CN112774646A - Preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye - Google Patents

Preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye Download PDF

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CN112774646A
CN112774646A CN202110027963.0A CN202110027963A CN112774646A CN 112774646 A CN112774646 A CN 112774646A CN 202110027963 A CN202110027963 A CN 202110027963A CN 112774646 A CN112774646 A CN 112774646A
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activated carbon
methyl orange
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陈章平
杨玲
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/262Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

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Abstract

The invention discloses a preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye, which comprises the steps of adding activated carbon into an acid solution, soaking the activated carbon in the acid solution for 2-4 hours, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in an alkaline solution for 4-6 hours, filtering, washing the activated carbon with distilled water to be neutral, drying the activated carbon at 102-108 ℃ for 6-10 hours, adding copper salt and iron salt into the distilled water, adding the treated activated carbon into the solution, shaking, stirring, filtering, drying the activated carbon at 70-80 ℃, putting the dried activated carbon into a tubular furnace, calcining the calcined activated carbon at 320-380 ℃ for 3-6 hours, adding the activated carbon into the distilled water, adding dopamine, stirring for 30-60 min, adding tris-HCl buffer solution, adjusting the pH value to 10.8-11.6, shaking and stirring at room temperature for 10-15 hours, and then continuously soaking the activated carbon in the metal salt filtrate, stirring for 8-12 h, filtering, and drying to obtain the activated carbon adsorbent. The activated carbon adsorbent disclosed by the invention has excellent regeneration adsorption performance on methyl orange.

