CN108946727B - Method for preparing activated carbon by using microalgae-alginate complex - Google Patents
Method for preparing activated carbon by using microalgae-alginate complex Download PDFInfo
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- CN108946727B CN108946727B CN201710357655.8A CN201710357655A CN108946727B CN 108946727 B CN108946727 B CN 108946727B CN 201710357655 A CN201710357655 A CN 201710357655A CN 108946727 B CN108946727 B CN 108946727B
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Abstract
The invention provides a method for preparing activated carbon by compounding microalgae-alginate and taking the obtained compound as a raw material, which comprises the step of reacting the microalgae-alginate compound through a physical activation process, a chemical activation process or a physical and chemical combined activation process so as to obtain the activated carbon. The invention uses the microalgae-alginate compound as the raw material for preparing the activated carbon, and the prepared activated carbon product has the advantages of large specific surface area, rich micropores, narrow pore size distribution and the like.
Description
Technical Field
The invention belongs to the field of activated carbon preparation, and particularly relates to a method for preparing activated carbon by using microalgae-alginate composite as a raw material.
Background
The activated carbon has the characteristics of large specific surface area, specially developed micropores, good electric and thermal conductivity, good chemical stability and the like, and is widely applied to the fields of catalysis, adsorption, medicines, new energy sources and the like. At present, the raw materials for preparing the activated carbon mainly come from wood, such as wood, coconut shell and the like, coal, such as lignite, bituminous coal, anthracite and the like, petroleum, such as petroleum coke and the like. In recent years, the use of other materials, such as biomass, to produce activated carbon has also received much attention. Microalgae is unicellular algae with a simple structure, the size of the unicellular algae is usually from several micrometers to several hundred micrometers, the unicellular algae has the characteristics of high light and efficiency, high biological yield, strong environmental adaptability and the like, is a biomass resource with great potential, and can be used for preparing biological oil and olefin, the food and medicine industry and the like. Alginate is polysaccharide formed by linear polymerization of monosaccharide aldehyde acid, is a pure compound, has a specific molecular formula and element composition, and has the characteristics of low toxic and side effects, degradability, high safety and the like. The use of alginates is currently mainly used as emulsifiers or thickeners in the food industry and the daily chemical industry, as binders or drug release agents in the pharmaceutical industry, etc. The active carbon is prepared by taking the microalgae-alginate composite as a raw material, so that the raw material source for preparing the active carbon can be enriched, the utilization of the microalgae and the alginate can be enriched, the oxygen content of the alginate is high as the microalgae is taken as a special unicellular life body, and the microalgae and the alginate are compounded, so that the active carbon material with rich pores and specific performance can be obtained.
CN102658083A discloses a method for preparing modified sludge activated carbon for removing multiple heavy metals in sewage sludge simultaneously, wherein sludge and sodium alginate are used as raw materials for preparing activated carbon, the method is to directly mix sodium alginate solution with sludge activated carbon to modify sludge activated carbon, and sodium alginate is not used as an activated carbon precursor to prepare activated carbon through carbonization. CN 104138743A discloses a preparation method of an algae-based magnetic activated carbon material, comprising the following steps: a. soaking the blue algae in the solution of the iron precursor for 12-24 hours; b. separating the soaked blue algae and then drying; c. and (3) carrying out high-temperature carbonization on the dried blue algae, and cooling to obtain the algae-based magnetic activated carbon material, wherein the iron precursor is subjected to high-temperature treatment in the method and does not generate pores, and the specific surface area of the obtained activated carbon is inevitably reduced by loading ferroferric oxide nanoparticles on the surface of the activated carbon.
Disclosure of Invention
The invention aims to provide a method for preparing activated carbon from novel raw materials.
