CN111334318A - Method for preparing plant-based biochar from single component through biological activation and modification - Google Patents
Method for preparing plant-based biochar from single component through biological activation and modification Download PDFInfo
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Abstract
A method for preparing plant-based biochar by using a single component through biological activation modification is characterized by comprising the following steps: the method specifically comprises the steps of taking shaddock peel, orange peel or orange peel as raw materials, sequentially carrying out raw material pretreatment, biological activation modification, filtering and washing, drying and high-temperature calcination, wherein the biological activation modification is to degrade pectin in the peel by using pectinase, degrade starch in the peel by using a-amylase or degrade protein in the peel by using acid protease. The invention effectively reserves more lignocellulose, so that the carbon yield is increased; the preparation process adopts one-time high-temperature calcination, does not use any strong acid and strong alkaline chemical reagent, does not need excessive cleaning after activation, reduces secondary pollution, and achieves the purposes of energy conservation and emission reduction; the method effectively increases the specific surface area of the biochar and obtains abundant pore structures; the charcoal prepared by the invention has excellent adsorption performance on rhodamine b.
Description
Technical Field
The invention relates to the technical field of carbon materials, in particular to a method for preparing plant-based biochar based on a single component through biological activation modification.
Background
The shaddock peel is used as part of shaddock and accounts for 44-54% of the weight of the shaddock, and mainly comprises cellulose, hemicellulose, lignin, pectin and water, and also contains a small amount of protein and water-soluble starch. The surface of the components contains a large number of active functional groups, and certain ions can be combined by means of ion exchange, chelation, complexation and the like. Therefore, the pomelo peel can be developed and utilized as a novel adsorption material, and the pomelo peel is used as a raw material for preparing the activated carbon, so that the pomelo peel is changed into valuable, and the pomelo peel adsorption material has important significance.
The biochar is a carbon-rich product formed by thermochemical reaction of biomass residues in an anoxic environment, and has wide sources and large reserves, and is a valuable green resource. At present, modification methods of biochar mainly focus on physical and chemical methods, but few biological modification methods are reported, and the existing biological modification methods mainly carry out biological activation on biomass raw materials in the aspect of degrading cellulose, hemicellulose and lignin. At present, the few reports of preparing the biochar by biological activation modification exist because the biological activation method is difficult to implement, the mechanism of biological activation is complex, and a specific way for accurately controlling biological activation modification is difficult. In view of this, a new method for preparing the plant-based biochar through biological activation modification is sought, so that the blank of the field of biological activation of the plant-based biochar prepared through activation modification in the prior art is filled, and the method has great significance.
Disclosure of Invention
The invention aims to provide a method for preparing plant-based biochar by using a single component through biological activation and modification, which can obviously improve the specific surface area and the pore structure of the biochar so as to improve the adsorption performance of the biochar.
The purpose of the invention is realized by the following technical scheme:
a method for preparing plant-based biochar by using a single component through biological activation modification is characterized by comprising the following steps: the method specifically comprises the steps of taking shaddock peel, orange peel or orange peel as raw materials, sequentially carrying out raw material pretreatment, biological activation modification, filtering and washing, drying and high-temperature calcination, wherein the biological activation modification is to degrade pectin in the peel by using pectinase, or degrade starch in the peel by using a-amylase, or degrade protein in the peel by using acid protease.
Further, the pectin in the degraded peel in the biological activation is specifically prepared by weighing pretreated peel powder and deionized water to prepare emulsion, wherein the dosage ratio of the peel powder to the deionized water is 1 g: 10-20mL, adding citric acid-sodium citrate buffer solution with pH of 5, adding pectinase, heating in water bath for enzymolysis, filtering with 200-mesh nylon net, and washing the filter residue with deionized water to neutrality.
Preferably, the pectin in the degraded peel in the biological activation is specifically prepared by weighing pretreated peel powder and deionized water to prepare emulsion, wherein the dosage ratio of the peel powder to the deionized water is 1 g: 15mL, then adding citric acid-sodium citrate buffer solution with pH being 5, adding pectinase according to the amount of 120U/g, heating and carrying out enzymolysis for 1.5h at 50 ℃ in a water bath, filtering by using a 200-mesh nylon net, and washing filter residues by using deionized water until the filter residues are neutral.
Further, the starch in the degraded peel is specifically prepared by weighing pretreated peel powder and adding water to prepare emulsion, wherein the dosage ratio of the peel powder to deionized water is 1 g: 5-15mL, then gelatinizing in a constant temperature water bath at 90 ℃ for 30-50min, and adding CaCl2Make the hydrolysate Ca2+Adjusting pH to 6.0 at concentration of 0.01mol/L, adding amylase at 80-130U/g, hydrolyzing at 58-60 deg.C for 50-120min, filtering with 200 mesh nylon net, and washing the filter residue with deionized water to neutrality.
