CN111186836A - Preparation method of corncob-based activated carbon - Google Patents
Preparation method of corncob-based activated carbon Download PDFInfo
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- CN111186836A CN111186836A CN201811350982.1A CN201811350982A CN111186836A CN 111186836 A CN111186836 A CN 111186836A CN 201811350982 A CN201811350982 A CN 201811350982A CN 111186836 A CN111186836 A CN 111186836A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid 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
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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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Abstract
The invention discloses a preparation method of corncob-based activated carbon. The method comprises the following steps: firstly, washing, drying and grinding the corncobs into powder, immersing the corncobs into a treatment solution, then placing the corncobs into a reaction kettle, heating to 180-300 ℃, reacting for 3-6 hours, and cooling to room temperature to obtain a material I; then, washing and drying the first material, and soaking the first material in a KOH solution to obtain a second material; and then placing the second material into a microwave oven, heating for 10-20 minutes in a nitrogen atmosphere, cooling to room temperature, filtering, washing the product with deionized water until the pH value is unchanged, and drying to obtain the corncob-based activated carbon. The preparation method provided by the invention has the advantages of simple process and short reaction time, and the prepared activated carbon has good adsorption property on methylene blue.
Description
Technical Field
The invention belongs to the technical field of activated carbon preparation, and particularly relates to a preparation method of corncob-based activated carbon.
Background
The biomass is rich in carbon and can be used for preparing various carbon functional materials as a renewable energy source, the consumption and the dependence of human beings on the traditional fossil energy sources can be greatly reduced by using the biomass, and the harm and the pollution to the environment caused by the use of the fossil energy sources are effectively relieved, so that the biomass has important significance on the energy utilization of sustainable development and the natural environment. In China, a large amount of biomass waste is treated by burning and burying or even directly discharging to the environment in most cases, and the conversion rate is about 15 percent. This not only causes environmental pollution, but also a serious waste of available resources. Therefore, biomass waste is properly treated, modified and utilized by taking measures, and the excellent characteristics of the biomass waste are developed, so that the biomass waste can be widely applied to a plurality of fields such as buildings, environmental protection, medicines and the like. The corncob is typical biomass waste which is widely distributed, has rich reserves, has the characteristics of reproducibility, easy biodegradation and the like, can be used for effectively chemically converting the corncob biomass waste into a novel environment-friendly material with excellent performance, and has wide application prospect.
The purpose of preparing the activated carbon by the biomass is to convert the biomass by a certain method to obtain a carbon material with an ideal pore structure and surface chemical groups. Hydrothermal carbonization is a thermochemical conversion technique that uses subcritical water to convert dry or wet biomass to carbonaceous products by fractionation techniques, which require relatively low temperatures and pressures and mild reaction conditions. The carbonization temperature depends on the type of starting material and its decomposition temperature, and in most cases the temperature required for hydrothermal carbonization is between 150 ℃ and 350 ℃. The hydrothermal carbonization leads the biomass to generate dehydration and decarbonylation reactions in the carbonization process, endows the biochar with rich chemical groups on the surface, and provides a better precursor for preparing the activated carbon. However, the single hydrothermal carbonization process still has some disadvantages, such as low specific surface area of the product, single structure, etc., which affect the subsequent activation effect. Generally, activated carbon is prepared by further activating a biomass raw material or a carbide precursor, but the conventional physical and chemical activation methods are long in time consumption, require high reaction temperature, cause high energy consumption, have high initial equipment investment cost, and most importantly, are difficult to control the pore size distribution according to the expected product.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of activated carbon, which takes biomass waste corncobs as raw materials to prepare the activated carbon with good methylene blue adsorption capacity and can be widely applied to the fields of decolorization, separation, wastewater treatment and the like. The preparation method has the advantages of simple process, short reaction time, energy conservation and good economic and social benefits.
The technical scheme of the invention is as follows:
a preparation method of corncob-based activated carbon comprises the following steps:
step one, washing, drying and grinding the corncobs into powder, immersing the corncobs into a treatment solution, then placing the corncobs into a reaction kettle, heating to 180-300 ℃, reacting for 3-6 hours, and cooling to room temperature to obtain a material I, wherein the treatment solution is a mixed solution of citric acid and water; step two, washing and drying the material I, and soaking the material I in a KOH solution to obtain a material II; and step three, placing the material II into a microwave oven, heating for 10-20 minutes in the nitrogen atmosphere, cooling to room temperature, filtering, washing the product with deionized water until the pH value is unchanged, and drying to obtain the corncob-based activated carbon.
