CN113213477A - Preparation method of straw activated carbon with high adsorption performance - Google Patents
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Abstract
The invention discloses a preparation method of straw activated carbon with high adsorption performance. Crushing and screening straw raw materials, and then carrying out densification pretreatment such as molding-baking to prepare straw particles; straw particles are crushed and screened into particles with proper size and part of impurity ash is removed, the particles are uniformly mixed with 55 mass percent phosphoric acid activating agent according to a certain proportion, the mixture is pre-activated for a certain time at a certain temperature by adopting a thermo-osmosis activation process, then the pre-activated particles are placed in a tubular furnace, the temperature is raised to a certain activation temperature under the protection of nitrogen for activation, the mixture is cooled to room temperature, the mixture is further washed and de-ashed by centrifugation, the pH value of the solution is neutral, and the mixture is dried to obtain the low-ash high-specific-gravity high-adsorbability straw activated carbon, wherein the yield is 47.24%, the ash content is 4.12%, the specific gravity is 0.313g/mL, the iodine adsorption value is 872mg/g, the methylene blue adsorption value is 210mg/g, and the caramel decolorization rate is 100%.
Description
Technical Field
The invention belongs to the technical field of high-value utilization of straw resources, and particularly relates to a preparation method of low-ash high-specific-gravity high-adsorption-performance straw activated carbon.
Background
The straw resources of villages and towns in China are rich, wherein the crop straws and the agricultural product processing residues account for more than 50% of the total amount of biomass resources in China, but the utilization efficiency is extremely low. As an important agricultural waste, the conventional treatment mode is mostly straw returning, burning or stacking and the like, the utilization efficiency is low, the utilization benefit is poor, and the environmental pollution is easily caused. The straw can be recycled and utilized in a material mode, so that waste can be turned into wealth, the problems of resource waste and environmental pollution are reduced, and the efficient and comprehensive utilization of straw resources is promoted.
The active carbon has huge specific surface area, abundant pore structures and good adsorption performance, is an environment-friendly adsorption and purification material, has wide application in various fields such as environmental protection, pollution control, energy storage, national defense and the like, plays an important role, and is an indispensable product of national economy.
The active carbon is prepared by taking the straws as the raw material, and a new idea is provided for high-value utilization of straw resources. However, due to the characteristics of loose straw tissue structure, high ash content, low carbon content and the like, the prepared activated carbon has high ash content, low specific gravity and poor adsorption performance, and the development and application of the straw activated carbon are seriously influenced. Therefore, the research on the preparation method of the straw activated carbon with low ash content, high specific gravity and high adsorption performance has great significance for high-valued and comprehensive utilization of the straw.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide a preparation method of high-performance straw activated carbon. The straw structure is densified through the forming-baking treatment, the specific gravity of the straw activated carbon is further improved, the ash content of the straw activated carbon is reduced through the raw material screening treatment and the subsequent centrifugal washing deashing treatment, and the adsorption performance of the straw activated carbon is improved through the hot infiltration activation process. The straw activated carbon with low ash content, high specific gravity and high performance is prepared by combining the processes, and the preparation method is simple, the process is easy to implement industrially, and the straw activated carbon has a good industrial application prospect.
The technical scheme of the invention is as follows: a preparation method of straw activated carbon with high adsorption performance comprises the following steps:
1) crushing and screening straw raw materials, and then carrying out densification pretreatment such as molding-baking to prepare straw particles;
2) crushing and screening straw particles into proper particle size and removing part of ash impurities;
3) uniformly mixing the crushed straw particles obtained in the step 2) with a phosphoric acid activator, and performing hot infiltration preactivation at a certain temperature;
4) placing the mixture obtained in the step 3) in a tubular furnace, heating and activating under the protection of nitrogen, and cooling to obtain an activated material;
5) and (4) centrifugally washing and deashing the activated material, washing with water until the pH of the solution is neutral, and drying to obtain the activated carbon.
