CN113249132A - Livestock and poultry manure anaerobic fermentation biogas residue biomass charcoal, and preparation method and application thereof - Google Patents
Livestock and poultry manure anaerobic fermentation biogas residue biomass charcoal, and preparation method and application thereof Download PDFInfo
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- CN113249132A CN113249132A CN202110339565.2A CN202110339565A CN113249132A CN 113249132 A CN113249132 A CN 113249132A CN 202110339565 A CN202110339565 A CN 202110339565A CN 113249132 A CN113249132 A CN 113249132A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
- C10B57/10—Drying
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing
Abstract
The invention discloses a preparation method of biogas residue biomass charcoal through anaerobic fermentation of livestock and poultry manure, which comprises the following steps: (1) drying the collected livestock and poultry manure anaerobic fermentation biogas residues to constant weight and mechanically crushing the biogas residues into powder for later use; (2) putting the powder obtained in the step (1) into a furnace for pyrolysis, and grinding the obtained black solid after pyrolysis is finished; (3) putting the powder ground in the step (2) into water, cleaning to be neutral and drying; (4) and (4) grinding the powder dried in the step (3) and sieving the powder with a 100-mesh sieve to obtain the biogas residue biomass charcoal. The method has the advantages of simple synthetic route, low preparation cost and large-scale production, and the prepared biogas residue biomass carbon can effectively adsorb bisphenol A in water and activate persulfate to degrade bisphenol A.
Description
Technical Field
The invention belongs to the technical field of biomass charcoal preparation and application, and particularly relates to biogas residue biomass charcoal obtained by anaerobic fermentation of livestock and poultry manure, and a preparation method and application thereof.
Background
Bisphenol a (bpa) is one of the most widely used industrial chemicals as a raw material for the production of polycarbonate plastics, epoxy resins and phenolic resins. According to the united states environmental protection agency's reports, over 100 million pounds of BPA are released into the environment each year. However, BPA is difficult to decompose in the environment and can cause serious damage to the reproductive organs of the organism. Therefore, it is highly desirable to develop a BPA treatment technique that is efficient, low cost, and free of secondary pollution.
Advanced Oxidation Processes (AOPs) are a technology that can efficiently degrade refractory organic pollutants in wastewater. In recent years, persulfate-based advanced oxidation processes (PS-AOPs) have shown promising application in the treatment of refractory pollutants. With hydroxyl radicals (HO) generated in Fenton or Fenton-like reaction system·-) In contrast, sulfate radicals (SO) generated in persulfate advanced oxidation processes4 ·-) Having a higher oxidation potential (E)02.5-3.1V) and longer half-life (30-40 μ s). Except for SO4 ·-In addition, there is a possibility that singlet oxygen may be generated during the persulfate activation1O2) And superoxide (O)2 ·-) They are also highly effective in removing contaminants. Because of the strong stability of persulfate, transition metal or nonmetal carbon-based materials are commonly used for activation. Although transition metals are effective in activating persulfates, significant metal leaching and expensive costs limit the practical application of this technology. Therefore, it is urgently needed to develop a functional material with low cost, environmental protection and no secondary pollution.
Biomass charcoal, a carbonaceous material produced by pyrolysis of biomass, is considered to be a persulfate activator that is inexpensive and has great potential for development. Studies have shown that the production cost per ton of biomass charcoal is $ 1000 cheaper than activated carbon. However, the biomass charcoal is an inert material, and the catalytic property of the biomass charcoal can be exerted only by regulating the surface of the biomass charcoal. The nitrogen doping can adjust sp2The electronic property of the hybrid carbon skeleton and the more active sites given to the biomass charcoal. Various nitrogen-doped biomass charcoals have been developed for persulfate activation, but their preparation methods are complex. In addition, an external nitrogen source (urea, melamine, ammonium chloride and the like) is generally required to be added in the preparation process of the nitrogen-doped biomass charcoal, which undoubtedly increases the preparation cost and limits the large-scale production of the nitrogen-doped biomass charcoal. Therefore, the development of the nitrogen-doped biomass carbon with low cost, simple preparation and environmental protection is very important for the persulfate advanced oxidation process.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide biomass charcoal which is simple in synthetic route, low in preparation cost and capable of being produced in a large scale and a preparation method thereof. The invention also aims to provide a method for degrading organic wastewater by using nitrogen-doped biomass charcoal activated persulfate, which has high organic pollutant removal efficiency and no secondary pollution.
