CN109160514B - Bean curd reaming method, bean curd powder preparation method, bean curd graded porous activated carbon and preparation method thereof - Google Patents
Bean curd reaming method, bean curd powder preparation method, bean curd graded porous activated carbon and preparation method thereof Download PDFInfo
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Abstract
A bean curd reaming method, a bean curd powder preparation method, bean curd graded porous activated carbon and a preparation method thereof belong to the technical field of new energy materials. A bean curd hole expanding method comprises freezing bean curd containing water until water is coagulated into ice, and preparing bean curd graded porous activated carbon. The pore structure in the bean curd matrix is reserved and expanded through the ice template process, so that in the subsequent method for preparing the bean curd multi-stage porous activated carbon, the activating agent enters pores by utilizing the capillary penetration of the bean curd pores in the soaking process. A method for preparing bean curd graded porous activated carbon comprises the steps of sequentially carrying out soaking, adsorbing and activating agent treatment and carbonization treatment on bean curd powder, preparing the porous activated carbon by a template-free method, directly taking bean curd with rich raw materials and low price as a biomass carbon source, and greatly improving the economic value of a biomass material with low additional value. In addition, the invention also relates to a preparation method of the bean curd powder and bean curd grading porous activated carbon.
Description
Technical Field
The invention relates to the technical field of new energy materials, and particularly relates to a bean curd hole expanding method, a bean curd powder preparation method, bean curd grading porous activated carbon and a preparation method thereof.
Background
With the exacerbation of energy crisis and the increasing demand for energy, the research and development of high-efficiency energy storage devices has become one of the social focuses. Electrochemical capacitor is a typical energy storage device, because it can be charged in several minutes or even several seconds, i.e. has high rate capability, and its long life, has a wide application prospect in many fields. However, the energy density of the device is low, so that the application of the device in more fields is limited, and the electrode material is used as a core component of an electrochemical capacitor device to determine the capacitance performance of the electrochemical capacitor device. The activated carbon has the advantages of high specific surface area, good conductivity, wide raw material source and the like, is widely used in the fields of water treatment, food industry decoloration, precious metal recovery and catalysis, and has increasingly prominent application in novel energy storage devices such as super capacitors, lithium ion batteries and the like in recent years. Hierarchical Porous Active Carbon (HPAC) not only has rich pore structure but also has reasonable pore structure distribution of different pore diameters, and the pore passages are mutually communicated, thereby being beneficial to the permeation of electrolyte and the rapid transmission of ions and having huge potential application value in a novel energy storage device super capacitor. Biomaterials that are inherently porous or potentially porous are of great interest due to their low cost, adjustable structure, good electronic conductivity and stability. In general, some natural biomass is pretreated and then calcined, and then activated by an activating agent, and then converted into hierarchical porous activated carbon AC. The structure and performance of the AC depends mainly on the activation process and the nature of the raw material.
The conventional method for preparing the hierarchical porous activated carbon mainly uses a polymer soft template and an oxide hard template to control the pore size distribution to obtain pore channel structures with different pore sizes, and the template method also involves the subsequent step of demoulding and is very inconvenient.
Disclosure of Invention
The invention aims to provide a bean curd hole expanding method, which can freeze water in bean curd to expand the pore structure of the bean curd by freezing and is used for preparing bean curd grading porous activated carbon.
The second purpose of the invention is to provide a method for preparing bean curd powder, which provides bean curd powder for preparing bean curd grading porous activated carbon.
The third purpose of the invention is to provide a method for preparing bean curd grading porous activated carbon, which adopts a template-free method to prepare the porous activated carbon.
The fourth purpose of the invention is to provide the bean curd graded porous activated carbon which is low in raw material cost and can be used as the electrode material of the super capacitor.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a bean curd reaming method for preparing bean curd graded porous activated carbon, which comprises the step of freezing bean curd containing water until the water is condensed into ice.
The invention provides a preparation method of bean curd powder, which comprises the following steps:
drying bean curd at room temperature, filtering to remove ice water, oven drying to constant weight, and pulverizing;
the bean curd is prepared by the bean curd reaming method.
