CN114349004A - Preparation method of biomass porous carbon for water treatment - Google Patents
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Abstract
The invention discloses a preparation method of biomass porous carbon for water treatment, which comprises the steps of preparing a dry biomass/alkaline activator mixture; combusting the biomass/alkaline activator mixture in flame at 400-500 ℃ to obtain a black fluffy precursor; carrying out segmented pyrolysis on the precursor in an inert gas atmosphere: cooling to room temperature after pyrolysis to obtain a semi-finished product, adding an excessive hydrochloric acid solution into the semi-finished product, uniformly stirring, standing for 4 hours, and filtering to obtain a black solid substance; repeatedly washing the black solid substance with deionized water, and filtering after each washing until the filtrate is neutral; and drying the washed black solid matter at 105 ℃, and grinding the black solid matter after drying to obtain the biomass porous carbon particles. The biomass porous carbon prepared by the method has high adsorption capacity, is friendly to water and avoids secondary pollution.
Description
Technical Field
The invention belongs to the technical field of biomass porous carbon preparation.
Background
The traditional raw materials for preparing the porous carbon mainly comprise non-renewable resources such as coal, petroleum, asphalt and the like. In recent years, the production of porous carbon using biomass as a carbon source has received increasing attention. The agricultural and forestry wastes are wide in source and low in cost, and the porous carbon prepared from the agricultural and forestry wastes can improve the product value and further solve the environmental problem. The higher the porosity of the biomass porous carbon is, the more excellent the performances of all aspects of the biomass porous carbon are, and particularly, the specific surface area and the adsorption capacity can be improved. However, the current biomass porous carbon used in water treatment is also required to be improved in adsorption capacity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of biomass porous carbon for water treatment, which solves the technical problem of how to improve the adsorption capacity of the biomass porous carbon.
In order to solve the technical problems, the technical scheme of the invention is as follows: a preparation method of biomass porous carbon for water treatment comprises the following steps:
preparing a dry biomass/alkaline activator mixture by a pretreatment process;
combusting the biomass/alkaline activator mixture in flame at 400-500 ℃ to obtain a black fluffy precursor;
and (2) carrying out segmented pyrolysis on the precursor in an inert gas atmosphere, wherein activation simultaneously occurs in the pyrolysis process: in the first stage of pyrolysis, the temperature is raised to 300 ℃ at the temperature raising speed of 3-10 ℃/min, and the temperature is kept for 1-3 h; the second stage of pyrolysis is to heat the mixture from 300 ℃ to 850 ℃ at a heating rate of 2-5 ℃/min and keep the temperature for 1-3 h;
cooling to room temperature after pyrolysis to obtain a semi-finished product, adding an excessive hydrochloric acid solution into the semi-finished product, uniformly stirring, standing for 4-6 hours, and filtering to obtain a black solid substance; repeatedly washing the black solid substance with deionized water, and filtering after each washing until the filtrate is neutral;
and drying the washed black solid matter at 105 ℃, and grinding the black solid matter after drying to obtain the biomass porous carbon which can be powder or porous carbon particles.
In order to obtain biomass porous carbon with higher adsorption capacity as much as possible, the flow rate of the inert gas is preferably controlled to be 40mL/min, and the concentration of hydrochloric acid is preferably controlled to be 1 mol/L.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the biomass/alkaline activator mixture is subjected to combustion treatment before pyrolysis, so that oxygen-containing functional groups on the surface of the biomass porous carbon can be increased, and the increase of the oxygen-containing functional groups can promote the improvement of adsorption capacity. Meanwhile, the combustion treatment enables hemicellulose and cellulose in the biomass to be partially decomposed to generate carbon dioxide, carbon monoxide and other small molecule gases and bio-oil. The small molecular gas enables the biomass after combustion to be fluffy and porous, and the biological oil is further combusted and decomposed into carbon dioxide and water. The holes generated by combustion are maintained in the subsequent pyrolysis, and the activator can fully act with the biomass carbon substrate to obtain better activation effect.