Further, the protein in the degraded peel is obtained by weighing pretreated peel powder, adding deionized water to prepare emulsion, wherein the dosage of the peel powder and the deionized water is 1 g: 15-20ml, adjusting the pH value of the emulsion to 3.0-4.0, carrying out enzymolysis at 30 ℃, adding acid protease according to the amount of 400-500U/g, placing the mixture in a shaking table for reaction for 30-50min, filtering, cleaning filter residues, and drying for later use.
The pericarp of the shaddock peel, the orange peel and the like contains abundant components such as pectin, protein, starch and the like, and the components are combined with components such as cellulose, lignin and the like in the cell wall of the shaddock peel through covalent bonds to form a stable structure which is intertwined with each other. The inventor finds that the existence of components such as pectin, protein, starch and the like can not obtain large specific surface area and pore size development when the active component (lignocellulose) in the peel is carbonized; the method adopts a biological activation mode to degrade pectin, starch or protein in the peel, so that the structure of lignocellulose is changed, a large specific surface area is obtained during later carbonization, and rich micropore and mesopore structures are formed.
Further, the raw material pretreatment specifically comprises the steps of cleaning the peel with water, drying at 80-100 ℃ for 8-10 hours, and crushing the dried peel into 2-5 mm small sections.
Further, the filtering, washing and drying are specifically to wash the biologically activated pericarp with distilled water until no enzyme activity exists in the water, and then dry the pericarp at 80-100 ℃ to constant weight.
Further, the high-temperature calcination is to place the dried peel with constant weight into a crucible, compact and cover the crucible, seal the crucible with tin foil paper, heat the crucible to 500-700 ℃ at a heating rate of 10 ℃/min, calcine the peel at constant temperature for 60-120 min, increase the specific surface area and pore volume of the final material, then reduce the temperature to 300-350 ℃ at a speed of 12 ℃/min, keep the temperature for 30-40 min, fully volatilize volatile substances, take out the crucible and naturally cool the crucible in a room temperature environment.
Specifically, the method for preparing the plant-based biochar by using the single component through biological activation modification is characterized by comprising the following steps of:
(1) cleaning the shaddock peel with water, drying at 80-100 ℃ for 8-10h, and crushing the dried peel into 2-5 mm small sections;
(2) degrading pectin in shaddock peel: weighing shaddock peel powder dried to constant weight, and adding deionized water to prepare a material-liquid ratio of 1 g: adding 10-20ml of emulsion into citric acid-sodium citrate buffer solution with pH of 5, adding pectinase into 100-150U/g of shaddock peel powder, heating in a water bath at 50 ℃ for enzymolysis for 1-2 h, filtering with a 200-mesh nylon net, and washing filter residues with deionized water to be neutral;
(3) washing the biologically activated shaddock peel with distilled water until no enzyme activity exists in the water, and drying at 80-100 ℃ to constant weight;
(4) and putting the dried shaddock peel with constant weight into a crucible, compacting and capping, sealing by using tin foil paper, heating to 500-700 ℃ at a heating rate of 10 ℃/min, calcining at a constant temperature for 60-120 min, then reducing the temperature to 300-350 ℃ at a speed of 12 ℃/min, keeping the temperature for 30-40 min, taking out the crucible, and naturally cooling in a room-temperature environment.
The components such as pectin, protein or starch are degraded and the calcination process is not properly matched, so that the structure of lignocellulose is easily excessively damaged, surface functional groups are decomposed, the structure is easily collapsed during later carbonization, the pore-size structure is collapsed, the specific surface area is small, and the adsorption performance is poor. The invention mildly removes pectin, starch or protein in the raw materials by combining the biological activation and the specific high-temperature calcination, loosens the structure of lignocellulose, effectively reserves more lignocellulose in the activation process, ensures that the finally prepared biochar has high yield, stable structure and no collapse, obtains a large specific surface area and rich pore-diameter structures, exposes the formed functional groups, forms a large amount of adsorption active sites and has excellent adsorption performance.
The invention has the following technical effects:
the invention adopts a single component of biological activation modification to remove pectin, starch or protein contained in the peel, (1) more lignocellulose is effectively reserved, so that the carbon yield is increased; (2) the preparation process adopts one-time high-temperature calcination, does not use any strong acid and strong alkaline chemical reagent, does not need excessive cleaning after activation, reduces secondary pollution, and achieves the purposes of energy conservation and emission reduction; (3) the method effectively increases the specific surface area of the biochar and obtains abundant pore structures; (4) the charcoal prepared by the method has excellent adsorption performance on rhodamine b, and the adsorption performance reaches 356 mg/g.