The invention provides a preparation method of bean curd grading porous activated carbon, which comprises the following steps:
sequentially carrying out soaking, adsorbing and activating agent treatment and carbonization treatment on the bean curd powder;
the bean curd powder is prepared by the preparation method of the bean curd powder.
The invention provides a bean curd graded porous activated carbon which is prepared by the preparation method of the bean curd graded porous activated carbon.
The embodiment of the invention has the beneficial effects that:
the invention provides a bean curd reaming method which is used for preparing bean curd grading porous activated carbon. The method is characterized in that water in the bean curd is condensed into ice by freezing, a pore structure in the bean curd matrix is reserved or even expanded by a simple ice template process, and pores of the bean curd matrix are communicated, so that in a subsequent method for preparing the bean curd hierarchical porous activated carbon, an activating agent enters the pores by utilizing the capillary permeation effect of the pores of the bean curd in the soaking process, and the activating agent uniformly and fully permeates into the bean curd powder matrix so as to facilitate the subsequent carbonization and activation pore-forming processes.
According to the preparation method of the bean curd powder, the bean curd prepared by the bean curd reaming method is filtered to remove water and the ice template, is dried and ground, retains the original rich pore structure after the ice template is removed, and provides the bean curd powder with the expanded pore structure for the subsequent preparation of the bean curd grading porous activated carbon.
The invention provides a preparation method of bean curd grading porous activated carbon, which prepares the porous activated carbon by a template-free method. The dried bean curd powder after reaming treatment is sequentially subjected to soaking, adsorbing and activating agent treatment and carbonization treatment, so that the bean curd powder after reaming treatment can be used for subsequently adsorbing more activating agents and performing carbonization and activation. The invention directly takes the bean curd with rich raw materials and low price as the biomass carbon source, has low cost and greatly improves the economic value of the biomass material with low added value. In addition, the preparation method mainly relates to a one-step high-temperature treatment process combining a freezing treatment process and carbonization and activation treatment, namely, the classified porous activated carbon with a good structure is prepared by a simple three-step method of bean curd matrix pore canal expansion, room-temperature activator osmotic adsorption and carbonization. The whole process of the method does not need multi-step high-temperature treatment, does not relate to steam treatment, does not need reaming processes such as hard template removal and the like, greatly simplifies the process route, saves energy, reduces cost, has extremely strong universality, and is almost applicable to all biomasses.
The bean curd graded porous activated carbon provided by the invention utilizes the cheap bean curd graded porous activated carbon, greatly improves the economic value of the biomass material with low added value, and provides a high-performance electrode material for the super capacitor.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an X-ray diffraction pattern of bean curd grade porous activated carbon obtained by different activator treatments according to an embodiment of the present invention;
FIG. 2 is a Raman spectrum of a bean curd-classified porous activated carbon treated with different activators in accordance with an embodiment of the present invention;
FIG. 3 is SEM images of bean curd grade porous activated carbon obtained by different activating agent treatments in the embodiment of the invention;
FIG. 4 is a nitrogen adsorption/desorption curve of bean curd grade porous activated carbon obtained by different activator treatments according to the embodiment of the present invention;
FIG. 5 is a diagram illustrating pore size distribution of bean curd grade porous activated carbon obtained by different activator treatments according to an embodiment of the present invention;
FIG. 6 shows a bean curd-sized porous activated carbon treated with different activators in accordance with an embodiment of the present inventionCharge and discharge curve (IAg)-1)；
FIG. 7 is a graph showing rate performance of bean curd-graded porous activated carbon treated with different activators in accordance with examples of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The method for enlarging pores in bean curd, the method for preparing bean curd powder, the bean curd-classified porous activated carbon and the method for preparing the same according to the embodiments of the present invention will be described in detail.
The invention provides a bean curd hole expanding method which comprises the step of freezing bean curd containing water until the water is condensed into ice.
Further, in order to completely coagulate the water in the bean curd into ice and complete the hole expanding process of the bean curd matrix, the water-containing bean curd is cut into blocks with the thickness of 0.5-1 cm, and the blocks are placed in an environment with the temperature of-25 to-3 ℃ for 8-18 h for freezing.