To this end, the present invention provides a method for preparing activated carbon using a microalgae-alginate complex as a raw material, the method comprising reacting the microalgae-alginate complex through a physical activation process, a chemical activation process, or a physicochemical combined activation process, thereby obtaining the activated carbon,
wherein the physical activation process comprises the steps of heating the microalgae-alginate complex to the temperature of 150-500 ℃ in the nitrogen atmosphere for carbonization, then introducing carbon dioxide, water vapor, air or nitrogen for activation at the temperature of 400-900 ℃, and finally cooling, washing and drying to obtain the activated carbon,
the chemical activation process comprises the steps of mixing the microalgae-alginate compound with an activating agent, heating to 500 ℃ for carbonization, heating to 900 ℃ for activation, and cooling, washing and drying to obtain the activated carbon, wherein the activating agent is one or more selected from sulfuric acid, phosphoric acid, nitric acid, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate and zinc chloride;
the physical and chemical combined activation process comprises the steps of heating the microalgae-alginate complex to 150-900 ℃ in a nitrogen atmosphere for carbonization, then mixing with an activating agent, heating to 400-900 ℃ for activation, and finally cooling, washing and drying to obtain the activated carbon, wherein the activating agent is one or more selected from sulfuric acid, phosphoric acid, nitric acid, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate and zinc chloride.
In a preferred embodiment, the microalgae is one or more selected from the group consisting of scenedesmus, chlorella, chrysophyceae, tetraselmis, cyanobacteria, green algae, botryococcus, diatoms, and dunaliella.
In a preferred embodiment, the alginate is one or more of potassium alginate, sodium alginate, calcium alginate, zinc alginate, iron alginate, copper alginate, cobalt alginate, nickel alginate, palladium alginate, magnesium alginate and barium alginate.
In a preferred embodiment, the microalgae-alginate complex is obtained by mixing an aqueous microalgae solution with alginate and then air drying.
In a preferred embodiment, in the microalgae-alginate complex, the mass ratio of microalgae to alginate is 1:0.5 to 1: 5.
In a preferred embodiment, the washing is carried out with an HCl solution and then with water to neutrality.
In a preferred embodiment, the temperature increase to 400-900 ℃ is carried out at a temperature increase rate of 1-10 ℃/min.
In a preferred embodiment, the mass ratio of the microalgae-alginate complex to the activator is from 1:0.5 to 1: 5.
In a preferred embodiment, during said physical activation, N is2The flow rate is 50-200 ml/min.
In a preferred embodiment, the drying is carried out at 80 to 150 ℃.
In a preferred embodiment, the carbonization time is 1 to 4 hours and the activation time is 0.5 to 4 hours.
The invention provides a novel method for preparing activated carbon by taking a composite obtained by compounding microalgae and alginate as a raw material, the method can take various composites of the microalgae and the alginate as the raw material, thereby combining the advantages of the microalgae and the alginate, and the prepared activated carbon has a special pore structure, large specific surface area, rich micropores, large micropore volume and excellent performance, and enriches the utilization of the microalgae and the alginate.
Drawings
FIG. 1 is an SEM image of activated carbon prepared according to example 1 of the present invention;
FIG. 2 is N of activated carbon prepared according to example 1 of the present invention2An adsorption-desorption curve;
FIG. 3 is an SEM image of activated carbon prepared according to example 2 of the present invention;
FIG. 4 is N of activated carbon prepared according to example 2 of the present invention2An adsorption-desorption curve;
FIG. 5 is an SEM image of activated carbon prepared according to example 3 of the present invention;
FIG. 6 is N of activated carbon prepared according to example 4 of the present invention2Adsorption and desorption curves.
The specific implementation mode is as follows:
the invention prepares the activated carbon by taking the compound obtained by compounding the microalgae and the alginate as a raw material, and optimizes the preparation process to reduce the carbonization temperature and the energy consumption, thereby finally obtaining the activated carbon material with high specific surface area and excellent performance. The method comprises the step of reacting the microalgae-alginate complex through a physical activation process, a chemical activation process or a physical and chemical combined activation process to prepare the activated carbon.