The technical scheme is as follows: the preparation method of the livestock and poultry manure anaerobic fermentation biogas residue biomass charcoal comprises the following steps:
(1) drying the collected livestock and poultry manure anaerobic fermentation biogas residues to constant weight and mechanically crushing the biogas residues into powder for later use;
(2) putting the powder obtained in the step (1) into a furnace for pyrolysis, and grinding the obtained black solid after pyrolysis is finished;
(3) putting the powder ground in the step (2) into water, cleaning to be neutral and drying;
(4) and (4) grinding the powder dried in the step (3) and sieving the powder with a 100-mesh sieve to obtain the biogas residue biomass charcoal.
The resulting biomass char is named DBCn (where n represents the pyrolysis temperature, e.g. biogas residue biomass char prepared at 500 ℃ is named DBC 500).
Further, the pyrolysis temperature is 500-800 ℃.
Further, the furnace in the step (2) is a muffle furnace, and the heating rate of the muffle furnace is 5-10 ℃/min.
Further, the drying temperature in the step (3) is 60-80 ℃.
Further, the livestock and poultry manure anaerobic fermentation biogas residue is cow manure anaerobic fermentation biogas residue.
The application of the biogas residue biomass charcoal obtained by anaerobic fermentation of livestock and poultry manure in treatment of BPA-containing wastewater.
Further, at normal temperature, adding cow dung biogas residue biomass charcoal and an oxidant into the BPA-containing wastewater, wherein the oxidant is PMS monosulfate, PDS peroxodisulfate and H hydrogen peroxide2O2One or more of them.
Further, 0.2g/L of cow dung biogas residue biomass charcoal and 5mmol/L of oxidant are added into BPA wastewater containing 10mg/L at normal temperature, wherein the oxidant is PMS, PDS and H2O2One or more of them.
In recent years, nitrogen-doped biomass charcoal is widely used in advanced oxidation processes as a catalytic material with excellent performance. Due to the huge specific surface area and the developed pore structure of the biomass charcoal, the biomass charcoal can effectively adsorb pollutants, so that the pollutants can be quickly removed. In addition, the nitrogen-doped biomass charcoal can effectively catalyze PMS, PDS and H2O2And the oxidizing agent decomposes to generate Reactive Oxygen Species (ROS) having a higher redox potential. These ROS can oxidize some of the recalcitrant pollutants that are difficult to remove by traditional sewage treatment techniques. It is worth noting that the raw materials required for preparing the biomass charcoal are wide in source, cheap and easy to obtain. Therefore, from the economic perspective, biomass charcoal is considered as a material with wide application prospect in the environment. The method takes the biogas residues obtained after the anaerobic fermentation of the livestock and poultry manure as the raw material, and obtains the nitrogen-doped biomass charcoal with high added value through pyrolysis. The method not only realizes the harmless treatment of the livestock and poultry manure, but also provides new insight for the synthesis of nitrogen-doped biomass charcoal in the advanced oxidation process.
Has the advantages that: the method has the advantages of simple synthetic route, low preparation cost and large-scale production, and the obtained cow dung biogas residue biomass carbon has excellent adsorption capacity and strong catalytic capacity. Wherein DBC800 not only can adsorb a large amount of BPA, but also can effectively activate PDS and PMS to realize the oxidative degradation of BPA. Therefore, DBC800 can be used as an ideal functional material for treating BPA-containing wastewater.