2. More importantly, the content of hemicellulose and cellulose in the biomass is reduced through combustion reaction at 400-500 ℃, and more oxygen elements are introduced. In the pyrolysis process, the content of the bio-oil generated by the pyrolysis of cellulose or hemicellulose is reduced, so that the filling or blocking of a part of pore structures generated by pyrolysis activation by the bio-oil is reduced, and the specific surface area and the porosity of the material are improved. With the increase of the specific surface area and the increase of the pore structure, the active sites of the porous carbon increase, and thus the adsorption capacity is improved. In addition, the introduced oxygen element forms oxygen-containing functional groups in pyrolysis, which is beneficial to removing cationic pollutants by adsorption.
3. The reduction of the content of the bio-oil is more friendly to the water body environment, and the secondary pollution of the biomass porous carbon in the water treatment application can be reduced. In addition, the alkaline activator is neutralized by hydrochloric acid and then repeatedly washed to be neutral, so that the water environment friendliness is improved.
4. The biomass is washed to remove dust and impurities in order to reduce the influence of the inactive adsorbent components on the activation process. And then, the biomass and the alkaline activating agent are mixed, and deionized water is added to be fully stirred, so that the alkaline activating agent can be promoted to be uniformly dispersed and distributed in the biomass, and preparation is made for preparing the high-adsorption-capacity biomass/alkaline activating agent in the subsequent steps.
5. The invention can effectively increase the pore structure, specific surface area and adsorption capacity of the biomass porous carbon, has simple and convenient whole preparation process and low cost, and is a novel method for preparing the biomass porous carbon, which is easy to realize. Provides a simple and effective way for preparing the high-performance biomass porous carbon, and further can expand the application field of the high-performance biomass porous carbon. Meanwhile, biomass is fully utilized, and the problem that the accumulation of biomass easily causes environmental pollution is solved.
Drawings
FIG. 1 is a pictorial representation of a black fluffy precursor obtained after a combustion treatment in example 1;
FIG. 2 is an SEM image of the biomass porous carbon prepared in comparative example 1;
FIG. 3 is an SEM image of the biomass porous carbon prepared in example 1;
FIG. 4 is a graph comparing nitrogen adsorption isotherms of biomass porous carbon prepared in example 1 and comparative example 1;
FIG. 5 is a graph comparing pore size distribution of biomass porous carbon prepared in example 1 and comparative example 1;
FIG. 6 is a comparison graph of methylene blue isotherms of different initial concentrations adsorbed by biomass porous carbon prepared in example 1 and comparative example 1;
fig. 7 is a comparison graph of isotherms of methyl orange adsorbed at different initial concentrations by the biomass porous carbon prepared in example 1 and comparative example 1.
Detailed Description
Example 1
(1) Cleaning and drying the purchased sorghum vinasse, weighing 30 g of the sorghum vinasse into a beaker, and adding KOH: weighing KOH and vinasse according to the weight ratio of vinasse =1:3, mixing the KOH and the vinasse, adding 200 mL of deionized water, stirring uniformly, standing at room temperature for 24h, then putting into a drying oven, and drying at 105 ℃ for 24h to obtain a vinasse/KOH mixture.
(2) Processing the dried mixture into blocks with appropriate volume (preferably, thickness: 0.3-0.5 cm, length and width: 1-1.5 cm), clamping with tweezers, placing on the flame of alcohol burner (1.5-2 cm away from the wick, and measuring at temperature of about 400-.
(3) And placing the obtained precursor into a corundum crucible, placing the corundum crucible into a tube furnace, heating to 300 ℃, keeping the temperature for 1 h, continuing to heat to 850 ℃, keeping the temperature for 1 h, cooling to room temperature, taking out the corundum crucible, repeatedly cleaning with 1M HCl and deionized water until the temperature is neutral (pH-7), filtering, collecting, placing the corundum crucible in a drying oven at 105 ℃, drying for 24h, and grinding to obtain the biomass porous carbon, wherein the biomass porous carbon is marked as FPC-3.