More particularly, in the present inventionIn the method, the microalgae-alginate compound is used as a raw material, and the operation process for preparing the activated carbon by adopting the physical activation process can be as follows: under nitrogen atmosphere, preferably N2Heating the microalgae-alginate complex to 500 ℃ at a flow rate of 50-200ml/min, such as 120ml/min, carrying out carbonization reaction, such as lasting for 1-4h, introducing carbon dioxide, water vapor, air or nitrogen, heating to 900 ℃ at 400 ℃ for activation, such as lasting for 0.5-4h, cooling, washing with HCl solution (such as 1M solution), washing with water and drying to obtain the activated carbon product.
More specifically, in the method of the present invention, the operation process for preparing activated carbon by using the microalgae-alginate complex as a raw material and using the chemical activation process may be as follows: mixing the microalgae-alginate complex with an activating agent, drying, such as natural airing, to obtain a mixture of the complex and the activating agent, wherein the mass ratio of the complex to the activating agent is preferably 1:0.5-1:5, and the carbonization reaction is preferably carried out at a temperature rise rate of 1-10 ℃/min to 150-500 ℃, for example, for 1-4 hours, under a nitrogen atmosphere. Then, for example, the mixture of the compound and the activating agent is heated to an activation temperature of 400 ℃ to 900 ℃ at a heating rate of 1-10 ℃/min, for example, after activation for 0.5-4h, the activated carbon product is obtained after cooling, HCl solution (for example, 1M solution) washing, water washing and drying, wherein the activating agent used can be one or more of sulfuric acid, phosphoric acid, nitric acid, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or zinc chloride.
More specifically, in the method of the present invention, the microalgae-alginate complex is used as a raw material, and the operation process for preparing the activated carbon by adopting the physical and chemical combined activation process is as follows: under nitrogen atmosphere, preferably N2The flow rate is 50-200ml/min, for example 120ml/min, the temperature of the microalgae-alginate composite is raised to 150 ℃ and 500 ℃ for carbonization reaction, for example, lasts for 1-4 h. Thereafter, the carbonized complex is preferably cooled and then mixed with an activating agent, preferably in a mass ratio of the microalgae-alginate complex to the activating agent of 1:0.5 to 1:5, and the mixture of the microalgae-alginate char and the activating agent is warmed up, for example at a warming-up rate of 1 to 10 ℃/minWhen the temperature is 400-900 ℃, for example, after activation for 0.5-4h, cooling, washing with HCl solution (for example, 1M solution), washing with water and drying are carried out to obtain the activated carbon product, wherein the activating agent used can be one or more of sulfuric acid, phosphoric acid, nitric acid, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or zinc chloride.
Preferably, in the method of the present invention, the microalgae-alginate complex may be prepared as follows: uniformly mixing the aqueous solution of microalgae (which can be pre-pulverized into powder) with alginate, preferably in a mass ratio of microalgae to alginate of 1:0.5-1:5, and drying, for example by natural air drying, to obtain the desired microalgae-alginate complex.
Preferably, in the method of the present invention, the microalgae used may be one or more of scenedesmus, chlorella, chrysophyceae, tetraselmis, cyanobacteria, green algae, botryococcus, diatoms and dunaliella.
Preferably, in the method of the present invention, the alginate used may be one or more of potassium alginate, sodium alginate, calcium alginate, zinc alginate, iron alginate, copper alginate, cobalt alginate, nickel alginate, palladium alginate, magnesium alginate and barium alginate.
Preferably, in the method of the present invention, the temperature at which the carbonization is carried out is preferably 150-390 deg.C
Preferably, in the process of the invention, the temperature at which the activation is carried out is preferably 400-690 ℃.