Further, in order to prevent the water in the bean curd from evaporating, before freezing, the bean curd blocks are packaged and sealed by plastic bags and then are frozen for 8-18 hours in an environment with the temperature of-25 to-3 ℃.
The invention provides a preparation method of bean curd powder, which comprises the steps of airing and filtering ice water at normal temperature after freezing and chambering, drying to constant weight, and crushing.
Further, after the frozen bean curd is taken out, the bean curd is aired at normal temperature for 2-5 hours, ice water is filtered out, then the bean curd is placed in an oven with the temperature of 80-120 ℃ to be dried to constant weight, and the dried bean curd is crushed by a crusher and then sieved by a 60-mesh sieve to obtain fine bean curd powder. The original rich pore structure is reserved after the ice template is removed, and the bean curd powder with expanded pore structure is provided for the subsequent preparation of the bean curd graded porous activated carbon.
The invention provides a preparation method of bean curd grading porous activated carbon, which comprises the steps of sequentially carrying out soaking, adsorbing and activating agent treatment and carbonization treatment on the prepared bean curd powder.
Further, the preparation method of the bean curd graded porous activated carbon comprises the following steps of sequentially carrying out impurity removal treatment, soaking with an adsorbent activator, carbonization treatment and post-treatment on the prepared bean curd powder:
1. impurity removal treatment
Adding bean curd powder into a beaker, adding a certain amount of acid solution, stirring for 0.5-1 h at normal temperature, transferring to a reaction kettle, heating to 100-120 ℃, reacting for 0.5-1 h to remove metal ions in the paste to obtain dark yellow paste, naturally cooling, performing suction filtration, washing with distilled water for multiple times until the pH value is neutral, and drying in an oven at 80-120 ℃ to constant weight;
preferably, the acid solution is hydrochloric acid or sulfuric acid with the concentration of 0.8-1.2 mol/L, and 10-15 mL of the acid solution is added into every gram of the bean curd powder.
2. Soaking adsorbent activator treatment
Weighing a proper amount of bean curd powder and an activating agent, adding distilled water, uniformly mixing, soaking for 9-15 h, and then placing in an oven at 80-120 ℃ for drying to constant weight. The pores in the bean curd matrix are opened in the freezing process, and a large number of pores can be left in the bean curd matrix after the ice template is removed, so that the permeation of an activating agent in the soaking process is facilitated.
The mass ratio of the bean curd powder to the activating agent is 1: 1-3, wherein the ratio of the volume of the added distilled water to the total mass of the bean curd powder and the activating agent is 1: 4 to 10.
Further, the activating agent comprises NaOH and K2CO3And KNO3Any one or more of them.
3. Carbonization treatment
Putting a certain amount of bean curd powder into a tubular furnace, introducing inert gas, heating to 280-320 ℃ at the speed of 3-6 ℃/min, keeping for 0.3-0.6 h, then continuously heating to 700-900 ℃ at the speed of 3-6 ℃/min, keeping for 2-3 h, and fully carbonizing and activating.
Further, the inert gas is any one or more of nitrogen, helium and argon.
4. Post-treatment
And (3) after natural cooling, taking out the carbonized product, washing the carbonized product by using dilute sulfuric acid and distilled water in sequence to remove the residual activating agent until the pH value is neutral, and then drying the carbonized product in an oven at the temperature of 80-120 ℃ until the weight is constant to obtain the bean curd graded porous activated carbon.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment of the invention provides a bean curd reaming method, a bean curd powder preparation method, bean curd grading porous activated carbon and a preparation method thereof.
1. Reaming of bean curd
Cutting water-containing bean curd into blocks with thickness of 1cm, packaging with plastic bag, sealing, and freezing at-8 deg.C for 12 hr.
2. Preparation of bean curd powder
Taking out the bean curd subjected to freezing reaming, airing the bean curd at normal temperature for 3h, filtering out ice water, then placing the bean curd in a drying oven at 100 ℃ for drying to constant weight, crushing the dried bean curd by using a crusher, and sieving by using a 60-mesh sieve to obtain fine bean curd powder.
