CN112403435A - Preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater - Google Patents
Preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater Download PDFInfo
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Abstract
The invention relates to a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater, which comprises the following steps: step one, pretreating raw materials; weighing raw materials; step three, heating and refluxing; step four, microwave activation; step five, washing and filtering; step six, drying; and step seven, cooling and storing. The active carbon prepared by the invention has a large amount of microporous structures, uniform pore size distribution and rich oxygen-containing functional groups on the surface, is beneficial to the attachment and deposition of dye molecules on the surface and is more suitable for adsorption. The removal rate of methylene blue dye can reach 99.9% to the maximum, the maximum adsorption capacity can reach 636.9mg/g, the method can be used for treating the dye wastewater containing cations, and the method has the advantages of simple preparation process, low cost, environmental protection and easy popularization.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a preparation method of KOH-microwave activated corncob activated carbon for treating wastewater containing cationic dye.
Background
The printing and dyeing wastewater is wastewater discharged from printing and dyeing factories which mainly process cotton, hemp, chemical fibers and blended products thereof. The printing and dyeing wastewater has the characteristics of large water quantity, high organic pollutant content, high alkalinity, large water quality change and the like, and belongs to one of industrial wastewater difficult to treat. Many methods for treating printing and dyeing wastewater include hydrogen peroxide oxidation, biodegradation, electrolysis, adsorption, and the like. The hydrogen peroxide oxidation method has simple treatment process, can effectively reduce the chroma of the waste water, has no secondary pollution, but has limited removal rate. The electrolysis method has high treatment efficiency but large power consumption and is not suitable for treating dye wastewater with large treatment capacity.
Activated carbon is a black solid carbon containing a porous structure. The sources of the activated carbon are very wide, and the most used activated carbon at present is prepared by high-temperature calcination of wood fiber, coconut shells and peach kernels. The carbon atoms in the activated carbon have various hybridization modes, and the combination arrangement of the carbon atoms is irregular, so that the activated carbon has a structure of a plurality of pores and gaps. The activated carbon contains a small amount of elements such as nitrogen, oxygen, hydrogen, chlorine and the like, and the elements form abundant functional groups such as hydroxyl, carboxyl and the like on the surface of the activated carbon, and the functional groups can chemically react with cations, so that the activated carbon can effectively remove the cations in the dye wastewater. In addition, the activated carbon has a relatively large specific surface area, which enables the activated carbon to have high adsorption efficiency and facilitates further modification of the activated carbon. In addition, the activated carbon has the advantages of high efficiency, economy, reproducibility and no secondary pollution, so that the activated carbon is widely applied to the treatment of the wastewater containing the cationic dye.
However, the adsorption performance of the existing activated carbon materials to cations and organic pollutants needs to be improved.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater, which can effectively solve the problems in the background technology.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater specifically comprises the following steps:
(1) the corncobs were washed with distilled water. Then, the mixture is dried in a constant temperature blast drying oven. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of KOH solution (5 wt%, 10 wt%, 15 wt%) in proportion, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600-800W, the activation time is 7-11 min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing the activated carbon with 0.1M HCl for three times, washing the activated carbon with distilled water until the pH value of a rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
Furthermore, in step (2), the optimum mass fraction of the desired KOH solution is 10% by weight.
In the step (4), the optimal power of the microwave activation is 600W, and the optimal activation time is 7 min.
The invention has the following technical effects:
the invention provides a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater, which is characterized in that crop waste corncobs are heated and refluxed in the presence of KOH, and in order to ensure that the interior and the exterior of the corncobs can be fully contacted with KOH molecules, when the corncobs are heated in a microwave chemical reactor, KOH and the corncobs react and form a certain active point in carbonized carbon oxygen in a short time, so that activation is simultaneously carried out to form micropores. And the water molecules in the KOH reagent are polar molecules, so that the microwave absorption capacity of the corncob meal can be enhanced, the reaction temperature required by the reaction can be reached in a short time by the reactor, and the preparation time is greatly shortened. Corncobs interact with KOH to form a large number of new holes on the basis of an initial hole structure, then the holes are further expanded, and the last holes are combined and communicated, so that high adsorption performance is achieved.