The present invention is further illustrated by the following specific examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
Example 1: preparation of active carbon by using flat algae-sodium alginate compound as raw material
Firstly, uniformly dispersing 25g of Platymonas powder in deionized water in a beaker, adding sodium alginate, uniformly mixing, wherein the mass ratio of the Platymonas and the sodium alginate is 1: 2, and naturally drying to obtain the Platymonas-sodium alginate composite. Then, in a tube furnace, under a nitrogen atmosphere (N)2The flow rate is 120ml/min), the temperature of the obtained compound is raised to 500 ℃ at the temperature raising rate of 2.5 ℃/min, and the carbonization reaction is carried out for 1 h; then 5 ℃ is addedHeating to 800 ℃ at a heating rate of/min, activating for 1h, cooling to room temperature in a nitrogen atmosphere, taking out a reaction product, washing the reaction product with 1M HCl solution for three times, and washing the reaction product with deionized water to be neutral; and finally drying in an oven at 110 ℃ for 12h to obtain the finished product of the activated carbon. FIG. 1 is an SEM image of an activated carbon prepared according to example 1 of the present invention, the obtained activated carbon has a special structure and rich pores with different sizes; FIG. 2 is N of activated carbon prepared according to example 1 of the present invention2The adsorption and desorption curve shows that the obtained active carbon has a certain specific surface area, rich micropores and larger pores. Therefore, the active carbon prepared by the method has a special pore structure, large specific surface area, rich micropores and excellent performance.
Example 2: preparation of active carbon by using scenedesmus-sodium alginate compound as raw material
Firstly, uniformly dispersing 25g of scenedesmus powder in deionized water in a beaker, adding sodium alginate, uniformly mixing to obtain an alginic acid-alginate composite, then adding potassium hydroxide, uniformly mixing to obtain a mixture, and naturally airing, wherein the mass ratio of scenedesmus to sodium alginate to potassium hydroxide is 1: 1. Under nitrogen atmosphere (N)2The flow rate is 120ml/min), the obtained mixture is heated to 500 ℃ at the heating rate of 2.5 ℃/min, and the carbonization reaction is carried out for 1 h; then the temperature is raised to 700 ℃ at the heating rate of 5 ℃/min for activation for 2 h. Then, cooling to room temperature in a nitrogen atmosphere, taking out a reaction product, washing the reaction product with an HCl solution with the concentration of 1M for three times, and then washing the reaction product with deionized water to be neutral; and finally drying in an oven at 110 ℃ for 12h to obtain the finished product of the activated carbon. FIG. 3 is an SEM image of an activated carbon prepared according to example 2 of the present invention, the resulting activated carbon containing abundant and uniform pores; FIG. 4 is N of activated carbon prepared according to example 2 of the present invention2The adsorption and desorption curve shows that the obtained active carbon has high specific surface area and rich micropores. Therefore, the active carbon prepared by the method has the advantages of rich pores, large specific surface area, rich micropores and excellent performance.
Example 3: preparation of active carbon by using golden algae-potassium alginate compound as raw material
First, in a beaker, 25g were putThe golden algae is uniformly dispersed in deionized water, potassium alginate is added and uniformly mixed, wherein the mass ratio of the golden algae to the potassium alginate is 1: 1, and the golden algae-potassium alginate compound is obtained by natural drying. Then, in a tube furnace, under a nitrogen atmosphere (N)2The flow rate is 120ml/min), the temperature of the obtained compound is raised to 500 ℃ at the temperature raising rate of 2.5 ℃/min so as to carry out carbonization reaction on the compound for 1 h; heating to 700 ℃ at the heating rate of 5 ℃/min for activation for 1h, cooling to room temperature under the nitrogen atmosphere, taking out a reaction product, cleaning the reaction product with 1M HCl solution for three times, and washing the reaction product with deionized water to be neutral; and finally drying in an oven at 110 ℃ for 12h to obtain the finished product of the activated carbon. Fig. 5 is an SEM image of the activated carbon prepared according to example 3 of the present invention, and the resulting activated carbon has well-developed pores. Therefore, the active carbon prepared by the method has developed pores and large specific surface area.
