CN111392710A - Biochar based on waste egg shells and preparation method and application thereof - Google Patents
Biochar based on waste egg shells and preparation method and application thereof Download PDFInfo
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- CN111392710A CN111392710A CN202010259456.5A CN202010259456A CN111392710A CN 111392710 A CN111392710 A CN 111392710A CN 202010259456 A CN202010259456 A CN 202010259456A CN 111392710 A CN111392710 A CN 111392710A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses biochar based on waste egg shells and a preparation method and application thereof. The technical scheme of the invention has the advantages of simple pretreatment, short pyrolysis time, good adsorption effect and good application value.
Description
Technical Field
The invention belongs to the technical field of biomass application, and particularly relates to biochar based on waste egg shells and a preparation method and application thereof.
Background
With the increase of the number of human beings and the development of intensive animal husbandry, antibiotics have been widely used for the prevention and treatment of infectious diseases of human beings and animals since the early 1990 s, such as tetracycline hydrochloride, which is a broad-spectrum antibiotic, and the action mechanism thereof is mainly to prevent the combination of aminoacyl and ribosomes, to prevent the growth of peptide chains and the synthesis of proteins, thereby inhibiting the growth of bacteria, and to be widely used for the treatment of diseases. However, most antibiotics including tetracycline cannot be completely metabolized by animals due to their poor biodegradability, and the continuous intensive use of antibiotics leads to the detection of antibiotics or their active substances in urine and feces in amounts of 70% to 90% of the amounts used, which in turn leads to the problem of antibiotic residues. Antibiotic residues in the environment can have adverse effects on soil organisms and plants. Antibiotics at low concentration levels can have an impact on human health and various ecosystems and are even a threat, and thus antibiotic residues in the environment are of great concern to various scholars.
In addition to the direct adverse effects of antibiotics causing residue problems, antibiotics also interact with manure, affecting the biomass and structural composition of soil microorganisms, and also producing compounds. These effects increase bacterial resistance, allowing more and more bacteria to develop antibiotic resistance genes, and these resistant pathogens can even infect humans and animals. Since 1994, the european union has prohibited chloramphenicol administration to food animals, but due to its side effects, high abundance of some resistance genes has still been detected. It is estimated that the number of deaths attributable to antibacterial drug resistance has exceeded 70 million people per year since 2014, with the expectation that it will continue to increase to 1000 million people by 2050.
Antibiotics further spread antibiotic-resistant microorganisms through water pollution, and serious harm is brought to ecological environment and human survival, so that the reduction and removal of the content of antibiotics become a problem to be solved urgently. Currently, technologies for removing antibiotics from water include adsorption, reverse osmosis, photocatalytic oxidation, and ion exchange, among which, charcoal adsorption is considered to be the most convenient and economical environmentally friendly method.
The biochar is a solid carbon material prepared by pyrolyzing animal or plant biomass under an anaerobic environment condition, has the advantages of low production cost, stable adsorption performance, high specific surface area, high porosity and rich and various surface functional groups, is beneficial to removing pollutants in an aqueous solution, and is a repairing adsorbent with a good application prospect in the aspect of water treatment. At present, research shows that the biochar has great potential in adsorbing antibiotics. Vitanage and the like discover that the acidic modified pine residue biochar improves the adsorption capacity of sulfadiazine and increases the specific surface area of the biochar. Anders et al found that the microbial community in the soil changed significantly after the addition of biochar, and Muhammad et al found that different types of biochar could cause different microbial community structural changes. Adsorption can greatly affect the homing and impact of contaminants in the environment through different mechanisms, for example, the main mechanisms of biochar adsorption of antibiotics include EDA pi-pi interactions and electrostatic interactions, both of which reveal the binding of metals and antibiotics to functional groups on biochar. In addition, the addition of heavy metals can promote or inhibit the adsorption of antibiotics, and researches show that the addition of Cu (II) can promote the adsorption of the biochar to the oxytetracycline and inhibit the adsorption of the ofloxacin, and also show that the addition of low-concentration Cu (II) can promote the adsorption capacity of the tetracycline coexisting on the biochar and the addition of high-concentration Cu (II) can inhibit the adsorption capacity of the tetracycline. The existing biochar can meet the requirement of antibiotic adsorption, but has the problems of expensive raw materials, low removal efficiency and the like.
Disclosure of Invention
Aiming at the defects of high manufacturing cost and low removal efficiency of the biochar in the prior art, the invention aims to provide a preparation method of biochar based on waste egg shells and application of the biochar to adsorption of tetracycline hydrochloride in wastewater.