Detailed Description
The present invention is described in detail below by way of examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations of the present invention based on the above-mentioned disclosure.
Example 1
A method for preparing plant-based biochar by using a single component through biological activation modification comprises the following steps:
(1) cleaning the shaddock peel with water, drying at 90 ℃ for 9 hours, and crushing the dried peel into 4mm small sections;
(2) weighing shaddock peel powder dried to constant weight, and adding deionized water to prepare a material-liquid ratio of 1 g: adding 15ml of emulsion into citric acid-sodium citrate buffer solution with pH of 5, adding pectase into 120U/g (pectase/pomelo peel powder), heating in water bath at 50 deg.C for enzymolysis for 1.5 hr, filtering with 200 mesh nylon net, and washing the residue with deionized water to neutrality;
(3) washing the biologically activated shaddock peel with distilled water until no enzyme activity exists in the water, and drying at 100 ℃ to constant weight;
(4) placing dried shaddock peel into a crucible, compacting, capping, sealing with tin foil paper, heating to 600 deg.C at a heating rate of 10 deg.C/min, calcining at constant temperature for 90min, cooling to 320 deg.C at a temperature of 12 deg.C/min, maintaining the temperature for 35min, and taking out the crucible and naturally cooling at room temperature.
In the embodiment, pectin components in the shaddock peel are degraded through biological activation modification, and finally, the prepared charcoal through calcination has a large specific surface area and rich micropore and mesopore structures.
Example 2
A method for preparing plant-based biochar by using a single component through biological activation modification comprises the following steps:
(1) cleaning the shaddock peel with water, drying at 80 ℃ for 10 hours, and crushing the dried peel into 5mm small sections;
(2) accurately weighing pomelo peel powder, adding water to prepare 1 g: gelatinizing 10ml of the emulsion in a water bath with constant temperature of 90 ℃ for 30min, and adding CaCl2Make the hydrolysate Ca2+The concentration was 0.01mol/L, pH was adjusted to 6.0 with HCl, amylase was added at 120u/g (amylase/grapefruit peel powder), and hydrolysis was carried out at 59 ℃ for 40 min. Filtering with 200 mesh nylon net, washing the filter residue with deionized water to neutrality.
(3) Washing the biologically activated shaddock peel with distilled water until no enzyme activity exists in the water, and drying at 80 ℃ to constant weight;
(4) placing dried shaddock peel into a crucible, compacting, capping, sealing with tin foil paper, heating to 700 deg.C at a heating rate of 10 deg.C/min, calcining at constant temperature for 60min, cooling to 350 deg.C at a temperature of 12 deg.C/min, keeping the temperature for 30min, and taking out the crucible and naturally cooling at room temperature.
In the embodiment, starch components in shaddock peel are removed through biological activation modification, and finally, the prepared charcoal through calcination has a larger specific surface area and a rich microporous structure.
Example 3
A method for preparing plant-based biochar by using a single component through biological activation modification comprises the following steps:
(1) cleaning the shaddock peel with water, drying at 100 ℃ for 8 hours, and crushing the dried peel into 2mm small sections;
(2) accurately weighing pomelo peel powder according to the material-liquid ratio of 1 g: adding 20mL of deionized water, adjusting pH to 3.5 with HCl, adjusting enzymolysis temperature to 30 ℃, adding protease at 450u/g (protease/pomelo peel powder), and reacting in a shaker for 40 min. Filtering with 200 mesh nylon net, washing the filter residue with deionized water to neutrality.
(3) Washing the biologically activated shaddock peel with distilled water until no enzyme activity exists in the water, and drying at 90 ℃ to constant weight;
(4) placing dried shaddock peel into a crucible, compacting, capping, sealing with tin foil paper, heating to 500 deg.C at a heating rate of 10 deg.C/min, calcining at constant temperature for 120min, cooling to 300 deg.C at a temperature of 12 deg.C/min, maintaining the temperature for 40min, and taking out the crucible and naturally cooling at room temperature.
In the embodiment, protein components in the shaddock peel are removed through biological activation modification, and finally, the prepared charcoal through calcination has a large specific surface area and an excellent microporous structure.