Example 4: preparation of activated carbon from chlorella-calcium alginate compound
Firstly, uniformly dispersing 25g of chlorella in deionized water in a beaker, adding calcium alginate, uniformly mixing, wherein the mass ratio of the chlorella to the calcium alginate is 1: 1, and naturally drying to obtain the chlorella-calcium alginate composite raw material. Then, in a tube furnace, under a nitrogen atmosphere (N)2Flow rate of 120ml/min), and the obtained composite was heated to 400 ℃ at a heating rate of 2.5 ℃/min to perform a carbonization reaction on the composite for 1 hour. And cooling to room temperature in a nitrogen atmosphere, taking out a reaction product, and uniformly mixing the reaction product with potassium hydroxide serving as an activating agent according to the mass ratio of 1: 1. Then, heating to 750 ℃ at the heating rate of 5 ℃/min, activating for 0.5h, cooling to room temperature under the nitrogen atmosphere, taking out a reaction product, cleaning the reaction product with 1M HCl solution for three times, and then washing the reaction product with deionized water to be neutral; and finally drying in an oven at 110 ℃ for 12h to obtain the finished product of the activated carbon. FIG. 6 is N of activated carbon prepared according to example 4 of the present invention2The adsorption and desorption curve shows that the obtained activated carbon has high specific surface area and contains abundant micropores. Therefore, the activated carbon prepared by the method has the advantages of large specific surface area, rich micropores and large micropore volume.
Although specific embodiments of the invention have been described in detail, those skilled in the art will appreciate. Various modifications and substitutions of those details may be made in light of the overall teachings of the disclosure, and such changes are intended to be within the scope of the present invention. The full scope of the invention is given by the appended claims and any equivalents thereof.
Claims (8)
1. A method for preparing activated carbon from microalgae-alginate complex, the method comprising reacting the microalgae-alginate complex by a physical activation process, a chemical activation process or a physicochemical combined activation process to obtain the activated carbon,
wherein the physical activation process comprises the steps of heating the microalgae-alginate complex to the temperature of 150-500 ℃ in the nitrogen atmosphere for carbonization, then introducing carbon dioxide, water vapor, air or nitrogen for activation at the temperature of 400-900 ℃, and finally cooling, washing and drying to obtain the activated carbon,
the chemical activation process comprises the steps of mixing the microalgae-alginate compound with an activating agent, heating to 500 ℃ for carbonization, heating to 900 ℃ for activation, and cooling, washing and drying to obtain the activated carbon, wherein the activating agent is one or more selected from sulfuric acid, phosphoric acid, nitric acid, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate and zinc chloride;
the physical and chemical combined activation process comprises the steps of heating the microalgae-alginate complex to 150-900 ℃ in a nitrogen atmosphere for carbonization, then mixing with an activating agent, heating to 400-900 ℃ for activation, and finally cooling, washing and drying to obtain the activated carbon, wherein the activating agent is one or more selected from sulfuric acid, phosphoric acid, nitric acid, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate and zinc chloride,
the microalgae is one or more selected from Scenedesmus obliquus, Chlorella, Chrysophyta, Platymonas, blue algae, Chlorella, Botryococcus, Diatom and Dunaliella;
the alginate is one or more of potassium alginate, sodium alginate and magnesium alginate;
the microalgae-alginate complex is obtained by mixing a microalgae aqueous solution with alginate and then drying in the air.
2. The method of claim 1, wherein the mass ratio of microalgae to alginate in the microalgae-alginate complex is from 1:0.5 to 1: 5.
3. The method of claim 1, wherein the washing is with an HCl solution and then with water to neutrality.
4. The method as claimed in claim 1, wherein the temperature increase to 400-900 ℃ is performed at a temperature increase rate of 1-10 ℃/min.
5. The method of claim 1, wherein the mass ratio of the microalgae-alginate complex to the activator is from 1:0.5 to 1: 5.
6. The method of claim 1, wherein during said physical activation, N is2The flow rate is 50-200 ml/min.
7. The method of claim 1, wherein the drying is performed at 80-150 ℃.
8. The method of claim 1, wherein the time for the carbonization is 1 to 4 hours and the time for the activation is 0.5 to 4 hours.
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| CN111204817B (en) * | 2020-01-15 | 2021-06-01 | 李立欣 | Magnetic composite carbon prepared from harmful algal bloom and plastic and preparation method thereof |
| CN114733481B (en) * | 2022-04-10 | 2023-04-25 | 平罗县德润活性炭有限公司 | Method for preparing composite activated carbon |
| CN114933304B (en) * | 2022-05-06 | 2024-01-12 | 浙江科技学院 | Process for preparing biochar by utilizing green algae |
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