The temperature of the molding-baking pretreatment in the step 1) is 210-270 ℃, and the time is 30-60 min.
The mass ratio of the straw particles to the phosphoric acid activator in the step 3) is 1: 1-5.
And 3) pre-activating at 120-180 ℃ for 30-90 min.
And 4) activating at 350-550 ℃ for 30-120 min.
And 5) the solution used for centrifugal washing and deashing is wood vinegar, and the pH value is 2.0-3.5.
The mass ratio of the activated material to the wood vinegar liquid in the step 5) is 1: 10-20, and the washing temperature is 40-80 ℃.
The preparation method is combined use of technologies such as densification pretreatment, thermal infiltration activation, centrifugal washing and deashing, and the like, and the straw activated carbon with low ash content, high specific gravity and high performance is prepared.
Has the advantages that:
the preparation method of the straw activated carbon is simple, the process is easy to implement industrially, and the problems of high ash content, small specific gravity, poor performance and the like of the traditional straw activated carbon preparation method can be effectively solved. The straw activated carbon has the advantages that the straw structure is densified through forming and subsequent baking treatment, the specific weight of the straw activated carbon is further improved, the ash content of the straw activated carbon is reduced through raw material screening treatment and subsequent centrifugal washing deashing treatment, the adsorption performance of the straw activated carbon is improved through a hot infiltration preactivation process, the straw activated carbon with low ash content, high specific gravity and high performance is prepared through the process combination, the performance index of the straw activated carbon is close to that of wood activated carbon, the straw activated carbon can be used in the fields of heavy metal adsorption, water pollution treatment and the like, and the straw activated carbon is beneficial to high-value utilization of the straw.
Drawings
FIG. 1 is a process scheme of the present invention.
Detailed Description
A preparation method of straw activated carbon with high adsorption performance comprises the following steps:
1) crushing and screening straw raw materials, and then carrying out densification pretreatment such as molding and baking to prepare straw particles;
2) crushing and screening straw particles into proper particle size and removing part of ash impurities;
3) uniformly mixing the crushed straw particles obtained in the step 2) with a phosphoric acid activator, and performing hot infiltration preactivation at a certain temperature;
4) placing the mixture obtained in the step 3) in a tubular furnace, heating and activating under the protection of nitrogen, and cooling to obtain an activated material;
5) and centrifugally washing and deashing the activated material, washing with water until the pH value of the solution is neutral, and drying to obtain the activated carbon.
The temperature of the molding-baking pretreatment in the step 1) is 210-270 ℃, and the time is 30-60 min.
The mass ratio of the straw particles to the phosphoric acid activator in the step 3) is 1: 1-1: 5.
And 3) pre-activating at 120-180 ℃ for 30-90 min.
And 4) activating at 350-550 ℃ for 30-120 min.
And 5) the solution used for centrifugal washing and deashing is wood vinegar, and the pH value is 2.0-3.5.
The mass ratio of the activated material to the wood vinegar liquid in the step 5) is 1: 10-1: 20, and the washing temperature is 40-80 ℃.
The preparation method is combined use of technologies such as molding-baking densification pretreatment, thermal infiltration activation, centrifugal washing deashing and the like, and the straw activated carbon with low ash content, high specific gravity and high adsorption performance is prepared.
Example 1:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 30min at 210 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:3, placing the mixture in a tubular furnace for preactivation at 120 ℃ for 30min, then heating to 400 ℃ at the heating rate of 10 ℃/min for activation for 60min to obtain an activated material, and cooling to room temperature. Adding the activated material into wood vinegar liquid with pH of 2.57 according to the mass ratio of 1:10, stirring and washing for 60min at 80 ℃, then centrifugally dewatering, further washing by using distilled water until the pH of the solution is neutral, and drying at 105 ℃ to obtain the straw activated carbon, wherein the ash content is 4.67%, the specific gravity is 0.327g/mL, the iodine adsorption value is 836mg/g, the methylene blue adsorption value is 187.5mg/g, and the caramel decolorization rate is 70%.