Description

Preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye
Technical Field
The invention belongs to the technical field of organic dye activated carbon adsorbents, and particularly relates to a preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye.
Background
At present, the development of times is rapid, and the treatment of wastewater is more and more emphasized while various industries pursue economic benefits. A large amount of organic pollutants discharged by enterprises such as textile, medicine, paper making and the like have great influence on the water quality of China, thereby threatening the life of human bodies. Among the sewage treatment methods, the adsorption method is a relatively effective and convenient treatment means. The traditional adsorbent mostly adopts an activated carbon material for water adsorption, and the activated carbon has a porous structure and a high specific surface area, is an excellent adsorption material and is widely applied.
However, the following problems also exist in the treatment of dye wastewater by using activated carbon: the cost of raw materials and energy consumption is large in the manufacturing process of the activated carbon, and the treatment mode of the activated carbon after saturated adsorption is generally incineration, landfill, waste and the like. If the activated carbon is a disposable consumer product, the economic cost is huge, and the activated carbon with saturated adsorption causes secondary pollution to the environment.
Disclosure of Invention
Aiming at the defect that the activated carbon adsorbent in the prior art can only treat organic dye methyl orange once and cannot be used as an adsorbent to carry out secondary adsorption treatment on the organic dye methyl orange, the invention aims to provide a preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye, which comprises the following steps:
s1: adding activated carbon into an acidic solution, soaking the activated carbon in the acidic solution for 2-4 hours, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in an alkaline solution for 4-6 hours, filtering, washing the activated carbon with distilled water to be neutral, and drying the activated carbon at 102-108 ℃ for 6-10 hours for later use.
S2: and adding a copper salt and an iron salt into distilled water, performing ultrasonic treatment to fully dissolve the copper salt and the iron salt, adding the activated carbon treated in the step S1 into the solution, vibrating and stirring for 6-12 h, filtering, drying at 70-80 ℃, putting into a tubular furnace, and calcining at 320-380 ℃ for 3-6 h for later use.
S3: adding the activated carbon obtained in the step S2 into distilled water, then adding dopamine, stirring for 30-60 min, then adding tris-HCl buffer solution, adjusting the pH value to 9.2-11.6, shaking and stirring at room temperature for 10-15 h, then continuously soaking in the filtrate obtained in the step S2, stirring for 8-12 h, filtering, and drying to obtain the activated carbon adsorbent.
Preferably, the acidic solution is any one of dilute sulfuric acid, dilute hydrochloric acid or dilute nitric acid with a mass fraction of 6-12%.
Preferably, the alkaline solution is a sodium hydroxide solution or a potassium hydroxide solution with a mass fraction of 8-15%.
Preferably, the copper salt is any one of copper sulfate, copper chloride and copper nitrate.
Preferably, the iron salt is any one of ferric sulfate, ferric chloride and ferric nitrate.
More preferably, the mass ratio of the copper salt to the iron salt is 0.6 to 0.9:0.5 to 1.
Preferably, the addition amount of the tris-HCl buffer solution is 8-15% of that of dopamine.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, firstly, an acidic solution is used for removing impurities in the activated carbon, then the activated carbon is soaked in an alkaline solution, so that the surface of the activated carbon is loose, the pore structure of the activated carbon is improved, more metal ions can be loaded when metal ions are further used for modification, the activated carbon is modified by the metal ions, then polydopamine is formed by dopamine under an acidic condition, the polydopamine has a plurality of active double bonds and catechol structures and can generate strong coordination with metal copper ions and iron ions, meanwhile, a polydopamine protective film is formed on the surface of the activated carbon, then, the polydopamine protective film is modified by the metal ion solution, the polydopamine protective film can protect the metal ions from falling off in the regeneration process of adsorbing methyl orange, and the diazo compounds such as polydopamine and methyl orange have certain affinity, so that the adsorption capacity is improved, meanwhile, the activated carbon has higher regeneration adsorption rate.
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye specifically comprises the following steps:
s1: adding activated carbon into dilute sulfuric acid with the mass fraction of 6%, soaking in the acid solution for 2 hours, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in sodium hydroxide solution with the mass fraction of 8% for 4 hours, filtering, washing with distilled water to be neutral, and drying at 102 ℃ for 6 hours for later use.
S2: adding copper sulfate and ferric sulfate into distilled water, performing ultrasonic treatment to fully dissolve the copper sulfate and ferric sulfate, adding the activated carbon treated in the step S1 into the solution, stirring for 6 hours under shaking, filtering, drying at 70-80 ℃, putting into a tubular furnace, and calcining for 3 hours at 320 ℃ for later use, wherein the mass ratio of the copper sulfate to the ferric sulfate is 0.6: 0.5.
S3: adding the activated carbon obtained in the step S2 into distilled water, then adding dopamine, stirring for 30min, then adding tris-HCl buffer solution, wherein the addition amount of the tris-HCl buffer solution is 8% of that of the dopamine, adjusting the pH value to 9.2, shaking and stirring for 10h at room temperature, then continuously soaking in the filtrate obtained in the step S2, stirring for 8h, filtering, and drying to obtain the activated carbon adsorbent.
Example 2
A preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye specifically comprises the following steps:
s1: adding activated carbon into dilute hydrochloric acid with the mass fraction of 12%, soaking in the acidic solution for 4h, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in a potassium hydroxide solution with the mass fraction of 15% for 6h, filtering, washing with distilled water to be neutral, and drying at 108 ℃ for 10h for later use.