(4) The prepared porous carbon (FPC-3) was used for Methylene Blue (MB) solution adsorption: weighing 10 mg of FPC-3 into a conical flask, respectively adding 40mL of methylene blue solution (100-700 mg/L) with different concentrations, shaking for 24h on an oscillator, and filtering and adsorbing the solution with a 0.45 mu m filter membrane; measuring absorbance of the methylene blue solution before and after adsorption at a wavelength of 664 nm by using an ultraviolet spectrophotometer, and calculating the concentration of the solution according to a standard curve (y =0.05569 x); and further calculates the adsorption capacity of FPC-3.
(5) The prepared porous carbon (FPC-3) was used for Methyl Orange (MO) solution adsorption: weighing 10 mg of FPC-3 into a conical flask, respectively adding 40mL of methyl orange solution (50-350 mg/L) with different concentrations, shaking for 24h on an oscillator, and filtering and adsorbing the solution with a 0.45 mu m filter membrane; measuring absorbance of the methyl orange solution before and after adsorption at a wavelength of 464 nm by using an ultraviolet spectrophotometer, and calculating the solution concentration according to a standard curve (y =0.07288 x); and then the FPC-3 adsorption capacity was calculated.
Comparative example 1 was provided for example 1, and comparative example 1 differed from example 1 only in that comparative example 1 lacked a combustion treatment step, i.e., staged pyrolysis (simultaneous activation and pyrolysis) was performed directly after pretreatment to produce a distillers' grains/KOH mixture.
The SEM image of the biomass porous carbon prepared in comparative example 1 is shown in fig. 2, the SEM image of the biomass porous carbon prepared in example 1 is shown in fig. 3, and comparing fig. 2 and fig. 3, it is apparent that the biomass porous carbon prepared in example 1 has denser pores. It can be seen from fig. 4 that the nitrogen adsorption capacity of example 1 is significantly higher than that of comparative example 1, and it can be seen from fig. 5 that the micro/meso pores of example 1 are more numerous than that of comparative example 1; with reference to fig. 4 and 5, the material of example 1 has a more developed pore structure, a higher specific surface area and more available active sites, which is more beneficial for adsorptive removal of contaminants. Comparing fig. 6, the adsorption capacity of example 1 for methylene blue greatly exceeds that of comparative example 1 for methylene blue, and likewise, the results of fig. 7 show that example 1 has a higher adsorption capacity for methyl orange than comparative example 1. This shows that the method obviously improves the adsorption capacity of methylene blue and methyl orange.
Example 2
(1) Using the same raw materials as in example 1, 30 g were weighed into a beaker, as NaOH: weighing KOH and vinasse according to the weight ratio of vinasse =1:5, mixing the KOH and the vinasse, adding 200 mL of deionized water, stirring uniformly, standing at room temperature for 24h, then putting into a drying oven, and drying at 105 ℃ for 24h to obtain a vinasse/NaOH mixture.
(2) Processing the dried mixture into blocks with proper volume (preferably, the thickness: 0.3-0.5 cm, the length and the width: 1-1.5 cm), clamping by tweezers, placing on the flame of an alcohol burner (1.5-2 cm away from a wick, and measuring at the temperature of about 400-. If the method is used for enlarging production, the alcohol lamp is only required to be replaced by a high-temperature furnace with a combustion chamber for controlling feeding and discharging.
(3) And placing the obtained precursor into a corundum crucible, placing the corundum crucible into a tube furnace, heating to 300 ℃, keeping the temperature for 1 h, continuing to heat to 850 ℃, keeping the temperature for 1 h, cooling to room temperature, taking out the corundum crucible, repeatedly cleaning with 1M HCl and deionized water until the temperature is neutral (pH-7), filtering, collecting, placing the corundum crucible in a drying oven at 105 ℃, drying for 24h, and grinding to obtain the biomass porous carbon, wherein the biomass porous carbon is marked as FPC-5.
(4) The prepared porous carbon (FPC-5) was used for Methylene Blue (MB) solution adsorption: weighing 10 mg of FPC-5 into a conical flask, respectively adding 40mL of methylene blue solution (100-700 mg/L) with different concentrations, shaking for 24h on an oscillator, and filtering and adsorbing the solution with a 0.45 mu m filter membrane; measuring absorbance of the methylene blue solution before and after adsorption at a wavelength of 664 nm by using an ultraviolet spectrophotometer, and calculating the concentration of the solution according to a standard curve (y =0.05569 x); and further calculates the adsorption capacity of FPC-5.