Example 2:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 30min at 240 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, placing the mixture in a tubular furnace for preactivation at 140 ℃ for 60min, then heating the mixture to 400 ℃ at the heating rate of 10 ℃/min for activation for 60min to obtain an activated material, and cooling the activated material to room temperature. Adding the activated material into wood vinegar with pH of 2.21 according to the mass ratio of 1:20, stirring and washing for 60min at 80 ℃, then centrifugally dewatering, further washing by using distilled water until the pH of the solution is neutral, and drying at 105 ℃ to obtain the straw activated carbon, wherein the ash content is 4.12%, the specific gravity is 0.313g/mL, the iodine adsorption value is 872mg/g, the methylene blue adsorption value is 210mg/g, and the caramel decolorization rate is 100%.
Example 3:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 60min at 240 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:5, placing the mixture in a tubular furnace for preactivation at 120 ℃ for 90min, heating the mixture to 350 ℃ at the heating rate of 10 ℃/min for activation for 30min to obtain an activated material, and cooling the activated material to room temperature. Adding the activated material into wood vinegar liquid with pH of 2.57 according to the mass ratio of 1:15, stirring and washing for 60min at 40 ℃, then centrifugally dewatering, further washing by using distilled water until the pH of the solution is neutral, and drying at 105 ℃ to obtain the straw activated carbon, wherein the ash content is 5.04%, the specific gravity is 0.336g/mL, the iodine adsorption value is 757mg/g, the methylene blue adsorption value is 172.5mg/g, and the caramel decolorization rate is 70%.
Example 4:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 30min at 270 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:3, placing the mixture in a tubular furnace for preactivation at 140 ℃ for 60min, then heating the mixture to 450 ℃ at the heating rate of 10 ℃/min for activation for 60min to obtain an activated material, and cooling the activated material to room temperature. Adding the activated material into wood vinegar with pH of 2.21 according to the mass ratio of 1:20, stirring and washing for 60min at 80 ℃, then centrifugally dewatering, further washing by using distilled water until the pH of the solution is neutral, and drying at 105 ℃ to obtain the straw activated carbon, wherein the ash content is 4.32%, the specific gravity is 0.319g/mL, the iodine adsorption value is 827mg/g, the methylene blue adsorption value is 187.5mg/g, and the caramel decolorization rate is 80%.
Example 5:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 60min at 210 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, placing the mixture in a tubular furnace for preactivation at 140 ℃ for 90min, then heating the mixture to 550 ℃ at the heating rate of 10 ℃/min for activation for 60min to obtain an activated material, and cooling the activated material to room temperature. Adding the activated material into wood vinegar liquid with the pH value of 2.21 according to the mass ratio of 1:10, stirring and washing for 60min at the temperature of 60 ℃, then centrifugally dewatering, further washing by using distilled water until the pH value of the solution is neutral, and drying at the temperature of 105 ℃ to obtain the straw activated carbon, wherein the ash content is 5.11%, the specific gravity is 0.339g/mL, the iodine adsorption value is 781mg/g, the methylene blue adsorption value is 180mg/g, and the caramel decolorization rate is 60%.
Example 6:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 60min at 240 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, placing the mixture in a tubular furnace for preactivation at 140 ℃ for 60min, then heating to 400 ℃ at the heating rate of 10 ℃/min for activation for 90min to obtain an activated material, and cooling to room temperature. Adding the activated material into wood vinegar liquid with pH of 2.21 according to the mass ratio of 1:20, stirring and washing for 60min at 80 ℃, then centrifugally dewatering, further washing by using distilled water until the pH of the solution is neutral, and drying at 105 ℃ to obtain the straw activated carbon, wherein the ash content is 4.17%, the specific gravity is 0.320g/mL, the iodine adsorption value is 858mg/g, the methylene blue adsorption value is 202.5mg/g, and the caramel decolorization rate is 100%.
