CN110743498A - Preparation method of edible fungus residue biochar - Google Patents
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Abstract
A preparation method of edible fungus dreg biochar is characterized by comprising the following steps: drying, crushing and sieving edible fungus residues, uniformly mixing the edible fungus residues with a zinc chloride solution, standing for 30-40 min, then centrifugally separating out the fungus residues, adding the fungus residues into a catalyst aqueous solution, carrying out hydrothermal carbonization after magnetic stirring, and then centrifuging, washing and drying; the catalyst aqueous solution is formed by mixing 80-95% of sulfuric acid and 60-85% of phosphoric acid in mass concentration with water according to a volume ratio of 1-2: 5-8: 20-40. The preparation method of the edible fungus dreg biochar based on the hydrothermal method can realize large specific surface area, and the BET specific surface area reaches 962m2The porosity is high, the pore size distribution is uniform, the stability is good, and the yield is high; has excellent adsorption performance to heavy metal ions, and the removal rate of the heavy metal ions can reach 20 times after the heavy metal ions are repeatedly utilized82.4% of the initial use.
Description
Technical Field
The invention relates to the technical field of carbon materials, in particular to a preparation method of edible fungus dreg hydrothermal biochar.
Background
Biochar is a carbon material with extremely high carbon content formed by pyrolysis and carbonization of biomass (crop waste, wood, plant tissues, animal bones and the like) under the anoxic condition. The activated carbon has an amorphous structure based on graphite microcrystals, has large specific surface area and porosity, and has strong adsorption force, antimicrobial decomposition capability and oxidation resistance, so that the field of adsorption and environmental remediation of biological carbon pollutants has strong application potential. Researches show that the biochar can effectively realize the adsorption of heavy metal ions and cyanide-containing wastewater in the wastewater, and is widely applied to special fields of blood purification, natural gas storage, military chemical protection, nuclear industry radioactive element adsorption, catalysts, catalyst carriers and the like, and shows excellent adsorption activity. Meanwhile, the biochar is an environment-friendly material with low cost and high efficiency, and is beneficial to industrial production. However, the source and composition of the raw materials of the biochar are very different, and the types and the number of the surface functional groups are limited, so that the application of the biochar in the aspect of polluted environment restoration is greatly limited. The biomass raw material containing more mineral substances and the higher pyrolysis temperature usually destroy the structure of functional groups on the surface of the biochar and reduce the types and the number of active functional groups on the surface of the biochar, thereby being not beneficial to the adsorption of pollutants, and especially reducing the adsorption performance of heavy metal ions. Edible fungi are an important food source for human beings. But a large amount of mushroom dregs are discarded as agricultural garbage, which causes serious water and soil pollution. At present, the mushroom dregs are used for fermenting to produce the organic fertilizer, and although the operation is simple, the problems of slow fermentation, low fertility, propagation of various diseases and the like exist. In the prior art, the bacterial residues are also used for preparing the biochar, but the problems of complex synthesis method, high energy consumption, low product adsorption performance and the like exist.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of edible fungus residue biochar based on a hydrothermal method, which is simple in process and mild and controllable in reaction conditions.
The purpose of the invention is realized by the following technical scheme:
a preparation method of edible fungus dreg biochar is characterized by comprising the following steps: drying, crushing and sieving edible fungus residues, uniformly mixing the edible fungus residues with a zinc chloride solution, standing for 30-40 min, then centrifugally separating out fungus residues, adding the fungus residues into a mixed catalyst aqueous solution, carrying out hydrothermal carbonization after magnetic stirring, and then centrifuging, washing and drying; the catalyst aqueous solution is formed by mixing 80-95% of sulfuric acid, 60-85% of phosphoric acid and water according to a volume ratio of 1-2: 5-8: 20-40.
Further, the drying is carried out for 2-4 h at the temperature of 100 ℃ in a blast drying oven, the crushing is carried out for 0.5-1 min at 25000 r/min on the dried edible fungus dregs, and the crushed edible fungus dregs are sieved by a sieve of 40-80 meshes.
Furthermore, the mass volume ratio of the edible fungus residues to the zinc chloride aqueous solution is 1g: 10-50 mL, and the mass concentration of the zinc chloride is 5% -10%.
The zinc chloride has an expansion effect on cellulose in the fungus residues, and is used for standing after the fungus residues are mixed with a zinc chloride aqueous solution, so that the zinc chloride fully enters the fungus residues, primary pore forming is performed on dissolved cellulose, and meanwhile, the zinc chloride provides conditions for rapid permeation of a subsequent mixed catalyst due to the expansion effect on the cellulose.