The preparation method of the corncob-based activated carbon comprises the following steps of adding the treatment fluid into the corncob in a liquid-material ratio of 5-20: 1;
the preparation method of the corncob-based activated carbon comprises the following steps of firstly, controlling the amount concentration of a citric acid substance in a treatment solution to be 1-3;
in the preparation method of the corncob-based activated carbon, the temperature rise speed of the temperature rise to 180-300 ℃ in the step one is 6-15 ℃/min;
the preparation method of the corncob-based activated carbon comprises the step two of soaking in KOH solution, wherein the mass ratio of KOH to the material I is 0.5-4: 1;
the preparation method of the corncob-based activated carbon comprises the step two of soaking in KOH solution for 8-12h at the temperature of 85-110 ℃;
the preparation method of the corncob-based activated carbon comprises the following steps that in the third step, the power of the microwave oven is 200-;
the preparation method of the corncob-based activated carbon comprises the third step of drying at the temperature of 95-110 ℃.
Compared with the prior art, the invention has the following advantages and technical effects:
1. the corncob-based activated carbon prepared by the preparation method provided by the invention has good performance, wherein the specific surface area reaches more than 500m2/g, and the methylene blue adsorption value exceeds 450 mg/g.
2. The preparation method provided by the invention has the advantages of simple process, simple and convenient operation and short reaction time, and the corncob-based activated carbon prepared from the waste biomass can be widely applied to the fields of decolorization, separation, wastewater treatment and the like, so that the energy is saved, the effect of changing waste into valuables is achieved, and the preparation method has good social and economic benefits.
Detailed description of the preferred embodiments
The following description is only exemplary of the present invention and is not intended to limit the present invention in any way; 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.
Example 1
A preparation method of corncob-based activated carbon comprises the following steps:
step one, washing, drying and grinding corncobs into powder, soaking 5g of the corncobs into 30mL of treatment solution, then placing the corncobs into a reaction kettle, heating to 200 ℃, reacting for 3 hours at the heating rate of 8 ℃/min, and cooling to room temperature to obtain a material I, wherein the treatment solution is 1mol/L citric acid solution; step two, after the material I is washed and dried, 1.12g of the material I is soaked in 20mL of KOH solution with the concentration of 1mol/L, and the material II is obtained after soaking for 9 hours at the temperature of 90 ℃; and step three, putting the material II into a microwave oven, setting the power of the microwave oven at 200W, heating for 8 minutes in the nitrogen atmosphere, cooling to room temperature, filtering, washing the product with deionized water until the pH value is unchanged, and drying at 105 ℃ to obtain the corncob-based activated carbon.
Example 2
A preparation method of corncob-based activated carbon comprises the following steps:
step one, washing, drying and grinding corncobs into powder, soaking 5g of the corncobs into 70mL of treatment solution, then placing the corncobs into a reaction kettle, heating to 250 ℃, reacting for 5 hours at the heating rate of 12 ℃/min, and cooling to room temperature to obtain a material I, wherein the treatment solution is 2mol/L citric acid solution; step two, after the material I is washed and dried, 1.12g of the material I is soaked in 40mL of KOH solution with the concentration of 1mol/L, and the material II is obtained after soaking for 10 hours at the temperature of 85 ℃; and step three, putting the material II into a microwave oven, setting the power of the microwave oven at 400W, heating for 12 minutes in a nitrogen atmosphere, cooling to room temperature, filtering, washing the product with deionized water until the pH value is unchanged, and drying at 105 ℃ to obtain the corncob-based activated carbon.
Example 3
A preparation method of corncob-based activated carbon comprises the following steps:
step one, washing, drying and grinding corncobs into powder, soaking 5g of the corncobs into 80mL of treatment solution, then placing the corncobs into a reaction kettle, heating to 275 ℃, reacting for 8 hours at the heating rate of 12 ℃/min, and cooling to room temperature to obtain a material I, wherein the treatment solution is 3mol/L citric acid solution; step two, after the material I is washed and dried, 1.12g of the material I is soaked in 60mL of KOH solution with the concentration of 1mol/L, and the material II is obtained after soaking for 8 hours at the temperature of 105 ℃; and step three, putting the material II into a microwave oven, setting the power of the microwave oven at 600W, heating for 20 minutes in a nitrogen atmosphere, cooling to room temperature, filtering, washing the product with deionized water until the pH value is unchanged, and drying at 108 ℃ to obtain the corncob-based activated carbon.
Example 4
A preparation method of corncob-based activated carbon comprises the following steps:
step one, washing, drying and grinding corncobs into powder, soaking 5g of the corncobs into 100mL of treatment solution, then placing the corncobs into a reaction kettle, heating to 225 ℃, reacting for 5 hours at the heating rate of 6 ℃/min, and cooling to room temperature to obtain a material I, wherein the treatment solution is 3mol/L citric acid solution; step two, after the material I is washed and dried, 1.12g of the material I is soaked in 40mL of KOH solution with the concentration of 1mol/L, and the material II is obtained after soaking for 12 hours at the temperature of 85 ℃; and step three, putting the material II into a microwave oven, setting the power of the microwave oven at 400W, heating for 15 minutes in a nitrogen atmosphere, cooling to room temperature, filtering, washing the product with deionized water until the pH value is unchanged, and drying at 110 ℃ to obtain the corncob-based activated carbon.