Comparative example 2 is provided for example 2, and comparative example 2 differs from example 2 only in that comparative example 2 lacks a combustion treatment step, i.e. the staged pyrolysis is carried out directly after pretreatment to produce a distillers' grains/KOH mixture.
Example 3
(1) Using the same starting materials as in example 1, 30 g were weighed into a beaker according to K2CO3: weighing KOH and the vinasse according to the weight ratio of vinasse =1:7, mixing the KOH and the vinasse, adding 200 mL of deionized water, stirring uniformly, standing at room temperature for 24h, then putting into a drying oven, and drying at 105 ℃ for 24h to obtain vinasse/K2CO3Mixing;
(2) processing the dried mixture into blocks with proper volume (preferably, the thickness: 0.3-0.5 cm, the length and the width: 1-1.5 cm), clamping the blocks by using tweezers, placing the blocks on the flame of an alcohol burner (at a distance of 1.5-2 cm from a wick, and measuring the temperature to be about 400-;
(3) and placing the obtained precursor into a corundum crucible, placing the corundum crucible into a tube furnace, heating to 300 ℃, keeping the temperature for 1 h, continuing to heat to 850 ℃, keeping the temperature for 1 h, cooling to room temperature, taking out the corundum crucible, repeatedly cleaning with 1M HCl and deionized water until the temperature is neutral (pH-7), filtering, collecting, placing the corundum crucible in a drying oven at 105 ℃, drying for 24h, and grinding to obtain the biomass porous carbon, wherein the biomass porous carbon is marked as FPC-7.
(4) The obtained porous carbon (FPC-7) was used for Methylene Blue (MB) solution adsorption: weighing 10 mg of FPC-7 into a conical flask, respectively adding 40mL of methylene blue solution (100-700 mg/L) with different concentrations, shaking for 24h on an oscillator, and filtering and adsorbing the solution with a 0.45 mu m filter membrane; measuring absorbance of the methylene blue solution before and after adsorption at a wavelength of 664 nm by using an ultraviolet spectrophotometer, and calculating the concentration of the solution according to a standard curve (y =0.05569 x); and further calculates the adsorption capacity of FPC-7.
Comparative example 3 is provided for example 3, and comparative example 3 differs from example 3 only in that comparative example 3 lacks a combustion treatment step, i.e. the staged pyrolysis is carried out directly after pretreatment to produce a distillers grains/KOH mixture.
The results of the comparison of the examples with the corresponding comparative examples are collated in the table below.
TABLE 1
| Material | Preparation conditions | Yield (%) | Specific surface area (m)2/g） | MB adsorption Capacity (mg/g) | MO adsorption Capacity (mg/g) | Remarks for note |
| FPC-3 | Pre-combustion | 15.28 | 1965 | 2276.32 | 546.97 | Example 1 |
| FPC-5 | Pre-combustion | 14.79 | 1593 | 1766.35 | / | Example 2 |
| FPC-7 | Pre-combustion | 15.84 | 1347 | 1383.95 | / | Example 3 |
| PC-3 | / | 12.49 | 1562 | 1550.15 | 321.57 | Comparative example 1 |
| PC-5 | / | 13.74 | 1484 | 1274.63 | / | Comparative example 2 |
| PC-7 | / | 16.10 | 1335 | 1028.12 | / | Comparative example 3 |
It is understood from the table that the specific surface area and methylene blue adsorption capacity increase more remarkably as the amount of the basic activator used increases. The adsorption capacity of each example using the combustion treatment was greatly improved in comparison with the adsorption capacity of each comparative example not using the combustion treatment. For example: the specific surface area of the porous carbon (FPC-3) prepared in example 1 was 1965 m2The adsorption capacity of methylene blue on cationic dye can reach 2276.32 mg/g, the adsorption capacity of methyl orange on anionic dye can reach 546.97 mg/g, and the pre-combustion treatment of the step (2) is not carried out under the same conditions in the comparative example 1The specific surface area of the prepared porous carbon (PC-3) is improved by about 26 percent, the methylene blue adsorption capacity is improved by about 47 percent, and the methyl orange adsorption capacity is improved by about 70 percent.