S2: adding copper chloride and ferric chloride into distilled water, performing ultrasonic treatment to fully dissolve the copper chloride and ferric chloride, then adding the activated carbon treated in the step S1 into the solution, stirring for 12 hours by shaking, filtering, drying, then drying at 80 ℃, putting into a tubular furnace, and calcining for 3-6 hours at 380 ℃ for later use, wherein the mass ratio of the copper chloride to the ferric chloride is 0.9: 1.
S3: adding the activated carbon obtained in the step S2 into distilled water, then adding dopamine, stirring for 60min, then adding tris-HCl buffer solution, wherein the addition amount of the tris-HCl buffer solution is 15% of that of the dopamine, adjusting the pH value to 11.6, shaking and stirring for 15h at room temperature, then continuously soaking in the filtrate obtained in the step S2, stirring for 12h, filtering, and drying to obtain the activated carbon adsorbent.
Example 3
A preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye specifically comprises the following steps:
s1: adding activated carbon into dilute nitric acid with the mass fraction of 8%, soaking in the acidic solution for 3h, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in a sodium hydroxide solution with the mass fraction of 10% for 5h, filtering, washing with distilled water to be neutral, and drying at 104 ℃ for 8h for later use.
S2: adding copper nitrate and ferric nitrate into distilled water, performing ultrasonic treatment to fully dissolve the copper nitrate and ferric nitrate, adding the activated carbon treated in the step S1 into the solution, stirring for 8 hours with shaking, filtering, drying at 75 ℃, putting into a tubular furnace, and calcining for 4 hours at 340 ℃ for later use, wherein the mass ratio of the copper nitrate to the ferric nitrate is 0.7: 0.8.
S3: adding the activated carbon obtained in the step S2 into distilled water, then adding dopamine, stirring for 40min, then adding tris-HCl buffer solution, wherein the addition amount of the tris-HCl buffer solution is 10% of that of the dopamine, adjusting the pH value to 9.8, shaking and stirring for 12h at room temperature, then continuously soaking in the filtrate obtained in the step S2, stirring for 10h, filtering, and drying to obtain the activated carbon adsorbent.
Example 4
A preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye specifically comprises the following steps:
s1: adding activated carbon into dilute sulfuric acid with the mass fraction of 10%, soaking in the acid solution for 4 hours, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in a potassium hydroxide solution with the mass fraction of 13% for 6 hours, filtering, washing with distilled water to be neutral, and drying at 106 ℃ for 9 hours for later use.
S2: adding copper sulfate and ferric nitrate into distilled water, performing ultrasonic treatment to fully dissolve the copper sulfate and ferric nitrate, adding the activated carbon treated in the step S1 into the solution, stirring for 10 hours by shaking, filtering, drying at 80 ℃, putting into a tubular furnace, and calcining for 5 hours at 360 ℃ for later use, wherein the mass ratio of copper salt to ferric salt is 0.8: 0.9.
S3: adding the activated carbon obtained in the step S2 into distilled water, then adding dopamine, stirring for 50min, then adding tris-HCl buffer solution, wherein the addition amount of the tris-HCl buffer solution is 13% of that of the dopamine, adjusting the pH value to 10.4, shaking and stirring for 13h at room temperature, then continuously soaking in the filtrate obtained in the step S2, stirring for 11h, filtering, and drying to obtain the activated carbon adsorbent.
Comparative example 1
A preparation method of activated carbon for adsorbing methyl orange dye specifically comprises the following steps:
s1: adding activated carbon into dilute sulfuric acid with the mass fraction of 6%, soaking in the acid solution for 2 hours, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in sodium hydroxide solution with the mass fraction of 8% for 4 hours, filtering, washing with distilled water to be neutral, and drying at 102 ℃ for 6 hours for later use.
S2: adding copper sulfate and ferric sulfate into distilled water, performing ultrasonic treatment to fully dissolve the copper sulfate and ferric sulfate, adding the activated carbon treated in the step S1 into the solution, stirring for 6 hours under shaking, filtering, drying at 70-80 ℃, putting into a tubular furnace, and calcining for 3 hours at 320 ℃ for later use, wherein the mass ratio of the copper sulfate to the ferric sulfate is 0.6: 0.5.
Experimental example:
and (3) performance testing: 10g of the activated carbon prepared in examples 1 to 4, which was washed and dried, was put into 1L of a methyl orange solution having a mass concentration of 800mg/L, and the mixture was adsorbed by shaking in a water bath at a constant temperature (30 ℃ C., 120r/min)16h, measuring the adsorption capacity P1Washing and adsorbing saturated modified activated carbon by deionized water, putting the washed and adsorbed modified activated carbon into an oven at the temperature of 105 ℃, drying for 8h, washing and drying by deionized water after regeneration by using a regeneration method in the prior art, then putting 0.5g of saturated modified activated carbon into a 250mL conical flask with a plug, adding 100mL of methyl orange solution with the mass concentration of 800mg/L, carrying out water bath oscillation adsorption for 16h under the condition of constant temperature (30 ℃, 120r/min), and measuring the regeneration adsorption capacity P2The regeneration rate of the activated carbon is calculated by adopting the following formula:
Figure BDA0002891017400000051
wherein, the test results are shown in the following table 1,
table 1. test results:
Figure BDA0002891017400000052
as can be seen from Table 1, the activated carbon adsorbents prepared in the embodiments 1-4 of the invention have the raw carbon adsorption capacity of about 118mg/g and the regeneration adsorption capacity of about 108mg/g, and have higher raw carbon adsorption capacity and regeneration adsorption capacity compared with the activated carbon in the comparative example 1; the regeneration rate of the activated carbon adsorbent prepared in the embodiments 1 to 4 of the invention is more than 91.4%, which is much higher than 64.4% in the comparative example 1, and the activated carbon capable of adsorbing methyl orange in the invention has excellent regeneration adsorption performance.