Drawings
FIG. 1 is a graph showing the adsorption kinetics (pseudo first order kinetics) of biomass carbon from biogas residues on BPA;
FIG. 2 is a graph showing the adsorption kinetics (pseudo-secondary kinetics) of the biogas residue biomass charcoal on BPA;
FIG. 3 shows the biogas residue biomass charcoal activation H2O2Degradation of BPA graphs;
FIG. 4 is a graph showing BPA degradation by activated PMS of biogas residue biomass charcoal;
FIG. 5 is a graph showing BPA degradation by activated PDS of biogas residue biomass charcoal;
FIG. 6 is a bar graph of BPA removal efficiency for different oxidation systems;
FIG. 7 shows DBC800 activating different oxidants (PMS, PDS, H)2O2) Degradation of BPA graphs;
FIG. 8 is a timing current diagram for the DBC800/PMS/BPA system.
Detailed Description
For a further understanding of the contents of the present invention, reference will now be made in detail to the following examples.
The detection method of BPA concentration comprises the following steps: and detecting the concentration of the BPA by adopting a high performance liquid chromatography. The detection instrument is a Fuli FL-5090 chromatograph. The detection conditions are as follows: the mobile phase is 70% methanol + 30% water, the flow rate is 1ml/min, and the detection wavelength is 227 nm.
Example 1
A synthetic route of cow dung biogas residue biomass charcoal comprises the following steps:
(1) drying the collected cow dung biogas residues at 60 ℃ for 12 hours, and mechanically crushing the cow dung biogas residues into powder for later use;
(2) taking 4 parts of the powder obtained in the step (1), respectively placing the 4 parts of the powder in a crucible with the number of 1# -4# samples, placing the 1# sample in a muffle furnace at 500 ℃, placing the 2# sample in a muffle furnace at 600 ℃, placing the 3# sample in a muffle furnace at 700 ℃, placing the 4# sample in a muffle furnace at 800 ℃, wherein the heating rate of the muffle furnace is 10 ℃/min, and the 1# -4# samples are respectively pyrolyzed for 2 hours;
(3) cooling the sample pyrolyzed in the step (2) and grinding the sample into black powder;
(4) repeatedly washing the sample obtained in the step (3) with distilled water, removing impurities in the sample and ensuring that the pH value of the solution is 7;
(5) drying the sample obtained after washing in the step (4) in an oven at 80 ℃ for 6 hours to constant weight, and grinding and sieving the sample with a 100-mesh sieve to obtain the cow dung biogas residue biomass charcoal;
the specific surface area and the pore volume and the pore diameter of the biogas residue biomass charcoal measured by a BET specific surface area test method are shown in the table 1.
TABLE 1
| Biomass charcoal | Specific surface area m2 g-1 | Pore volume cm3 g-1 | Pore size nm |
| DBC500 | 28.824 | 0.031 | 4.062 |
| DBC600 | 57.367 | 0.066 | 3.853 |
| DBC700 | 53.150 | 0.065 | 3.831 |
| DBC800 | 66.796 | 0.082 | 3.818 |
Example 2:
the biogas residue biomass charcoal prepared in example 1 was used as an adsorbent for BPA. The experimental procedure was as follows:
(1) a100 mL beaker was used as a reactor, and 50mL of 10mg/L BPA wastewater was added, each being numbered from # 1 to # 4.
10mg of sample # 1 from example 1 was added to reactor # 1;
10mg of sample # 2 from example 1 was added to reactor # 2;
10mg of sample # 3 from example 1 was added to reactor # 3;
10mg of sample # 4 from example 1 was added to reactor # 4.
Magnetic stirring (150rpm) was carried out separately, and samples were taken at preset time intervals.
And detecting the concentration of the residual BPA by adopting a high performance liquid chromatography, and drawing an adsorption kinetics curve.
The dynamic results of adsorption of BPA on biogas residue biomass charcoal prepared at different temperatures in example 1 are shown in fig. 1 and 2. As can be seen from fig. 1 and 2, the adsorption capacity of the biogas residue biomass carbon to BPA is improved along with the increase of the pyrolysis temperature, and the result of the kinetic fitting more conforms to pseudo-second-order kinetics, which indicates that the BPA adsorption process belongs to chemical adsorption.
Example 3
Experimental procedures and conditions were similar to those of example 2, and 5mM of H was added to the # 1-4 reactors after equilibrium of BPA adsorption2O2Stirred and sampled.