Further, the mass volume ratio of the edible fungus residues subjected to centrifugal separation to the catalyst aqueous solution is 1: 10-40, the stirring speed of the intensive stirring is 1000-1500 rpm, and the stirring time is 0.5-1 h.
The phosphoric acid has weak expansion effect on cellulose in the edible fungus residues, and the phosphoric acid is difficult to permeate into the edible fungus residues for action due to the existence of lignin. The small amount of sulfuric acid is used for promoting the permeation of phosphoric acid on raw materials, and simultaneously, the phosphoric acid and the lignocellulose are hydrolyzed cooperatively, so that the lignocellulose is hydrolyzed into low relative molecular polysaccharides and monosaccharides, graphite microcrystals with large topological structures are formed, and the types and the number of functional groups on the surface of the prepared biochar are increased.
Further, the hydrothermal carbonization is to mix edible fungus residues and a mixed catalyst aqueous solution, magnetically stir the mixture, transfer the mixture to a high-pressure reaction kettle, seal the mixture, raise the temperature to 50-60 ℃ at a speed of 1-2 ℃/min, keep the temperature for 1 hour, then raise the temperature to 180-250 ℃ at a temperature rise speed of 3-5 ℃/min, and react for 2-4 hours.
In the preparation process, the catalyst has poor dispersibility in the edible fungus residues, so that the prepared biochar has undeveloped pores and uneven pore size distribution, and the adsorption performance of the biochar is influenced finally. The inventors found that phosphoric acid reacts with lignin at 50 to 60 ℃ in the temperature rise process to change the structure of lignin and promote hydrolysis. In the hydrothermal carbonization process, the heating is divided into two stages, the heating and heat preservation are carried out in the first stage, so that the phosphoric acid and the lignin are reacted, the structure of the lignin is damaged, the phosphoric acid and the sulfuric acid can quickly permeate into the edible fungus residues, the carbonization temperature is increased at a specific speed in the second stage, the phosphoric acid and the zinc chloride are quickly and uniformly diffused to form a framework, and finally prepared active carbon is developed in aperture and uniform in aperture distribution.
Further, after the hydrothermal carbonization is finished, naturally cooling to room temperature, centrifuging for 5-10 min at 5000-8000 rpm, collecting precipitates, sequentially washing with distilled water and ethanol, and drying at 40-60 ℃ for 4-8 h to obtain the edible fungus residue based hydrothermal biochar.
Specifically, the preparation method of the edible fungus dreg biochar comprises the following steps:
(1) taking edible fungus residue waste, and drying in a forced air drying oven at 100 ℃; crushing the dried edible fungus residues at 25000 r/min for 0.5-1 min, and sieving with a 40-80 mesh sieve to obtain edible fungus residue powder;
(2) adding the sieved edible fungus residue powder into a zinc chloride aqueous solution with the mass concentration of 5-10%, uniformly stirring, and standing for 30-40 min, wherein the mass-volume ratio of the edible fungus residue powder to the zinc chloride is 1g: 10-50 mL;
(3) centrifuging and filtering the edible fungus residues treated in the step (2), adding the edible fungus residues into a mixed catalyst aqueous solution, and stirring for 0.5-1 h at 1000-1500 rpm, wherein the mixed catalyst is prepared from sulfuric acid, phosphoric acid and water, and the volume ratio of the sulfuric acid to the phosphoric acid to the water is 1-2: 5-8: 20-40;
(4) mixing the edible fungus residues and the mixed catalyst aqueous solution, magnetically stirring, transferring to a high-pressure reaction kettle, sealing, raising the temperature to 50-60 ℃ at the speed of 1-2 ℃/min, preserving the temperature for 1h, raising the temperature to 180-250 ℃ at the temperature raising speed of 3-5 ℃/min, and reacting for 2-4 h;
(5) and after the hydrothermal carbonization is finished, naturally cooling to room temperature, centrifuging for 5-10 min at 5000-8000 rpm, collecting precipitates, sequentially washing the precipitates with distilled water and ethanol, and drying for 4-8 h at 40-60 ℃ to obtain the edible fungus residue based hydrothermal biochar.