The adsorption performance of the biochar prepared in the examples 1-3 on rhodamine b is shown in table 1:
table 1:
| example 1 | Example 2 | Example 3 | |
| Specific surface area | 562m2/g | 432m2/g | 386m2/g |
| Adsorption of rhodamine b | 356mg/g | 318mg/g | 304mg/g |
Example 4
Taking shaddock peel as a raw material, adopting the steps (1) to (4) of the embodiment 1, cooling the shaddock peel, and mixing the cooled shaddock peel with KOH, wherein the mixing mass ratio is 1: 3; then high-temperature calcination is carried out, the calcination temperature is 700 ℃, the calcination time is 90min, 0.1mol/L hydrochloric acid is added after activation to wash the pH value to be 4-6, and then the washing solution is washed by distilled water until the pH value of the washing solution is 6-8.
The BET specific surface area of the biochar prepared in the example is 1070.32m2The saturated adsorption capacity to rhodamine b is 763 mg/g.
Comparative example 1
Taking shaddock peel as a raw material, sequentially carrying out the steps (1) and (4) in the embodiment 1, and then mixing the shaddock peel with KOH according to the mass ratio of 1: 3; then high-temperature calcination is carried out, the calcination temperature is 700 ℃, the calcination time is 90min, 0.1mol/L hydrochloric acid is added after activation to wash the pH value to be 4-6, and then the washing solution is washed by distilled water until the pH value of the washing solution is 6-8.
The BET specific surface area of the biochar prepared by the invention is 807.63m2The saturated adsorption capacity to rhodamine b is 534 mg/g.
From the above example 4 and comparative example 1, it can be seen that the invention adopts a pretreatment mode of biological activation modification of a single component, which is beneficial to obtaining a large specific surface area and a rich pore structure of the biochar, and effectively improves the adsorption performance of the prepared biochar.
Comparative example 2
No biological activation modification is carried out:
(1) cleaning the shaddock peel with water, drying at 80-100 ℃ for 8-10h, and crushing the dried peel into 2-5 mm small sections;
(2) filling the crushed shaddock peel into a crucible, compacting and covering, sealing by using tin foil paper, heating to 600 ℃ at the heating rate of 10 ℃/min, calcining at the constant temperature for 90min, then reducing the temperature to 350 ℃ at the speed of 12 ℃/min, keeping the temperature for 30min, taking out the crucible, and naturally cooling in a room-temperature environment.
Comparative example 3
(a) The procedure of example 1 was followed by the same procedure as in example 1 except that the pectin and starch components in the grapefruit peel were sequentially degraded according to the procedure (2) of example 1 and the procedure (2) of example 2.
(b) Starch and protein in the shaddock peel are sequentially degraded according to the step (2) of example 2 and example 3, and the rest of the steps are the same as example 2.
(c) Pectin, starch and protein in the shaddock peel were sequentially degraded according to examples 1-3, and the remaining steps were the same as in example 1.
Specific surface properties and adsorption properties to rhodamine b of comparative examples 1 and 2 are shown in table 2:
table 2:
as shown in tables 1 and 2, the adsorption performance of the charcoal is still higher than that of the charcoal without any activation means but the adsorption effect is much lower than that of the charcoal with a single activation-modified component due to the destruction of the structure of lignocellulose in the pericarp, the structure collapses to some extent during carbonization, the pore diameter of part of pores becomes large, the specific surface area becomes small, the surface functional groups formed between the degraded components and lignocellulose are decomposed during the degradation process, the types and the number of functional groups are reduced, the adsorption performance is reduced, but the degradation of the components such as pectin and starch in the pericarp, and the like, although part of the functional groups are decomposed, the structure of lignocellulose becomes loose, the pore structure is formed during the calcination process, and more functional groups are exposed on the surface, so that the final adsorption performance of the biological carbon is still better than that of the biological carbon without any activation means.
Claims (8)
1. A method for preparing plant-based biochar by using a single component through biological activation modification is characterized by comprising the following steps: the method specifically comprises the steps of taking shaddock peel, orange peel or orange peel as raw materials, sequentially carrying out raw material pretreatment, biological activation modification, filtering and washing, drying and high-temperature calcination, wherein the biological activation modification is to degrade pectin in the peel by using pectinase, or degrade starch in the peel by using a-amylase, or degrade protein in the peel by using acid protease.
2. The method for preparing plant-based biochar from the single component through biological activation modification as claimed in claim 1, wherein the single component is selected from the group consisting of: the pectin in the degraded peel in the biological activation process is specifically prepared by weighing pretreated peel powder and adding deionized water to prepare emulsion, wherein the dosage of the peel powder and the deionized water is 1 g: 10-20mL, adding citric acid-sodium citrate buffer solution with pH = 5, adding pectinase according to the amount of 100-150U/g, heating and performing enzymolysis for 1-2 h in a water bath at 50 ℃, filtering by using a 200-mesh nylon net, and washing by using deionized water until the solution is neutral.
