing nitrogen for 15min, heating the mixture at 220 ℃ for reaction for 10h, cooling the mixture to room temperature, washing the mixture with deionized water until the pH value of the filtrate is neutral, and drying the mixture at 60 ℃ to obtain the carboxylic acid functionalized hydrothermal carbon.
Example 3
The preparation method of the carboxylic acid functionalized hydrothermal carbon comprises the following steps:
weighing 50g of waste bamboo powder into a 500mL high-pressure reaction kettle with a polytetrafluoroethylene lining, adding 180mL of hydrochloric acid solution with the concentration of 0.5mol/L, uniformly stirring, reacting at 220 ℃ for 24 hours, cooling, performing suction filtration, washing with deionized water, adding 500mL of sodium hydroxide solution with the concentration of 0.25mol/L, stirring for 2 hours, performing suction filtration, washing with deionized water until the filtrate is neutral, and performing suction filtration to obtain the hydrothermal bamboo charcoal.
Respectively weighing 9g of hydrothermal bamboo charcoal, 18g of itaconic acid, 0.9g of ammonium persulfate and 9g of sodium hydroxide, putting the materials into a mortar, grinding the materials into uniform powder, pouring the powder into a 500mL high-pressure reaction kettle with a polytetrafluoroethylene lining, introducing nitrogen for 30min, heating the powder at 220 ℃ for reaction for 12h, cooling the powder to room temperature, washing the powder with deionized water until the pH of the filtrate is neutral, and drying the powder at 80 ℃ to obtain the carboxylic acid functionalized hydrothermal carbon.
Initial concentration on adsorption effect:
the carboxylic acid-functionalized hydrothermal carbon prepared in example 1 was tested for adsorption effect according to various initial concentrations, as shown in fig. 1. According to FIG. 1a, under the condition of 298K, as the initial concentration of methylene blue is increased from 300mg/g to 1200mg/g, the adsorption amount of the adsorbent for the methylene blue is obviously increased from 373.75mg/g to 1032.95mg/g; when the initial concentration of Pb (II) increased from 50mg/g to 350mg/g, the adsorption amount of Pb (II) increased from 61.79mg/g to 285.16mg/g.
IFHC recycle:
the methylene blue solution with the concentration of 1100mg/L and 0.50g of the adsorbent prepared in the example 1 are mixed and shaken until the adsorption is saturated, a desorption experiment is carried out by taking a mixed solution of ethanol and 0.2mol/L hydrochloric acid solution (volume ratio is 1).
After mixing and adsorbing 250mg/L Pb (II) solution and 0.50g of adsorbent, carrying out desorption experiment by taking 0.1mol/L nitric acid as desorption solution, activating the regenerated adsorbent by 0.25mol/L sodium hydroxide solution, washing by deionized water, drying and testing the adsorption capacity of the adsorbent.
As can be seen from the recycling test chart in FIG. 2, the adsorption capacity of the adsorbent to methylene blue and lead ions is still kept above 90% after 5 cycles, which shows that the carboxylic acid functionalized hydrothermal carbon is an adsorption material with stable structure and recycling function, and has great prospect in water pollution treatment.
Claims (10)
1. A preparation method of a carboxylic acid functionalized hydrothermal carbon adsorption material is characterized by comprising the following steps:
adding bamboo powder and a dilute hydrochloric acid solution into a reaction kettle, carbonizing by adopting a hydrothermal carbonization method, cooling, performing suction filtration and washing after the reaction is finished, adding a sodium hydroxide solution, stirring, performing suction filtration, washing and drying after the reaction is finished, and obtaining hydrothermal bamboo charcoal;
and adding itaconic acid, ammonium persulfate and sodium hydroxide solid into the hydrothermal bamboo charcoal, grinding until the mixture is uniformly mixed, putting the mixture into a reaction kettle, introducing nitrogen, heating for reaction, cooling after the reaction is finished, performing suction filtration, washing and drying to obtain the carboxylic acid functionalized hydrothermal carbon adsorption material.
2. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the concentration of the dilute hydrochloric acid solution in the step (1) is 0.5-1.0 mol/L.
3. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the addition ratio of the bamboo powder and the dilute hydrochloric acid solution in the step (1) is 40-50g:160-180 mL; the adding proportion of the bamboo powder and the sodium hydroxide solution is 40-50g:400-500 mL.
4. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the concentration of the sodium hydroxide solution in the step (1) is 0.2-0.25mol/L, and the stirring time is 1-4h.
5. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the carbonization temperature in the step (1) is 200-220 ℃, and the carbonization time is 12-24 h.
6. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the washing solvent in steps (1) and (2) is deionized water.
7. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the mass ratio of the hydrothermal bamboo charcoal, the itaconic acid, the ammonium persulfate and the sodium hydroxide in the step (2) is 8-9g:16-18g:0.8-1.0g:8-9 g.
8. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the nitrogen gas is introduced in the step (2) for 15-30min.
9. The preparation method of the carboxylic acid functionalized hydrothermal carbon adsorption material according to claim 1, wherein the reaction temperature in the step (2) is 200-220 ℃, and the reaction time is 8-12 h.
10. The application of the carboxylic acid functionalized hydrothermal carbon adsorption material prepared by the preparation method of any one of claims 1-9 in adsorbing methylene blue and metal cations.
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| CN116492995A (en) * | 2023-03-29 | 2023-07-28 | 桂林理工大学 | Preparation method and application of 1,3, 5-benzene tricarboxylic acid modified UIO-66 (Zr) metal organic framework material |
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