In the preparation process, if the control is not good, the raw materials are excessively hydrolyzed into polysaccharide and monosaccharide with smaller molecules, so that graphite microcrystals with topological structures cannot be formed finally; according to the method, the edible fungus residues are subjected to preliminary pore forming by using zinc chloride, under the expansion effect of the zinc chloride on cellulose and the promotion effect of sulfuric acid, the catalyst mixed by sulfuric acid and phosphoric acid quickly permeates into the edible fungus residues, and under the synergistic effect of the zinc chloride, the sulfuric acid and the phosphoric acid, the hydrolysis temperature is reduced, so that the edible fungus residues are subjected to catalytic hydrolysis and dehydration at a lower temperature, and the phenomenon that the specific surface area and the pore structure are reduced due to overhigh temperature is avoided; the zinc chloride and the phosphoric acid form different frameworks, the carbon is deposited on the surface of the carbon in the carbonization process, and after the zinc chloride and the phosphoric acid are washed away, the biochar with a porous structure with a huge specific surface area and different pore diameters is formed; under the synergistic action of sulfuric acid and phosphoric acid, the variety and number of the functional groups on the surface of the biochar are increased. Phosphoric acid is crosslinked with high glycan (a general name of cellulose and hemicellulose) and degradation products thereof in the raw material in the process of heating at a specific speed to form a phosphate ester bond, so that the shrinkage of cell walls after hydrolysis and dehydration of the raw material in the hydrothermal process is prevented, and the prepared biochar has a developed pore-size structure. Through the synergistic cooperation of the steps, the edible fungus dreg is prevented from being excessively hydrolyzed, and the edible fungus dreg biochar with developed aperture and specific surface area and uniform aperture distribution is prepared.
The high glycan is a generic term for cellulose and hemicellulose.
The invention has the following beneficial effects:
the method for preparing the edible fungus residue biochar based on the hydrothermal method can also realize large specific surface area, and the BET specific surface area reaches 962m2The porosity is high, the pore size distribution is uniform, and the stability is good; the method is used for preparing the edible fungus residue biochar based on a hydrothermal method, the carbonization temperature is low, the energy consumption is saved, the types and the number of surface functional groups are large, and the method has excellent adsorption performance on heavy metal ions; the recycling performance is good, and when the heavy metal ions are recycled for 20 times, the removal rate of the heavy metal ions can reach 82.4% of the initial use rate. The hydrothermal biological carbon material with excellent adsorption performance is prepared by utilizing the edible fungus residue waste, and the method has important practical significance for efficient and scientific utilization of the fungus residue waste.
Drawings
FIG. 1: SEM image of biochar prepared in example 1 of the invention.
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 preparation method of edible fungus residue biochar comprises the following steps:
(1) taking pleurotus geesteranus residue waste, and drying in a forced air drying oven at 100 ℃; pulverizing the dried Pleurotus geesteranus residue at 25000 r/min for 0.5min, and sieving with 40 mesh sieve to obtain Pleurotus geesteranus residue powder;
(2) adding the sieved pleurotus geesteranus residue powder into a zinc chloride aqueous solution with the mass concentration of 5-10%, uniformly stirring, and standing for 40min, wherein the mass-volume ratio of the pleurotus geesteranus residue powder to the zinc chloride is 1g:50 mL;
(3) centrifugally filtering the pleurotus geesteranus residues treated in the step (2), adding the pleurotus geesteranus residues into a mixed catalyst, and stirring for 0.5 hour at 1500 revolutions per minute, wherein the mixed catalyst is prepared by mixing sulfuric acid, phosphoric acid and water in a volume ratio of 1:8: 30;
(4) mixing the pleurotus geesteranus residues and the catalyst aqueous solution, magnetically stirring, transferring to a high-pressure reaction kettle, sealing, raising the temperature to 60 ℃ at the speed of 2 ℃/min, preserving the temperature for 1h, raising the temperature to 240 ℃ at the temperature rise speed of 4 ℃/min, and reacting for 3 h;
(5) and after hydrothermal carbonization, naturally cooling to room temperature, centrifuging at 6000 r/min for 8min, collecting precipitate, washing with distilled water and ethanol in sequence, and drying at 50 ℃ for 6h to obtain the pleurotus geesteranus residue-based hydrothermal biochar.
In this example 1, the pleurotus geesteranus mushroom dregs are waste mushroom dregs after pleurotus geesteranus planting, wherein the waste mushroom dregs comprise, by mass, 60-70% of wood chips, 10-20% of cottonseed hulls, 10-20% of wheat bran, 1-2% of calcium superphosphate and 1-2% of quicklime.