3. The method for preparing plant-based biochar from the single component through biological activation modification as claimed in claim 1, wherein the single component is selected from the group consisting of: the starch in the degraded peel is prepared by weighing pretreated peel powder, adding water to prepare emulsion, wherein the dosage ratio of the peel powder to deionized water is 1 g: 5-15mL, then gelatinizing in a constant temperature water bath at 90 ℃ for 30-50min, and adding CaCl2Make the hydrolysate Ca2+Adjusting pH =6.0 at concentration of 0.01mol/L, adding amylase at 80-130U/g, performing hydrolysis reaction at 58-60 deg.C for 50-120min, filtering with 200 mesh nylon net, and washing the filter residue with deionized water to neutrality.
4. The method for preparing plant-based biochar from the single component through biological activation modification as claimed in claim 1, wherein the single component is selected from the group consisting of: the protein in the degraded peel is specifically that pretreated peel powder is weighed, deionized water is added to prepare emulsion, and the dosage of the peel powder and the deionized water is 1 g: 15-20ml, adjusting the pH of the emulsion to be =3.0-4.0, adjusting the enzymolysis temperature to be 30 ℃, adding acid protease according to the amount of 400-500U/g, placing the mixture in a shaking table for reaction for 30-50min, filtering, cleaning filter residues, and drying for later use.
5. The method for preparing plant-based biochar from the bioactivation modified single component as claimed in any one of claims 1 to 4, wherein: the raw material pretreatment is specifically to clean the peel with water, dry the peel for 8-10 hours at 80-100 ℃, and crush the dried peel into 2-5 mm small sections.
6. The method for preparing plant-based biochar from the bioactivation modified single component as claimed in any one of claims 1 to 5, wherein: the filtering, washing and drying are specifically to wash the biologically activated pericarp with distilled water until no enzyme activity exists in the water, and then dry the pericarp at 80-100 ℃ to constant weight.
7. The method for preparing plant-based biochar from the bioactivation modified single component as claimed in any one of claims 1 to 6, wherein: and the high-temperature calcination is to place the dried peel with constant weight into a crucible, compact and cover the peel, seal the peel with tin foil paper, heat the peel to 500-700 ℃ at a heating rate of 10 ℃/min, calcine the peel at a constant temperature for 60-120 min, then reduce the temperature to 300-350 ℃ at a speed of 12 ℃/min, keep the temperature for 30-40 min, take out the crucible and naturally cool the crucible in a room-temperature environment.
8. A method for preparing plant-based biochar by biological activation and modification of a single component is characterized by comprising the following steps:
(1) cleaning the shaddock peel with water, drying at 80-100 ℃ for 8-10h, and crushing the dried peel into 2-5 mm small sections;
(2) weighing dried shaddock peel powder and adding deionized water to prepare a feed liquid ratio of 1 g: adding 10-20ml of emulsion into a citric acid-sodium citrate buffer solution with pH = 5, adding pectinase into the pomelo peel powder according to 100-150U/g, heating in a water bath at 50 ℃ for enzymolysis for 1-2 h, filtering with a 200-mesh nylon net, and washing filter residues with deionized water to be neutral;
(3) washing the biologically activated shaddock peel filter residue with distilled water until no enzyme activity exists in the water, and drying at 80-100 ℃ to constant weight;
(4) and putting the dried shaddock peel with constant weight into a crucible, compacting and capping, sealing by using tin foil paper, heating to 500-700 ℃ at a heating rate of 10 ℃/min, calcining at a constant temperature for 60-120 min, then reducing the temperature to 300-350 ℃ at a speed of 12 ℃/min, keeping the temperature for 30-40 min, taking out the crucible, and naturally cooling in a room-temperature environment.
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| CN113512438A (en) * | 2021-06-10 | 2021-10-19 | 北京工商大学 | Preparation method of high-performance biochar |
| CN115304050A (en) * | 2022-08-12 | 2022-11-08 | 云南师范大学 | Preparation method of citrus peel biochar and application of citrus peel biochar in wastewater treatment |
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| CN115304050A (en) * | 2022-08-12 | 2022-11-08 | 云南师范大学 | Preparation method of citrus peel biochar and application of citrus peel biochar in wastewater treatment |
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| CN113713766B (en) | 2023-04-21 |
| CN113713766A (en) | 2021-11-30 |
| CN111334318B (en) | 2021-07-27 |
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