The invention is realized by the following technical scheme:
a preparation method of biochar based on waste egg shells specifically comprises the following steps:
1) drying the cleaned eggshell in a drying oven and then crushing for later use;
2) placing pulverized ovum gallus Domesticus crusta in a tube furnace, heating to 200 deg.C under nitrogen atmosphere, and maintaining for 20 min; continuously heating to 400 deg.C, and maintaining for 20 min; continuously heating to 700 deg.C, and maintaining for 60 min;
3) cooling to room temperature under the protection of nitrogen, sieving, and reserving 80-60 mesh biochar for later use.
Further, in the step (1), the drying condition is that the temperature is 105 ℃, and the drying time is 8 hours.
Further, the temperature rise condition in the step (2) is 10 ℃/min.
In another aspect of the present invention, the biochar based on waste egg shells prepared by the above preparation method is also within the protection scope of the present invention.
In another aspect of the invention, the application of the biochar based on the waste egg shells in wastewater treatment is provided, in particular to the application of the biochar based on the waste egg shells in adsorption of tetracycline hydrochloride in wastewater.
Preferably, the optimum pH for removing tetracycline hydrochloride from the wastewater is 9.
The invention has the beneficial effects that:
the economic benefits of the invention are as follows: simple pretreatment, short pyrolysis time, good adsorption effect and good application value.
The social benefit of the invention is as follows: 300 million tons of eggshells are discarded every year in China. The biochar prepared by pyrolysis changes waste into valuable, is used as a good adsorbent for the tetracycline hydrochloride in the wastewater, and accords with the concepts of low-carbon, environment-friendly, economy and sustainable development in China.
Drawings
FIG. 1 is an SEM image of biochar prepared by the present invention;
FIG. 2 is the effect of different pH on adsorption capacity;
FIG. 3 is the effect of reaction time on adsorption capacity.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
The embodiment provides a biochar based on waste egg shells, which is prepared by the following steps:
1) cleaning egg white on the surface of waste egg shells, drying in an electric heating air blast drying oven at 105 deg.C for 8 hr, and grinding the dried egg shells.
2) Placing the ground eggshells in a tube furnace, and continuously introducing N2. The following temperature programming method is adopted: heating to 200 deg.C at a speed of 10 deg.C/min, and standing for 20 min; heating to 400 deg.C at a speed of 10 deg.C/min, and standing for 20 min; heating to 700 deg.C at a speed of 10 deg.C/min, and standing for 60 min. In N2Cooling to room temperature under protection and taking out.
3) And cooling, and then sieving, and reserving 80-60 meshes of biochar for later use.
Example 2 characterization of biochar
The biochar prepared in the example is verified in aspects of SEM characteristic structure, Fourier infrared spectrum, pH and the like.
1) Biological carbon SEM representation structure
The raw material of egg shell, biochar and adsorbed biochar were characterized by SEM (scanning electron microscope). As can be seen from figure 1, the raw material of the eggshell is smooth, the surface wrinkles are increased after the raw material is prepared into the biochar, and the pore-shaped structure is more. The rough surface improves the specific surface area of the biochar and provides more point positions for adsorption.
2) EDS elemental analysis
Elemental analysis is shown in table 1:
TABLE 1 elemental analysis of eggshell raw materials
It can be seen that after the raw material is prepared into biochar, the content of each element is reduced due to volatilization of the elements caused by temperature rise during cracking, and the N element is completely disappeared.
Example 3 application of biochar prepared from eggshells to tetracycline hydrochloride adsorption
1) Influence of pH on the adsorption
As can be seen from the observation of FIG. 2, when the solution concentration is constant, the adsorption capacity sequence of tetracycline hydrochloride is from pH11 > pH9 > pH7 > pH5 > pH3 in order of increasing to decreasing, and the best adsorption effect of tetracycline hydrochloride by biochar at 500mg/m L and pH9 is 683.75 when all the pH values are compared, thereby finding that higher pH values have other interaction forces stronger than electrostatic interaction for deprotonated tetracycline hydrochloride.
2) Effect of reaction time on adsorption Capacity
In the test, 16 time points are selected, and the adsorption capacity of the biochar at different temperatures and different times is observed. As can be seen from FIG. 3, the adsorption capacity of tetracycline hydrochloride increases with the gradual increase of time under other fixed conditions, and the adsorption is generally stable at the early stage temperature and mainly at the later stage under the four time conditions. The maximum adsorption rate is 1260min-2880min at 15 ℃ and 25 ℃, and 540min-900min at 35 ℃. The adsorption effect is best at 45 ℃, and the maximum adsorption quantity is 1228.05 mg/g. It can thus be seen that the increase in temperature favors the adsorption of the biochar.