The biochar prepared in the example 1 has excellent specific surface area in the field of biochar prepared based on a hydrothermal method, and the BET specific surface area is 962m2The method avoids the use of a high-temperature calcination method, saves energy consumption, ensures that the surface functional groups are not damaged, and has excellent adsorption performance on heavy metal ions, such as Cd2+Has an adsorption amount of 210.3mg/g, Pb2+The adsorption amount of (A) is 220.7mg/g, Cr6+The adsorption amount of (a) is 204.4 mg/g; when the heavy metal ions are repeatedly used for 20 times, the removal rate of the heavy metal ions can reach 81.6 percent of the initial use.
Example 2
A preparation method of edible fungus residue biochar comprises the following steps:
(1) taking the agrocybe aegerita fungus residue waste, and drying in a forced air drying oven at 100 ℃; pulverizing the dried agrocybe aegerita dregs at 25000 r/min for 1min, and sieving with a 80-mesh sieve to obtain agrocybe aegerita dreg powder;
(2) adding the sieved agrocybe aegerita fungus dreg powder into a zinc chloride aqueous solution with the mass concentration of 5-10%, uniformly stirring, and standing for 30min, wherein the mass-volume ratio of the agrocybe aegerita fungus dreg powder to the zinc chloride is 1g:10 mL;
(3) centrifugally filtering the tea tree mushroom dregs treated in the step (2), adding the tea tree mushroom dregs into a mixed catalyst, and stirring for 1h at 1000 revolutions per minute, wherein the mixed catalyst is prepared by sulfuric acid, phosphoric acid and water according to the volume ratio of 2:5: 40;
(4) mixing the agrocybe cylindracea fungus residues with a catalyst aqueous solution, magnetically stirring, transferring to a high-pressure reaction kettle, sealing, raising the temperature to 50 ℃ at the speed of 1 ℃/min, preserving the temperature for 1h, raising the temperature to 250 ℃ at the temperature raising speed of 5 ℃/min, and reacting for 4 h;
(5) and after hydrothermal carbonization, naturally cooling to room temperature, centrifuging for 5min at 5000 r/min, collecting precipitate, sequentially washing with distilled water and ethanol, and drying at 60 ℃ for 4h to obtain the agrocybe cylindracea fungi residue based hydrothermal charcoal.
The specific surface area of the biochar prepared in the example 2 is 910m2And/g, when the catalyst is repeatedly used for 20 times, the removal rate of heavy metal ions can reach 80.9 percent of the first use rate.
Example 3
A preparation method of edible fungus residue biochar comprises the following steps:
(1) taking the agrocybe aegerita fungus residue waste, and drying in a forced air drying oven at 100 ℃; pulverizing the dried agrocybe aegerita fungus residues for 1min at the rotating speed of 25000 revolutions per minute, and sieving with a 60-mesh sieve to obtain edible fungus residue powder;
(2) adding the sieved agrocybe aegerita fungus residues into a zinc chloride aqueous solution with the mass concentration of 10%, uniformly stirring, and standing for 35min, wherein the mass-volume ratio of the agrocybe aegerita fungus residues to the zinc chloride is 1g:40 mL;
(3) centrifugally filtering the tea tree mushroom dregs treated in the step (2), adding the tea tree mushroom dregs into a mixed catalyst, and stirring for 1h at 1200 revolutions per minute, wherein the mixed catalyst is prepared by sulfuric acid, phosphoric acid and water according to the volume ratio of 1.5:6: 20;
(4) mixing the agrocybe cylindracea fungus residues with a catalyst aqueous solution, magnetically stirring, transferring to a high-pressure reaction kettle, sealing, raising the temperature to 55 ℃ at the speed of 1.5 ℃/min, preserving the temperature for 1h, raising the temperature to 180 ℃ at the temperature rise speed of 3 ℃/min, and reacting for 2 h;
(5) and after hydrothermal carbonization, naturally cooling to room temperature, centrifuging at 8000 rpm for 10min, collecting precipitate, washing with distilled water and ethanol in sequence, and drying at 40 ℃ for 8h to obtain the agrocybe cylindracea fungi residue based hydrothermal charcoal.
The specific surface area of the biochar prepared in the example 3 is 922m2And/g, when the catalyst is repeatedly used for 20 times, the removal rate of heavy metal ions can reach 82.4 percent of that of the heavy metal ions used for the first time.
The initial concentration of heavy metal ions is measured by a water sample containing heavy metals, then the biochar prepared by the method is added, the biochar is placed into a constant-temperature water bath oscillator, after oscillation is carried out for 12 hours at 25 ℃, supernate is obtained through centrifugation, the concentration of the residual heavy metals in the water sample is measured by a spectrophotometer, and the adsorption capacity of the biochar to the heavy metal ions can be obtained according to the difference value of the concentrations of the heavy metals before and after the concentration of the heavy metals is shown in Table 1.
