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CN-122006665-A - Porous carbon material for adsorbing heavy metals and preparation method and application thereof

CN122006665ACN 122006665 ACN122006665 ACN 122006665ACN-122006665-A

Abstract

The invention provides a porous carbon material for adsorbing heavy metals, and a preparation method and application thereof, and relates to the technical field of adsorbent preparation. The preparation method of the porous carbon material comprises the steps of S1, adding dopamine hydrochloride and N-methylolacrylamide into absolute ethyl alcohol, uniformly stirring, adding concentrated sulfuric acid for reaction, carrying out suction filtration, washing to neutrality to obtain DTA, S2, adding acrylamide, acrylonitrile, acrylic acid and 3- (acrylamide methyl) -5-benzoyl-4-hydroxy-2-methoxybenzene sulfonic acid into water to obtain a solution system, sequentially adding sodium hydroxide, carrying out ultrasonic treatment on an intermediate product DTA and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone, placing under a mercury lamp light source for irradiation, washing, freeze-drying to obtain PAAAS-D, and S3, carrying out carbonization under an inert atmosphere after heating pre-oxidation treatment on PAAAS-D to obtain CPAAAS-D. The porous carbon material has rich active sites and an optimized pore canal structure, and can efficiently adsorb Fe, co and Ni heavy metal ions.

Inventors

  • YU LIANGMIN
  • YANG JIAN
  • YAN XUEFENG
  • MO WEIJUN
  • WANG JIANPENG

Assignees

  • 中国海洋大学三亚海洋研究院

Dates

Publication Date
20260512
Application Date
20260414

Claims (10)

  1. 1. The preparation method of the porous carbon material for adsorbing heavy metals is characterized by comprising the following specific preparation steps of: S1, adding dopamine hydrochloride and N-methylol acrylamide into absolute ethyl alcohol, uniformly stirring, adding concentrated sulfuric acid for reaction, carrying out suction filtration, and washing to neutrality to obtain an intermediate product DTA; The structural formula of the DTA is as follows: ; S2, adding acrylamide, acrylonitrile, acrylic acid and 3- (acrylamide methyl) -5-benzoyl-4-hydroxy-2-methoxyl benzenesulfonic acid into water to obtain a solution system, sequentially adding sodium hydroxide, an intermediate product DTA and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone, carrying out ultrasonic treatment, irradiating under a mercury lamp light source, washing, and freeze-drying to obtain PAAAS-D; the structural formula of PAAAS-D is as follows: ; Wherein w, x, y, z are the moles of acrylamide, acrylonitrile, acrylic acid, and 3- (acrylamidomethyl) -5-benzoyl-4-hydroxy-2-methoxybenzenesulfonic acid, respectively; and S3, heating and pre-oxidizing PAAAS-D, and carbonizing in an inert atmosphere to obtain the target porous carbon material.
  2. 2. The method for preparing a porous carbon material for adsorbing heavy metals according to claim 1, wherein in step S1, the molar ratio of dopamine hydrochloride to N-methylolacrylamide is 1-1.5:4-6; The concentration of the dopamine hydrochloride in the absolute ethyl alcohol is 0.125-0.3g/mL.
  3. 3. The method for preparing a porous carbon material for adsorbing heavy metals as set forth in claim 1, wherein in step S1, the addition amount of the concentrated sulfuric acid is 8% -10% of the volume of the absolute ethanol; The reaction temperature is 35-40 ℃ and the reaction time is 2-3 days.
  4. 4. The method for preparing a porous carbon material for adsorbing heavy metals as set forth in claim 1, wherein in step S2, the molar ratio of acrylamide, acrylonitrile, acrylic acid and 3- (acrylamidomethyl) -5-benzoyl-4-hydroxy-2-methoxybenzenesulfonic acid is 10:3-5:3-5:0.3-0.7; The solid content in the solution system is 15% -25%.
  5. 5. The method for preparing a porous carbon material for adsorbing heavy metals according to claim 1, wherein in step S2, the mass ratio of sodium hydroxide, intermediate DTA and 2-hydroxy-4- (2-hydroxyethoxy) -2-methylpropionacetone is 3.5:0.6-1:1.5-2.5.
  6. 6. The method for producing a porous carbon material for adsorbing heavy metals as set forth in claim 1, wherein in step S3, the temperature-rising pre-oxidation treatment is carried out at a temperature-rising rate of 1 to 3 ℃ per minute up to 200 ℃ for 2 to 3 hours.
  7. 7. The method for preparing a porous carbon material for adsorbing heavy metals as set forth in claim 1, wherein in step S3, the carbonization is performed under an inert atmosphere by raising the temperature to 600-900 ℃ at a temperature raising rate of 1-3 ℃ per minute under a nitrogen atmosphere, and maintaining for 2-3 hours.
  8. 8. A porous carbon material for adsorbing heavy metals, characterized by being produced by the production method according to any one of claims 1 to 7.
  9. 9. The use of a porous carbon material for the adsorption of heavy metals as claimed in claim 8 for the adsorption of heavy metal ions.
  10. 10. The use according to claim 9, wherein the heavy metal ions are at least one of Fe ions, co ions and Ni ions.