The foregoing embodiments are intended to illustrate that the invention may be implemented or used by those skilled in the art, and modifications to the above embodiments will be apparent to those skilled in the art, and therefore the invention includes, but is not limited to, the above embodiments, any methods, processes, products, etc., consistent with the principles and novel and inventive features disclosed herein, and fall within the scope of the invention.
Claims (7)
1. A preparation method of biochar based on waste egg shells is characterized by comprising the following steps:
1) drying the cleaned eggshell in a drying oven and then crushing for later use;
2) placing pulverized ovum gallus Domesticus crusta in a tube furnace, heating to 200 deg.C under nitrogen atmosphere, and maintaining for 20 min; continuously heating to 400 deg.C, and maintaining for 20 min; continuously heating to 700 deg.C, and maintaining for 60 min;
3) cooling to room temperature under the protection of nitrogen, sieving, and reserving 80-60 mesh biochar for later use.
2. The method for preparing biochar based on waste egg shells according to claim 1, wherein the drying condition in the step (1) is that the temperature is 105 ℃, and the drying time is 8 hours.
3. The method for preparing biochar based on waste egg shells according to claim 1, wherein the temperature rise condition in the step (2) is 10 ℃/min.
4. The biochar based on waste egg shells prepared by the preparation method of claim 1.
5. Use of the biochar based on waste egg shells of claim 4 in wastewater treatment.
6. The use according to claim 5, for adsorbing tetracycline hydrochloride in wastewater.
7. The use according to claim 6, wherein the pH optimum for the removal of tetracycline hydrochloride from wastewater is 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010259456.5A CN111392710A (en) | 2020-04-03 | 2020-04-03 | Biochar based on waste egg shells and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010259456.5A CN111392710A (en) | 2020-04-03 | 2020-04-03 | Biochar based on waste egg shells and preparation method and application thereof |
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| CN111392710A true CN111392710A (en) | 2020-07-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111744459A (en) * | 2020-07-22 | 2020-10-09 | 安徽农业大学 | Preparation method of rice straw modified biochar for removing tetracycline in water body |
| CN114849648A (en) * | 2022-06-15 | 2022-08-05 | 昆明理工大学 | Preparation method of adsorbent for efficiently removing heavy metal Cr (VI) |
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| CN107123550A (en) * | 2017-05-16 | 2017-09-01 | 郭家林 | A kind of egg shell derives the preparation method of three-dimensional honeycomb shape carbon material |
| CN109455699A (en) * | 2017-09-06 | 2019-03-12 | 哈尔滨工业大学 | A kind of graphene and its preparation method and application prepared using shell or eggshell waste |
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| CN110756168A (en) * | 2019-12-04 | 2020-02-07 | 河南师范大学 | Preparation method and application of modified biochar for adsorbing tetracycline in wastewater |
-
2020
- 2020-04-03 CN CN202010259456.5A patent/CN111392710A/en active Pending
Patent Citations (5)
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| CN104370285A (en) * | 2014-10-23 | 2015-02-25 | 北京大学 | Method for macroscopically preparing high-quality graphene by using bio-mineralized material |
| CN107123550A (en) * | 2017-05-16 | 2017-09-01 | 郭家林 | A kind of egg shell derives the preparation method of three-dimensional honeycomb shape carbon material |
| CN109455699A (en) * | 2017-09-06 | 2019-03-12 | 哈尔滨工业大学 | A kind of graphene and its preparation method and application prepared using shell or eggshell waste |
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Non-Patent Citations (1)
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| LING ZHAO ET AL.: "Mineral Constituents Profile of Biochar Derived from Diversified Waste Biomasses: Implications for Agricultural Applications", 《JOURNAL OF ENVIRONMENTAL QUALITY》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111744459A (en) * | 2020-07-22 | 2020-10-09 | 安徽农业大学 | Preparation method of rice straw modified biochar for removing tetracycline in water body |
| CN114849648A (en) * | 2022-06-15 | 2022-08-05 | 昆明理工大学 | Preparation method of adsorbent for efficiently removing heavy metal Cr (VI) |
| CN114849648B (en) * | 2022-06-15 | 2023-11-21 | 昆明理工大学 | Preparation method of adsorbent for efficiently removing heavy metal Cr (VI) |
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