One feature of the present invention is that the pre-combustion is performed prior to pyrolysis. The biomass can generate solid biochar, liquid bio-oil and pyrolysis gas in the pyrolysis process, wherein the generated bio-oil fills and blocks partial pores due to high viscosity, poor volatility, strong corrosivity and easy coking, so that the specific surface area is reduced. On one hand, the pre-combustion treatment can rapidly heat the biomass/alkaline activator mixture to generate a large amount of bio-oil and pyrolysis gas in a short time, partial pores are generated by gas escape and expand the mixture, and the partial pores are reserved in subsequent activation, so that the possibility that the activator can contact with the carbon bodies more fully is provided; on the other hand, in an air environment, the produced bio-oil and combustible gas can be immediately combusted and decomposed in a flame, and simultaneously more oxygen elements are introduced, so that conditions are created for forming more oxygen-containing functional groups. Therefore, the bio-oil in the preparation process of the biomass porous carbon can be reduced through the pre-combustion treatment, more oxygen is introduced, better conditions are provided for subsequent activation, and a more developed pore structure and a larger specific surface area can be generated.
Claims (9)
1. A preparation method of biomass porous carbon for water treatment is characterized by comprising the following steps:
preparing a biomass/alkaline activator mixture by a pretreatment process;
combusting the biomass/alkaline activator mixture in flame at 400-500 ℃ to obtain a black fluffy precursor;
and (2) carrying out segmented pyrolysis on the precursor in an inert gas atmosphere, wherein activation simultaneously occurs in the pyrolysis process: in the first stage, the temperature is raised to 300 ℃ at the temperature raising speed of 3-10 ℃/min and is kept for 1-3 h; in the second stage, the temperature is raised from 300 ℃ to 850 ℃ at the temperature raising speed of 2-5 ℃/min and is kept for 1-3 h;
cooling to room temperature after pyrolysis to obtain a semi-finished product, adding an excessive hydrochloric acid solution into the semi-finished product, uniformly stirring, standing for 4-6 hours, and filtering to obtain a black solid substance; repeatedly washing the black solid substance with deionized water, and filtering after each washing until the filtrate is neutral;
and drying the washed black solid matter, and grinding the black solid matter after drying to obtain the biomass porous carbon.
2. The preparation method of the biomass porous carbon for water treatment according to claim 1, wherein the pretreatment process comprises the following steps:
repeatedly washing the biomass with deionized water to remove dust and impurities, and then drying at 105 ℃;
and mixing the dried biomass with an alkaline activator, adding deionized water, fully stirring, standing at normal temperature for 24 hours, and drying at 105 ℃ for 24 hours to obtain a dried biomass/alkaline activator mixture.
3. The preparation method of the biomass porous carbon for water treatment according to claim 2, wherein the mass ratio of the alkaline activator to the biomass is 1:3 to 1: 7.
4. The preparation method of the biomass porous carbon for water treatment according to claim 1, wherein the alkaline activator is one or two or more of potassium hydroxide, potassium carbonate and sodium hydroxide.
5. The preparation method of the biomass porous carbon for water treatment according to claim 1, wherein the staged pyrolysis is performed in a tubular furnace, and inert gas is introduced into the tubular furnace at a rate of 20-60 mL/min to form an inert gas atmosphere.
6. The preparation method of the biomass porous carbon for water treatment according to claim 1, wherein the concentration of the hydrochloric acid solution is 0.1-2 mol/L.
7. The preparation method of the biomass porous carbon for water treatment according to claim 1, characterized in that a vacuum filtration device is adopted for filtration.
8. The method for preparing the biomass porous carbon for water treatment according to claim 1, wherein the biomass comprises vinasse, bagasse, pomelo peel, orange peel and coconut shell.
9. The method for preparing biomass porous carbon for water treatment according to claim 1, wherein combustion is performed in a high temperature furnace having a combustion chamber.
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