Biogas residue biomass charcoal activation H prepared at different temperatures in example 12O2The effect of degrading BPA-containing wastewater is shown in figure 3. As shown in fig. 3, biogas residue biomass charcoal is paired with H2O2The activation capacity is weak. Value ofIt is noted that biogas residue biomass charcoal prepared at different pyrolysis temperatures is activated by H2O2The effect of (c) is different. Wherein, DBC800 is to H2O2Has the strongest activation capability. From the figure, DBC800 is best at removing BPA, so subsequent studies have been mainly developed around DBC 800.
Example 4
The experimental procedure and conditions were similar to those of example 2, and after equilibrium of BPA adsorption, 5mM PMS was added to the # 1-4 reactor, respectively, and stirred and sampled.
The effect of activating PMS to degrade BPA-containing wastewater by biogas residue biomass charcoal prepared at different temperatures in example 1 is shown in FIG. 4. As shown in fig. 4, the effect of activating PMS by biogas residue biomass charcoal prepared at different pyrolysis temperatures is different. Among them, DBC800 has the strongest activation capability to PMS. From the figure, the effects of DBC800 in adsorbing and activating PMS to degrade BPA are both optimal, so subsequent studies are mainly performed around DBC 800. At the same time, a reaction rate constant k is establishedapp(min-1) And equilibrium adsorption quantity qe(mg/g) and the results show that the correlation between the two samples is determined by qe(mg/g) increase, reaction rate constant kapp(min-1) The increase indicates that the adsorption process is effective in promoting BPA removal.
Example 5
Experimental procedures and conditions were similar to those of example 2, and 5mM of PDS was added to the # 1-4 reactor after equilibrium of BPA adsorption, followed by stirring and sampling.
The effect of activating PDS by biogas residue biomass charcoal prepared at different temperatures in example 1 on degrading BPA-containing wastewater is shown in FIG. 5. As shown in fig. 5, the effect of PDS activation by biogas residue biomass charcoal prepared at different pyrolysis temperatures is different. Among them, DBC800 has the strongest activation ability for PDS. In addition, the reaction rate constant k is discussedapp(min-1) And equilibrium adsorption quantity qe(mg/g) and the results show that q is a correlatione(mg/g) and reaction rate constant kapp(min-1) A good positive linear relationship exists between the BPA and the BPA, which shows that the adsorption process can effectively promote the removal of the BPA. From the figure, DBC800 adsorbs and activates PDS degradation BThe effect of PA is optimal, so subsequent studies have mainly been spread around DBC 800.
Example 6
Sample # 4 prepared in example 1 DBC800 was used as a catalyst. The experimental procedure was as follows:
(1) 3 100mL beakers were used as reactors, 50mL of 10mg/L BPA wastewater was added, and the reactors were numbered # 1- # 3, respectively. 10mg of the sample No. 4 in example 1 is added into the reactor No. 1-3 respectively; magnetic stirring (150rpm) was performed separately, and sampling tests were performed at preset time intervals. When the adsorption of BPA reaches equilibrium, 5mM H is added into the 1# -3# reactor respectively2O2PMS, PDS, stirred and sampled.
Biogas residue biomass charcoal DBC800 activated H prepared in example 12O2The effect of degrading the BPA-containing wastewater by PMS and PDS is shown in FIG. 6. As shown in FIG. 6, the obtained biomass charcoal DBC800 is paired with H2O2The activation capability is the weakest, the activation capability to PDS is stronger, and the activation capability to PMS is the strongest.
The BPA removal rates obtained in examples 3-6 were plotted in a histogram. The conclusion is as follows:
as shown in FIG. 7, DBCn/H2O2The system has a weak BPA removal effect and almost contributes to the adsorption effect of the biomass charcoal. The DBCn/PDS system greatly improves the BPA removal effect, and shows that the biogas residue biomass charcoal can effectively activate PDS to degrade BPA. For the DBCn/PMS system, the BPA removal effect is the best. Furthermore, it is known by comparison that the catalytic performance of DBC800 is better than that of DBC500, DBC600 and DBC700, which may be attributed to the larger specific surface area and good pore structure of DBC800, thus providing more active sites to adsorb pollutants and catalyze the decomposition of oxidants.