Description

Porous carbon material for adsorbing heavy metals and preparation method and application thereof Technical Field The invention relates to the technical field of adsorbent preparation, in particular to a porous carbon material for adsorbing heavy metals, and a preparation method and application thereof. Background The rapidly growing metal industry has contributed greatly to the development of society, but at the same time constitutes a serious pollution threat, and Fe/Co/Ni ions as typical transition metal ions are widely used in electroplating, mining, battery manufacturing and electronic waste recovery, resulting in their large discharge into wastewater. Fe 3+,Co2+ and Ni 2+ pollution can induce the generation of high-activity hydroxyl free radicals mainly through Fenton reaction, so that oxidative damage, DNA breakage and protein denaturation of organism cells are caused, and serious threat is caused to the ecological system and human health. At present, the traditional Fe/Co/Ni ion pollution removal technology has obvious limitations, such as chemical precipitation method realizes high removal rate through pH-induced hydroxide or sulfide formation, but simultaneously generates a large amount of low-density sludge which is difficult to dispose. Membrane separation methods such as nanofiltration and reverse osmosis achieve excellent rejection rates through size exclusion and charge rejection, but still face membrane fouling and high energy consumption challenges. The adsorption method has the advantages of simple operation, small secondary pollution and strong selectivity, and becomes a potential method. The carbon-based adsorption material has the advantages of good chemical stability, wide application range, easy recycling and environmental friendliness, and is widely applied to the field of water pollution treatment. However, the development of carbon-based materials with high-efficiency adsorption performance and good cycle stability still faces challenges, on one hand, the introduction of functional groups into the carbon-based adsorbent through post-modification is easy to cause uneven structure and limit the adsorption capacity of the carbon-based adsorbent, and on the other hand, the material often has the problem of reduced regeneration efficiency in the cycle use process, which affects the economical efficiency and the sustainability in practical application. Disclosure of Invention In view of the above, the invention provides a porous carbon material for adsorbing heavy metals, and a preparation method and application thereof. The technical scheme of the invention is realized as follows: The preparation method of the porous carbon material for adsorbing heavy metals comprises the following specific preparation steps: S1, adding dopamine hydrochloride and N-methylol acrylamide into absolute ethyl alcohol, uniformly stirring, adding concentrated sulfuric acid for reaction, carrying out suction filtration, and washing to neutrality to obtain an intermediate product DTA; the structural formula of DTA is: ; S2, adding acrylamide, acrylonitrile, acrylic acid and 3- (acrylamide methyl) -5-benzoyl-4-hydroxy-2-methoxyl benzenesulfonic acid into water to obtain a solution system, sequentially adding sodium hydroxide, an intermediate product DTA and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone, carrying out ultrasonic treatment, irradiating under a mercury lamp light source, washing, and freeze-drying to obtain PAAAS-D; PAAAS-D has the structural formula: ; Wherein w, x, y, z are the moles of acrylamide, acrylonitrile, acrylic acid, and 3- (acrylamidomethyl) -5-benzoyl-4-hydroxy-2-methoxybenzenesulfonic acid, respectively; S3, carbonizing PAAAS-D under inert atmosphere after heating and pre-oxidizing treatment to obtain the porous carbon material, which is named CPAAAS-D. Further, in the step S1, the mol ratio of the dopamine hydrochloride to the N-methylol acrylamide is 1-1.5:4-6; The concentration of the dopamine hydrochloride in the absolute ethyl alcohol is 0.125-0.3g/mL. Further, in the step S1, the adding amount of the concentrated sulfuric acid is 8% -10% of the volume of the absolute ethyl alcohol; The reaction temperature is 35-40 ℃ and the reaction time is 2-3 days. Further, in the step S2, the molar ratio of the acrylamide, the acrylonitrile, the acrylic acid and the 3- (acrylamide methyl) -5-benzoyl-4-hydroxy-2-methoxybenzene sulfonic acid is 10:3-5:3-5:0.3-0.7; The solid content in the solution system is 15% -25%. Further, in the step S2, the mass ratio of the sodium hydroxide, the intermediate product DTA and the 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone is 3.5:0.6-1:1.5-2.5. Further, in the step S3, the temperature rising pre-oxidation treatment is to raise the temperature to 200 ℃ at a temperature rising rate of 1-3 ℃ per minute for 2-3 hours. Further, in the step S3, the carbonization is carried out under the inert atmosphere, namely, the carbonization is carried ou