Claims (7)

1. The preparation method of the activated carbon capable of regenerating and adsorbing the methyl orange dye is characterized by comprising the following steps of:
s1: adding activated carbon into an acidic solution, soaking the activated carbon in the acidic solution for 2-4 hours, filtering, washing the activated carbon with distilled water to be neutral, soaking the activated carbon in an alkaline solution for 4-6 hours, filtering, washing the activated carbon with distilled water to be neutral, and drying the activated carbon at 102-108 ℃ for 6-10 hours for later use;
s2: adding a copper salt and an iron salt into distilled water, performing ultrasonic treatment to fully dissolve the copper salt and the iron salt, then adding the activated carbon treated in the step S1 into the solution, vibrating and stirring for 6-12 h, filtering, drying, then drying at 70-80 ℃, putting into a tubular furnace, and calcining at 320-380 ℃ for 3-6 h for later use;
s3: adding the activated carbon obtained in the step S2 into distilled water, then adding dopamine, stirring for 30-60 min, then adding tris-HCl buffer solution, adjusting the pH value to 9.2-11.6, shaking and stirring at room temperature for 10-15 h, then continuously soaking in the filtrate obtained in the step S2, stirring for 8-12 h, filtering, and drying to obtain the activated carbon adsorbent.
2. The method for preparing activated carbon capable of regenerating and adsorbing methyl orange dye according to claim 1, wherein the acid solution is any one of dilute sulfuric acid, dilute hydrochloric acid or dilute nitric acid with a mass fraction of 6-12%.
3. The preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye according to claim 1, wherein the alkaline solution is 8-15% by weight of sodium hydroxide solution or potassium hydroxide solution.
4. The method for preparing activated carbon capable of regenerating and adsorbing methyl orange dye according to claim 1, wherein the copper salt is any one of copper sulfate, copper chloride and copper nitrate.
5. The method for preparing activated carbon capable of regenerating and adsorbing methyl orange dye according to claim 1, wherein the iron salt is any one of ferric sulfate, ferric chloride and ferric nitrate.
6. The preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye according to claim 1, wherein the mass ratio of the copper salt to the iron salt is 0.6-0.9: 0.5-1.
7. The method for preparing activated carbon capable of regenerating and adsorbing methyl orange dye according to claim 1, wherein the amount of tris-HCl buffer added is 8-15% of dopamine.
CN202110027963.0A 2021-01-11 2021-01-11 Preparation method of activated carbon capable of regenerating and adsorbing methyl orange dye Withdrawn CN112774646A (en)

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CN113751495A (en) * 2021-09-06 2021-12-07 安徽大学 Soil remediation agent for chlorophenol pollution
CN113908811A (en) * 2021-10-29 2022-01-11 兰溪市欧翔新材料有限公司 Preparation method of biomass charcoal material for removing phosphorus from sewage
CN114700103A (en) * 2022-04-12 2022-07-05 广州大学 Immobilized preparation method of metal-free carbon-based catalyst, product and application thereof
CN116535027A (en) * 2023-04-10 2023-08-04 广东绿韶环保工程有限公司 Sustainable reclaimed water recycling system treatment method

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN113751495A (en) * 2021-09-06 2021-12-07 安徽大学 Soil remediation agent for chlorophenol pollution
CN113751495B (en) * 2021-09-06 2022-04-22 安徽大学 Soil remediation agent for chlorophenol pollution
CN113908811A (en) * 2021-10-29 2022-01-11 兰溪市欧翔新材料有限公司 Preparation method of biomass charcoal material for removing phosphorus from sewage
CN114700103A (en) * 2022-04-12 2022-07-05 广州大学 Immobilized preparation method of metal-free carbon-based catalyst, product and application thereof
CN114700103B (en) * 2022-04-12 2023-10-27 广州大学 Immobilization preparation method of metal-free carbon-based catalyst, product and application of product
CN116535027A (en) * 2023-04-10 2023-08-04 广东绿韶环保工程有限公司 Sustainable reclaimed water recycling system treatment method
CN116535027B (en) * 2023-04-10 2023-11-10 广东绿韶环保工程有限公司 Sustainable reclaimed water recycling system treatment method

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