Example 7
Using sample # 4 DBC800 prepared in example 1 as a catalyst, the experimental procedure was as follows:
a carbon paper electrode supporting DBC800 powder was first prepared. The preparation method comprises the following steps: nafion solution (5.0 wt%, 0.1mL) and DBC800 powder (10mg) and ethanol (1mL) were mixed, and the mixture was then ultrasonically dispersed for 3h to give a homogeneous suspension. And uniformly coating 20 mu L of suspension on the surface of the carbon paper, and drying the carbon paper coated with the suspension at 60 ℃ for 8h to obtain the carbon paper electrode. The electrochemical experiments were performed on an electrochemical workstation CHI 760E, selecting a three-electrode system, with a silver/silver chloride electrode (Ag/AgCl) and a platinum wire as reference and counter electrodes, respectively. The chronoamperometric measurements were carried out with a deviation of 0.0V (vs. Ag/AgCl), the test time was set to 250s, and PMS solution and BPA solution were added at 50s and 150s, respectively. The current output of the DBC800 working electrode after PMS/BPA addition is given in FIG. 8. After addition of PMS and BPA at 50s and 150s, respectively, significant current generation was observed, which demonstrates strong electron transfer between PMS, BPA and DBC800 surfaces. Thus, the degradation of BPA is rapidly achieved.
Claims (10)
1. A preparation method of biogas residue biomass charcoal through anaerobic fermentation of livestock and poultry manure is characterized by comprising the following steps:
(1) drying the collected livestock and poultry manure anaerobic fermentation biogas residues to constant weight and mechanically crushing the biogas residues into powder for later use;
(2) putting the powder obtained in the step (1) into a furnace for pyrolysis, and grinding the obtained black solid after pyrolysis is finished;
(3) putting the powder ground in the step (2) into water, cleaning to be neutral and drying;
(4) and (4) grinding and sieving the powder dried in the step (3) to obtain the biomass charcoal of the anaerobic fermentation biogas residues of the livestock and poultry manure.
2. The method of claim 1, wherein the pyrolysis temperature is from 500 ℃ to 800 ℃.
3. The method according to claim 1, wherein the furnace in the step (2) is a muffle furnace, and the heating rate of the muffle furnace is 5-10 ℃/min.
4. The method according to claim 1, wherein the drying temperature in the step (3) is 60 to 80 ℃.
5. The method according to claim 1, wherein the grinding and sieving in step (4) is 100 mesh sieving.
6. The preparation method according to claim 1, wherein the livestock and poultry manure anaerobic fermentation biogas residue is cow manure anaerobic fermentation biogas residue.
7. Livestock and poultry manure anaerobic fermentation biogas residue biomass charcoal prepared by the preparation method of any one of claims 1 to 6.
8. The use of the biomass charcoal of the anaerobic fermentation biogas residue of livestock and poultry manure prepared in the claim 7 in the treatment of bisphenol A-containing wastewater.
9. The application of the method as claimed in claim 8, wherein the cow dung biogas residue biomass charcoal and an oxidant are added into the bisphenol A-containing wastewater at normal temperature, wherein the oxidant is peroxymonosulfate, peroxydisulfate or hydrogen peroxide.
10. The application of claim 9, wherein 0.2g/L of cow dung biogas residue biomass charcoal and 5mmol/L of oxidant are added to the BPA wastewater containing 10 mg/L.
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| CN113828361A (en) * | 2021-09-16 | 2021-12-24 | 广州大学 | Waste recycling catalyst, preparation method thereof and application thereof in treatment of organic pollutants |
| CN113828361B (en) * | 2021-09-16 | 2023-11-10 | 广州大学 | Catalyst for recycling waste, preparation method thereof and application thereof in treatment of organic pollutants |
| CN115518639A (en) * | 2022-07-19 | 2022-12-27 | 广州大学 | Environment-friendly catalyst prepared from livestock and poultry manure, synthetic method and application |
| CN115518639B (en) * | 2022-07-19 | 2023-11-03 | 广州大学 | Environment-friendly catalyst for preparing livestock and poultry manure, synthesis method and application |
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Application publication date: 20210813 |