The active carbon prepared by the invention has a large amount of microporous structures, uniform pore size distribution and rich oxygen-containing functional groups on the surface, is beneficial to the attachment and deposition of dye molecules on the surface and is more suitable for adsorption.
The active carbon prepared by the method has the highest removal rate of 99.9 percent for methylene blue dye, the maximum adsorption capacity of 636.9mg/g, can be used for treating wastewater containing cationic dye, and has the advantages of simple preparation process, low cost and environmental protection.
Detailed description of the preferred embodiments
The adsorption performance of the activated carbon is characterized by the removal rate of methylene blue. The determination steps are as follows:
weighing 0.01g of the activated carbon obtained by the group (5) in the microwave power of 600w for 7min, respectively, adding the activated carbon into a conical flask containing 50mL of methylene blue solution with the initial concentration of 50, 100, 200, 300, 400 and 500mg/L, respectively, sealing the flask mouth, and transferring the flask into a constant-temperature shaking table to adsorb the methylene blue under the condition of keeping out of the sun. The rotation speed of the shaker was 150rpm, the temperature of the water bath was set at 30 ℃ and the time was set at 24h until equilibrium was reached. After the adsorption experiment was completed, the methylene blue solution after adsorption was taken out and filtered by using a syringe and a needle filter (0.22 μm), and the supernatant was separated. And measuring the absorbance of the solution at 664nm by using an ultraviolet-visible spectrophotometer, wherein the methylene blue removal rate of the activated carbon can be obtained by using a standard curve by using a methylene blue solution of 10mg/L as a standard sample and distilled water as a blank sample.
Example 1:
a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater comprises the following steps:
(1) the corncobs were washed with distilled water. Then, the mixture is dried in a constant temperature blast drying oven. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of a KOH solution with a mass fraction of 10 wt%, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600W, the activation time is 7min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing with 0.1HCl, washing with distilled water until the pH value of the rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
The methylene blue adsorption experiment of the activated carbon obtained above shows that the methylene blue removal rate of the activated carbon is about 99.9% and the equilibrium adsorption capacity is about 249.9mg/g in 50mL of methylene blue solution with the concentration of 50 mg/L.
Example 2:
a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater comprises the following steps:
(1) the corncobs were washed with distilled water. Then, the mixture is dried in a constant temperature blast drying oven. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of a KOH solution with a mass fraction of 10 wt%, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600W, the activation time is 7min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing with 0.1HCl, washing with distilled water until the pH value of the rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
The methylene blue adsorption test of the activated carbon obtained above shows that the methylene blue removal rate of the activated carbon is about 96.4% and the equilibrium adsorption amount is about 482.1mg/g in 50mL of methylene blue solution with the concentration of 100 mg/L.
Example 3:
a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater comprises the following steps:
(1) the corncobs were washed with distilled water. Then, the mixture is dried in a constant temperature blast drying oven. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of a KOH solution with a mass fraction of 10 wt%, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600W, the activation time is 7min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing with 0.1HCl, washing with distilled water until the pH value of the rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
The methylene blue adsorption experiment of the activated carbon obtained in the above way shows that the methylene blue removal rate of the activated carbon is about 57.0% and the equilibrium adsorption amount is about 570.2mg/g in 50mL of methylene blue solution with the concentration of 200 mg/L.
Example 4:
a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater comprises the following steps:
(1) the corncobs were washed with distilled water. Then, the mixture is dried in a constant temperature blast drying oven. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of a KOH solution with a mass fraction of 10 wt%, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600W, the activation time is 7min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing with 0.1HCl, washing with distilled water until the pH value of the rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
The methylene blue adsorption experiment of the activated carbon obtained above shows that the methylene blue removal rate of the activated carbon is about 40.6% and the equilibrium adsorption capacity is about 609.5mg/g in 50mL of methylene blue solution with the concentration of 300 mg/L.