3. Impurity removal treatment
Weighing 5.0g of dried bean curd powder, adding into a beaker, adding 60mL of 1mol/L diluted hydrochloric acid solution, stirring for 0.5h at normal temperature, transferring into a reaction kettle, heating to 120 ℃ for reaction for 1h to obtain dark yellow paste, naturally cooling, performing suction filtration, washing with distilled water for multiple times until the pH value is neutral, and drying in an oven at 100 ℃ to constant weight.
4. Soaking adsorbent activator treatment
Weighing 2.0g of dried bean curd powder and 4.0g of NaOH, adding 25mL of distilled water, uniformly mixing, soaking for 12h, and drying in an oven at 100 ℃ to constant weight.
5. Carbonization treatment
Putting a certain amount of bean curd powder into a tube furnace, introducing nitrogen, heating to 300 deg.C at a speed of 5 deg.C/min, maintaining for 0.5h, heating to 800 deg.C at a speed of 5 deg.C/min, and maintaining for 2h to fully carbonize and activate.
6. Post-treatment
And (3) after natural cooling, taking out the carbonized product, washing the carbonized product by using 0.1mol/L dilute sulfuric acid and distilled water in sequence to remove the residual activating agent until the pH value is neutral, and then placing the carbonized product in a 100 ℃ oven to dry the carbonized product to constant weight to obtain the bean curd graded porous activated carbon.
Example 2
The embodiment of the invention provides a bean curd reaming method, a bean curd powder preparation method, bean curd grading porous activated carbon and a preparation method thereof.
1. Reaming of bean curd
Cutting the water-containing bean curd into blocks with thickness of 0.5cm, packaging with plastic bag, sealing, and freezing at-3 deg.C for 8 hr.
2. Preparation of bean curd powder
Taking out the bean curd subjected to freezing reaming, airing the bean curd at normal temperature for 2h, filtering out ice water, then placing the bean curd in an oven at 80 ℃ for drying to constant weight, crushing the dried bean curd by using a crusher, and sieving by using a 60-mesh sieve to obtain fine bean curd powder.
3. Impurity removal treatment
Weighing 5.0g of dried bean curd powder, adding into a beaker, adding 50mL of 0.8mol/L dilute sulfuric acid solution, stirring for 1h at normal temperature, transferring into a reaction kettle, heating to 120 ℃, reacting for 0.5h to obtain dark yellow paste, naturally cooling, performing suction filtration, washing with distilled water for multiple times until the pH value is neutral, and drying in an oven at 80 ℃ to constant weight.
4. Soaking adsorbent activator treatment
Weighing 2.0g dried bean curd powder and 2.0g 2.0g K2CO3Adding 16mL of distilled water, uniformly mixing, soaking for 9h, and drying in an oven at 80 ℃ to constant weight.
5. Carbonization treatment
Putting a certain amount of bean curd powder in a tubular furnace, introducing helium, heating to 280 deg.C at 3 deg.C/min, maintaining for 0.3 hr, heating to 700 deg.C at 3 deg.C/min, maintaining for 2.5 hr, and carbonizing and activating.
6. Post-treatment
And (3) after natural cooling, taking out the carbonized product, washing the carbonized product by using 0.05mol/L dilute sulfuric acid and distilled water in sequence to remove the residual activating agent until the pH value is neutral, and then placing the carbonized product in an oven at 80 ℃ to dry the carbonized product until the weight is constant, thus obtaining the bean curd graded porous activated carbon.
Example 3
The embodiment of the invention provides a bean curd reaming method, a bean curd powder preparation method, bean curd grading porous activated carbon and a preparation method thereof.
1. Reaming of bean curd
Cutting the water-containing bean curd into blocks with thickness of 1cm, packaging with plastic bag, sealing, and freezing at-25 deg.C for 18 hr.
2. Preparation of bean curd powder
Taking out the bean curd subjected to freezing and reaming, airing the bean curd at normal temperature for 5h, filtering out ice water, then placing the bean curd in a 120 ℃ oven for drying until the weight is constant, crushing the dried bean curd by using a crusher, and sieving by using a 60-mesh sieve to obtain fine bean curd powder.