Table 1:
| adsorption of heavy metal ions | Cd2+ | Pb2+ | Cr6+ |
| Example 1 | 210.3mg/g | 220.7mg/g | 204.4mg/g |
| Example 2 | 217.2mg/g | 222.6mg/g | 210.7mg/g |
| Example 3 | 214.5mg/g | 225.9mg/g | 212.6mg/g |
Claims (7)
1. A preparation method of edible fungus dreg biochar is characterized by comprising the following steps: drying, crushing and sieving edible fungus residues, uniformly mixing the edible fungus residues with a zinc chloride solution, standing for 30-40 min, then centrifugally separating out fungus residues, adding the fungus residues into a mixed catalyst aqueous solution, carrying out hydrothermal carbonization after magnetic stirring, and then centrifuging, washing and drying; the mixed catalyst aqueous solution is formed by mixing 80-95% of sulfuric acid and 60-85% of phosphoric acid in a mass concentration with water according to a volume ratio of 1-2: 5-8: 20-40.
2. The method for preparing the edible fungus dreg biochar as claimed in claim 1, which is characterized in that: the drying is carried out for 2-4 h at the temperature of 100 ℃ in a blast drying oven, the crushing is carried out for 0.5-1 min at 25000 r/min on the dried edible fungus dregs, and the crushed edible fungus dregs are sieved by a 40-80 mesh sieve.
3. The method for preparing the edible fungus residue biochar as claimed in claim 1 or 2, wherein the method comprises the following steps: the mass volume ratio of the edible fungus residues to the zinc chloride aqueous solution is 1g: 10-50 mL, and the mass concentration of the zinc chloride is 5% -10%.
4. The method for preparing the edible fungus residue biochar as claimed in any one of claims 1 to 3, wherein the method comprises the following steps: the volume ratio of the edible fungus residues subjected to centrifugal separation to the mixed catalyst aqueous solution is 1: 10-40, the stirring speed of the intensive stirring is 1000-1500 rpm, and the stirring time is 0.5-1 h.
5. The method for preparing edible fungus residue biochar as claimed in any one of claims 1 to 4, wherein the method comprises the following steps: the hydrothermal carbonization is to mix edible fungus residues and a catalyst aqueous solution, magnetically stir the mixture, transfer the mixture to a high-pressure reaction kettle, seal the reaction kettle, raise the temperature to 50-60 ℃, preserve heat for 1 hour, then raise the temperature to 180-250 ℃ and react for 2-4 hours.
6. The method for preparing the edible fungus dreg biochar as claimed in claim 1, which is characterized in that: and after the hydrothermal carbonization is finished, naturally cooling to room temperature, centrifuging for 5-10 min at 5000-8000 rpm, collecting precipitates, washing the precipitates with distilled water and ethanol in sequence, and drying at 40-60 ℃ for 4-8 h to obtain the edible fungus residue-based hydrothermal biochar.
7. A preparation method of edible fungus residue biochar comprises the following steps:
(1) taking edible fungus residue waste, and drying in a forced air drying oven at 100 ℃; crushing the dried edible fungus residues at 25000 r/min for 0.5-1 min, and sieving with a 40-80 mesh sieve to obtain edible fungus residue powder;
(2) adding the sieved edible fungus residue powder into a zinc chloride aqueous solution with the mass concentration of 5-10%, uniformly stirring, and standing for 30-40 min, wherein the mass-volume ratio of the edible fungus residue powder to the zinc chloride is 1g: 10-50 mL;
(3) centrifuging and filtering the edible fungus residues treated in the step (2), adding the edible fungus residues into a mixed catalyst, and stirring for 0.5-1 h at 1000-1500 rpm, wherein the mixed catalyst is prepared from sulfuric acid, phosphoric acid and water, and the volume ratio of the sulfuric acid to the phosphoric acid to the water is 1-2: 5-8: 20-40;
(4) mixing the edible fungus residues with the mixed catalyst aqueous solution, magnetically stirring, transferring to a high-pressure reaction kettle, sealing, raising the temperature to 50-60 ℃, preserving the temperature for 1h, raising the temperature to 180-250 ℃, and reacting for 2-4 h;
(5) and after the hydrothermal carbonization is finished, naturally cooling to room temperature, centrifuging for 5-10 min at 5000-8000 rpm, collecting precipitates, sequentially washing the precipitates with distilled water and ethanol, and drying for 4-8 h at 40-60 ℃ to obtain the edible fungus residue based hydrothermal biochar.
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