Example 5:
a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater comprises the following steps:
(1) the corncobs were washed with distilled water. Then, the mixture is dried in a constant temperature blast drying oven. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of a KOH solution with a mass fraction of 10 wt%, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600W, the activation time is 7min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing with 0.1HCl, washing with distilled water until the pH value of the rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
The methylene blue adsorption experiment of the activated carbon obtained above shows that the methylene blue removal rate of the activated carbon is about 30.8% and the equilibrium adsorption capacity is about 617.0mg/g in 50mL of methylene blue solution with the concentration of 400 mg/L.
Example 6:
a preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater comprises the following steps:
(1) the corncobs were washed with distilled water. Then, the mixture is dried in a constant temperature blast drying oven. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of a KOH solution with a mass fraction of 10 wt%, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600W, the activation time is 7min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing with 0.1HCl, washing with distilled water until the pH value of the rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
The methylene blue adsorption experiment of the activated carbon obtained above shows that the methylene blue removal rate of the activated carbon is about 25.5% and the equilibrium adsorption capacity is about 635.4mg/g in 50mL of methylene blue solution with the concentration of 500 mg/L.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those of ordinary skill in the art can readily practice the present invention as described herein; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (3)
1. A preparation method of KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater comprises the following steps: step one, pretreating raw materials; weighing raw materials; step three, refluxing, heating and drying; step four, microwave activation; step five, washing and filtering; step six, drying; step seven: cooling and storing; the method is characterized in that:
(1) washing the corncobs with distilled water, and then placing the corncobs in a constant-temperature air-blast drying oven for drying. Then, the dried corncobs are taken out and crushed by a crusher and then screened by a 50-mesh screen, the screened corncob powder is uniformly spread and placed in a vacuum drying oven, and the dried corncob powder is dried for 24 hours under the condition of 60 ℃ so as to remove the moisture of the raw materials. Finally, the dried corncob meal is collected and placed in a dryer for use.
(2) 5g of corncob powder was added to 100mL of KOH solution (5 wt%, 10 wt%, 15 wt%) in proportion, stirred and mixed well.
(3) And (3) placing the mixture obtained in the step (2) into a round-bottom flask with the volume of 250mL, adding magnetons, and refluxing in a constant-temperature water bath kettle at 80 ℃ for 5 hours. After completion of the reflux, the mixture was placed in a vacuum oven and dried at 105 ℃ for 24 hours to remove water.
(4) And (4) taking out the solid mixture obtained in the step (3), placing the solid mixture in a three-neck flask for microwave activation, wherein the activation power is 600-800W, the activation time is 7-11 min, and obtaining the product activated carbon after the reaction is finished.
(5) And (3) after the temperature in the three-neck flask is reduced to room temperature, collecting the activated carbon, washing the activated carbon by using 0.1M HCl, washing the activated carbon by using distilled water until the pH value of a rinsing solution is about neutral, and filtering the obtained activated carbon by suction filtration.
(6) And (4) putting the activated carbon obtained in the step (5) into a vacuum drying oven, and drying for 24 hours at the temperature of 105 ℃.
(7) And (4) cooling the product dried in the step (6) to room temperature, grinding to obtain a finished product, and sealing and storing.
2. The method for preparing KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater according to claim 1, wherein the KOH-microwave activated corncob activated carbon comprises the following steps: in the step (2), the optimal mass fraction of the KOH solution is 10 wt%.
3. The method for preparing KOH-microwave activated corncob activated carbon for treating cationic dye-containing wastewater according to claim 1, wherein the KOH-microwave activated corncob activated carbon comprises the following steps: in the fourth step, the optimal power of microwave activation is 600W, and the optimal activation time is 7 min.
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Application publication date: 20210226 |