3. Impurity removal treatment
Weighing 5.0g of dried bean curd powder, adding into a beaker, adding 75mL of 1.2mol/L dilute sulfuric acid solution, stirring for 0.5h at normal temperature, transferring into a reaction kettle, heating to 100 ℃ for reaction for 1h to obtain dark yellow paste, naturally cooling, performing suction filtration, washing with distilled water for multiple times until the pH value is neutral, and drying in an oven at 120 ℃ until the weight is constant.
4. Soaking adsorbent activator treatment
Weighing 2.0g dried bean curd powder and 6.0g KNO3And adding 80mL of distilled water, uniformly mixing, soaking for 15h, and drying in an oven at 120 ℃ to constant weight.
5. Carbonization treatment
Putting a certain amount of bean curd powder into a tubular furnace, introducing argon, heating to 320 ℃ at the speed of 6 ℃/min, keeping for 0.6h, continuing to heat to 900 ℃ at the speed of 6 ℃/min, keeping for 3h, and fully carbonizing and activating.
6. Post-treatment
And (3) after natural cooling, taking out the carbonized product, washing the carbonized product by using 0.2mol/L dilute sulfuric acid and distilled water in sequence to remove the residual activating agent until the pH value is neutral, and then placing the carbonized product in a 120 ℃ oven to dry the carbonized product until the weight is constant to obtain the bean curd graded porous activated carbon.
The X-ray diffraction pattern, Raman spectrum, SEM image, nitrogen adsorption and desorption curve, pore size distribution, and charge and discharge curve (IAg) of the bean curd-classified porous activated carbon prepared in examples 1 to 3 were measured respectively-1) And rate performance curves, as shown in fig. 1, 2, 3, 4, 5, 6 and 7; specific surface area and pore structure parameters of the bean curd-classified porous activated carbon prepared in examples 1 to 3 were measured, respectively, as shown in table 1:
TABLE 1 specific surface area and pore Structure parameters of Bean curd-classified porous activated carbon prepared in examples 1 to 3
Tofu-classified porous activated carbon obtained in example 1: referring to fig. 1, a broad peak at 25-28 ° corresponds to an amorphous carbon structure, and the broad peak near 42 ° belongs to a peak of a graphite structure, indicating that the crystallinity of the product is not complete; referring to FIG. 2, the intensity ratio I of the graphite structure to the disordered structure of Raman spectrumG/ID0.70, indicating a higher degree of order; referring to fig. 3, after NaOH activation, a large number of ravine-shaped void structures are formed on the surface of the material; referring to FIG. 4, FIG. 5 and Table 1, the results of nitrogen desorption show that the mesoporous structure is largely mesoporous, the pore size distribution is concentrated at 3.5nm, and the specific surface area is 1142.64cm2g-1(ii) a Referring to FIGS. 6 and 7, the frozen bean curd having the highest discharge time after the NaOH high-temperature activation treatment can be 1Ag-1Then reach 368 Fg-1，20Ag-1Can reach 241Fg-1The magnification retention rate was 65.49%.