The corncob-based activated carbon prepared in the above examples was subjected to performance tests, and the results are shown in the following table:
TABLE 1 corncob-based activated carbon specific surface area and methylene blue adsorption value
| Item | Specific surface area/m2/g | Methylene blue adsorption value/mg/g |
| Example 1 | 511.80 | 451.75 |
| Example 2 | 621.80 | 474.82 |
| Example 3 | 649.23 | 481.24 |
| Example 4 | 857.59 | 550.24 |
From the results, the preparation method provided by the invention successfully prepares the activated carbon from the biomass waste corncobs, the specific surface area reaches over 500m2/g, and the adsorption value to methylene blue exceeds 450 mg/g. In the development process of the invention, researchers find that the treatment liquid has obvious influence on the surface functional groups of the activated carbon material and is also the key for improving the adsorption performance of the activated carbon material.
In conclusion, the corncob-based activated carbon prepared by the preparation method provided by the invention is simple in process, short in reaction time and good in adsorption performance, the application range of the corncob-based activated carbon is expanded, and the economic benefit is improved.
Claims (8)
1. A preparation method of corncob-based activated carbon is characterized by comprising the following steps:
step one, washing, drying and grinding the corncobs into powder, immersing the corncobs into a treatment solution, then placing the corncobs into a reaction kettle, heating to 180-300 ℃, reacting for 3-6 hours, and cooling to room temperature to obtain a material I, wherein the treatment solution is a mixed solution of citric acid and water;
step two, washing and drying the material I, and soaking the material I in a KOH solution to obtain a material II;
and step three, placing the material II into a microwave oven, heating for 10-20 minutes in the nitrogen atmosphere, cooling to room temperature, filtering, washing the product with deionized water until the pH value is unchanged, and drying to obtain the corncob-based activated carbon.
2. The process for the production of corncob-based activated carbon as claimed in claim 1, wherein the liquid-to-material ratio of the treatment liquid to the corncobs added in the first step is 5-20: 1;
3. the method for producing a corncob-based activated carbon as claimed in claim 1, wherein the amount concentration of the citric acid substance in the treatment liquid of the step one is 1 to 3;
4. the method for preparing corncob-based activated carbon as in claim 1, wherein the temperature rise rate of the temperature rise to 180-300 ℃ in the step one is 6-15 ℃/min;
5. the method for preparing corncob-based activated carbon as claimed in claim 1, wherein in the second step, the activated carbon is soaked in a KOH solution, wherein the mass ratio of KOH to the first material is 0.5-4: 1;
6. the method for preparing corncob-based activated carbon as claimed in claim 1, wherein in the second step, the activated carbon is soaked in KOH solution for 8-12h at 85-110 ℃;
7. the preparation method of corncob based activated carbon as in claim 1, wherein in the third step, the power of the microwave oven is 200-800 w;
8. the method for preparing corncob-based activated carbon as claimed in claim 1, wherein the drying temperature in the third step is 95-110 ℃.
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| CN201811350982.1A CN111186836A (en) | 2018-11-14 | 2018-11-14 | Preparation method of corncob-based activated carbon |
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| CN201811350982.1A CN111186836A (en) | 2018-11-14 | 2018-11-14 | Preparation method of corncob-based activated carbon |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919462A (en) * | 2021-02-05 | 2021-06-08 | 中国铝业股份有限公司 | Preparation method of nano activated carbon |
| CN113694035A (en) * | 2021-10-09 | 2021-11-26 | 药大制药有限公司 | Preparation method of sildenafil tablets |
| CN114804099A (en) * | 2022-04-23 | 2022-07-29 | 河南工业大学 | Preparation method of corncob-based activated carbon activated by two-step method, product and application of product |
| CN116041989A (en) * | 2023-01-10 | 2023-05-02 | 聚能新材料科技(荆门)有限公司 | Biomass carbon sphere, preparation method thereof, antistatic composite material and preparation method thereof |
| CN116443849A (en) * | 2023-04-27 | 2023-07-18 | 安徽建筑大学 | Porous carbon material with high specific surface area and preparation method and application thereof |
-
2018
- 2018-11-14 CN CN201811350982.1A patent/CN111186836A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919462A (en) * | 2021-02-05 | 2021-06-08 | 中国铝业股份有限公司 | Preparation method of nano activated carbon |
| CN113694035A (en) * | 2021-10-09 | 2021-11-26 | 药大制药有限公司 | Preparation method of sildenafil tablets |
| CN114804099A (en) * | 2022-04-23 | 2022-07-29 | 河南工业大学 | Preparation method of corncob-based activated carbon activated by two-step method, product and application of product |
| CN116041989A (en) * | 2023-01-10 | 2023-05-02 | 聚能新材料科技(荆门)有限公司 | Biomass carbon sphere, preparation method thereof, antistatic composite material and preparation method thereof |
| CN116443849A (en) * | 2023-04-27 | 2023-07-18 | 安徽建筑大学 | Porous carbon material with high specific surface area and preparation method and application thereof |
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Application publication date: 20200522 |