Example 7:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 60min at 240 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, placing the mixture in a tubular furnace for pre-activation at 180 ℃ for 60min, then heating the mixture to 450 ℃ at the heating rate of 10 ℃/min for activation for 90min to obtain an activated material, and cooling the activated material to room temperature. Adding the activated material into wood vinegar with pH of 2.57 according to the mass ratio of 1:20, stirring and washing for 60min at 80 ℃, then centrifugally dewatering, further washing by using distilled water until the pH of the solution is neutral, and drying at 105 ℃ to obtain the straw activated carbon, wherein the ash content is 4.58%, the specific gravity is 0.325g/mL, the iodine adsorption value is 824mg/g, the methylene blue adsorption value is 195mg/g, and the caramel decolorization rate is 90%.
The activation conditions (activation temperature of 400 ℃ and activation time of 60min) of example 2 are selected, and compared with the influences of the processes such as forming-baking pretreatment, heat penetration activation, centrifugal washing and the like on the preparation and performance of the straw activated carbon, the results are as follows:
comparative example 1:
crushing and screening straw raw materials into 1-2 mm, uniformly mixing the straw raw materials with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, placing the straw raw materials in a tubular furnace for preactivation at 140 ℃ for 60min, then heating to 400 ℃ at the heating rate of 10 ℃/min for activation for 60min to obtain an activated material, and cooling to room temperature. Adding the activated material into wood vinegar liquid with the pH value of 2.21 according to the mass ratio of 1:20, stirring and washing for 60min at 80 ℃, then centrifugally dewatering, further washing by using distilled water until the pH value of the solution is neutral, drying at 105 ℃ to obtain the straw activated carbon, wherein the ash content is 6.74%, the specific gravity is 0.197g/mL, the iodine adsorption value is 812mg/g, the methylene blue adsorption value is 187.5mg/g, and the caramel decolorization rate is 90%.
Comparative example 2:
crushing and screening straw raw materials into 1-2 mm, uniformly mixing the straw raw materials with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, placing the straw raw materials in a tubular furnace for preactivation at 140 ℃ for 60min, then heating to 400 ℃ at the heating rate of 10 ℃/min for activation for 60min to obtain an activated material, and cooling to room temperature. The activated material is washed by distilled water until the pH value of the solution is neutral, and the activated material is straw activated carbon after being dried at 105 ℃, wherein the ash content is 8.78 percent, the specific gravity is 0.194g/mL, the iodine adsorption value is 793mg/g, the methylene blue adsorption value is 180mg/g, and the caramel decolorization rate is 80 percent.
Comparative example 3:
crushing and screening straw raw materials into 1-2 mm, uniformly mixing the straw raw materials with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:5, putting the mixture into a tubular furnace, heating the mixture to 400 ℃ at the heating speed of 10 ℃/min, activating the mixture for 90min to obtain an activated material, and cooling the activated material to room temperature. The activated material is washed by distilled water until the pH value of the solution is neutral, and the activated material is straw activated carbon after being dried at 105 ℃, wherein the ash content is 8.85 percent, the specific gravity is 0.203g/mL, the iodine adsorption value is 724mg/g, the methylene blue adsorption value is 172.5mg/g, and the caramel decolorization rate is 70 percent.
Comparative example 4:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 30min at 240 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, placing the mixture in a tubular furnace for preactivation at 140 ℃ for 60min, then heating the mixture to 400 ℃ at the heating rate of 10 ℃/min for activation for 60min to obtain an activated material, and cooling the activated material to room temperature. The activated material is washed by distilled water until the pH value of the solution is neutral, and the activated material is straw activated carbon after being dried at 105 ℃, wherein the ash content is 6.12 percent, the specific gravity is 0.310g/mL, the iodine adsorption value is 806mg/g, the methylene blue adsorption value is 195mg/g, and the caramel decolorization rate is 80 percent.