Example 2 preparation of bean curd graded porous activated carbon: referring to fig. 1, a broad peak at 25-28 ° corresponds to an amorphous carbon structure, and the broad peak near 42 ° belongs to a peak of a graphite structure, indicating that the crystallinity of the product is not complete; referring to FIG. 2, the intensity ratio I of the graphite structure to the disordered structure of Raman spectrumG/ID0.62, indicating a degree of order greater than that after NaOH activationThe porous active carbon is reduced; please refer to fig. 3, through K2CO3After the activation treatment, a fine pore structure is formed on the surface of the material; referring to FIG. 4, FIG. 5 and Table 1, the results of nitrogen desorption show that there are some microporous structures and few mesoporous structures, the pore size distribution is concentrated at 1.8nm, and the specific surface area is 1298.95cm2g-1(ii) a Please refer to fig. 6 and 7, K2CO3The frozen bean curd has long discharge time after high temperature activation treatment, and can be in 1Ag-1When reaching 383.3Fg-1，20Ag-1Can reach 119Fg-1。
Example 3 preparation of bean curd graded porous activated carbon: referring to fig. 1, a broad peak at 25-28 ° corresponds to an amorphous carbon structure, and the broad peak near 42 ° belongs to a peak of a graphite structure, indicating that the crystallinity of the product is not complete; referring to FIG. 2, the intensity ratio I of the graphite structure to the disordered structure of Raman spectrumG/ID0.58, indicating a significant reduction in the degree of order compared to the other activators; please refer to fig. 3, via KNO3After the activation treatment, a fine pore structure is formed on the surface of the material; referring to FIG. 4, FIG. 5 and Table 1, the results of nitrogen desorption show that the structure of a large number of micropores and a part of mesopores are formed, the pore size distribution is concentrated at 1.75nm, and the specific surface area is 1626.36cm2g-1(ii) a Referring to FIGS. 6 and 7, KNO3The frozen bean curd after high temperature activation has long discharge time under low current and short discharge time under high current, and can be discharged under 1Ag-1Reach 203Fg-1，20Ag-1Can reach 35Fg-1。
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (9)
1. A preparation method of bean curd grading porous activated carbon is characterized by comprising the following steps:
sequentially carrying out soaking, adsorbing and activating agent treatment and carbonization treatment on the bean curd powder;
the soaking adsorbent activator treatment comprises: adding the bean curd powder and an activating agent into distilled water, uniformly mixing, soaking for 9-15 h, and drying;
the bean curd powder is obtained by bean curd hole expanding method, and the bean curd hole expanding method comprises the following steps: freezing the water-containing bean curd until the water content is frozen into ice; the bean curd with water condensed into ice is placed at normal temperature for airing and filtering to remove ice water, and then is dried to constant weight and crushed.
2. A method for preparing a bean curd-graded porous activated carbon as defined in claim 1, wherein in the bean curd hole expanding method, the method for freezing the water-containing bean curd comprises freezing the water-containing bean curd at-25 to-3 ℃ for 8 to 18 hours.
3. A method for preparing a bean curd-graded porous activated carbon as claimed in claim 1, wherein in the soaking adsorbent activator treatment, the mass ratio of the bean curd powder to the activator is 1: 1-3, wherein the ratio of the volume amount of the added distilled water to the total mass of the bean curd powder and the activating agent is 1: 4 to 10.
4. A method of preparing bean curd grade porous activated carbon as claimed in claim 1, wherein the activator comprises NaOH, K2CO3And KNO3Any one or more of them.
5. A method of preparing bean curd grade porous activated carbon as claimed in claim 1, wherein the carbonization treatment comprises:
under the protection of inert gas, heating the bean curd powder to 700-900 ℃, and continuously carbonizing for 2-3 h;
the bean curd powder is treated by the soaking adsorption activating agent.
6. A method for preparing a bean curd-graded porous activated carbon as set forth in claim 1, wherein before the soaking adsorbent activator treatment, a bean curd powder is subjected to impurity removal treatment including:
adding bean curd powder into an acid solution, stirring for 0.5-1 h at normal temperature, heating to 100-120 ℃, reacting for 0.5-1 h, performing suction filtration, washing with distilled water for multiple times until the pH value is neutral, and drying.
7. A method for preparing a bean curd-graded porous activated carbon as defined in claim 6, wherein the acidic solution is hydrochloric acid or sulfuric acid having a concentration of 0.8 to 1.2mol/L, and 10 to 15mL of the acidic solution is added per gram of bean curd powder.
8. A method for preparing bean curd grade porous activated carbon as claimed in claim 1, wherein after the carbonization treatment, a post-treatment is further required, the post-carbonization treatment comprising:
naturally cooling the bean curd powder to normal temperature, washing with dilute sulfuric acid and distilled water in sequence until the pH value is neutral, and drying.
9. A bean curd-classified porous activated carbon produced by the method for producing a bean curd-classified porous activated carbon according to any one of claims 1 to 8.
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