Comparative example 5:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 30min at 240 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, putting the mixture into a tubular furnace, heating the mixture to 400 ℃ at the heating speed of 10 ℃/min, activating the mixture for 60min to obtain an activated material, and cooling the activated material to room temperature. Adding the activated material into wood vinegar with pH of 2.21 according to the mass ratio of 1:20, stirring and washing for 60min at 80 ℃, then centrifugally dewatering, further washing by using distilled water until the pH of the solution is neutral, and drying at 105 ℃ to obtain the straw activated carbon with ash content of 5.32%, specific gravity of 0.287g/mL, iodine adsorption value of 791mg/g, methylene blue adsorption value of 180mg/g and caramel decolorization rate of 80%.
Comparative example 6:
crushing and screening straw raw materials, molding by adopting a flat die machine, and baking for 30min at 240 ℃ to prepare straw particles; crushing and screening straw particles into 1-2 mm, uniformly mixing the straw particles with a phosphoric acid solution with the mass fraction of 55% according to the mass ratio of 1:4, putting the mixture into a tubular furnace, heating the mixture to 400 ℃ at the heating speed of 10 ℃/min, activating the mixture for 60min to obtain an activated material, and cooling the activated material to room temperature. The activated material is washed by distilled water until the pH value of the solution is neutral, and the activated material is straw activated carbon after being dried at 105 ℃, wherein the ash content is 6.18 percent, the specific gravity is 0.313g/mL, the iodine adsorption value is 772mg/g, the methylene blue adsorption value is 180mg/g, and the caramel decolorization rate is 70 percent.
By comprehensively analyzing the results of the example 2 and the comparative examples 1 to 6, it can be seen that the ash content of the straw activated carbon can be remarkably reduced and the specific gravity and the adsorption performance of the straw activated carbon can be improved through the combined processes of the forming-baking pretreatment, the thermal infiltration activation, the centrifugal washing and the like.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A preparation method of straw activated carbon with high adsorption performance is characterized by comprising the following steps:
1) crushing and screening straw raw materials, and then carrying out molding-baking densification pretreatment to obtain straw particles;
2) crushing and screening straw particles into proper particle size and removing part of impurity ash;
3) uniformly mixing the crushed straw particles obtained in the step 2) with a phosphoric acid activator, and performing hot infiltration preactivation at a certain temperature;
4) placing the mixture obtained in the step 3) in a tubular furnace, heating and activating under the protection of nitrogen, and cooling to obtain an activated material;
5) and (4) centrifugally washing and deashing the activated material, washing with water until the pH of the solution is neutral, and drying to obtain the activated carbon.
2. The preparation method of the straw activated carbon with high adsorption performance according to claim 1, wherein the temperature of the molding-baking pretreatment in the step 1) is 210-270 ℃ and the time is 30-60 min.
3. The preparation method of the straw activated carbon with high adsorption performance according to claim 1, wherein the mass ratio of the straw particles to the phosphoric acid activator in the step 3) is 1: 1-5, and the mass percentage concentration of phosphoric acid is 55%.
4. The preparation method of the straw activated carbon with high adsorption performance according to claim 1, wherein the preactivation temperature in the step 3) is 120-180 ℃, and the preactivation time is 30-90 min.
5. The preparation method of the straw activated carbon with high adsorption performance according to claim 1, wherein the activation temperature in the step 4) is 350-550 ℃, and the activation time is 30-120 min.
6. The preparation method of straw activated carbon with high adsorption performance according to claim 1, wherein the solution used in the centrifugal washing and deashing in the step 5) is wood vinegar, and the pH value is 2.0-3.5.
7. The preparation method of the straw activated carbon with high adsorption performance according to claim 1, wherein the mass ratio of the activated material to the wood vinegar in the step 5) is 1: 10-20, and the washing temperature is 40-80 ℃.
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