CN112939187A - Method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate - Google Patents
Method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate Download PDFInfo
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- CN112939187A CN112939187A CN202110135481.7A CN202110135481A CN112939187A CN 112939187 A CN112939187 A CN 112939187A CN 202110135481 A CN202110135481 A CN 202110135481A CN 112939187 A CN112939187 A CN 112939187A
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
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Abstract
The invention discloses a method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate, which is characterized by taking the sludge back, standing until sludge and water are separated, pouring out supernatant, filtering the sludge, drying to constant weight, mixing the sludge with nitrogenous organic matters, putting the mixture into a tubular furnace for pyrolysis in a nitrogen atmosphere, taking out the mixture, washing the mixture to be neutral by using clear water, and drying to obtain biochar; adding biochar and peroxydisulfate into the sewage containing organic pollutants and heavy metals at normal temperature and normal pressure, and continuously stirring the whole system to remove the organic pollutants and the heavy metals in the sewage. The nitrogen-doped sludge biochar can efficiently activate the peroxydisulfate after high-temperature pyrolysis, can react with most of organic pollutants and remove heavy metals, and has high reaction rate and low influence of pH in water.
Description
Technical Field
The invention relates to a method for removing organic pollutants and heavy metals in a water body, in particular to a method for efficiently and jointly removing the organic pollutants and the heavy metals in the water body by utilizing high-temperature pyrolysis nitrogen-doped sludge biochar and using peroxydisulfate in parallel in the field of water treatment, and belongs to the technical field of water treatment.
Background
In recent years, the economic growth rate of China enters a high-speed development level, the industrialization process is further improved, the exploitation and the use of surface water are increased day by day, and the problem of water pollution is increasingly serious. With the lapse of time, a considerable part of pollutants in surface water, including common pollutants, novel pollutants, heavy metals and the like, easily pass through surface runoff and rainwater scouring, and gradually immerse in groundwater environment and soil horizon, bring adverse effects to ecological environment and human survival safety. The pollution components of the polluted wastewater mainly comprise heavy metals and organic matters, the water and soil pollution form is a point-area surface, the pollution substances tend to increase from inorganic components to organic components, and the pollution elements tend to increase from single components to multiple mixtures.
Relevant researches show that the harm of water and soil pollution to ecology and human health is huge and even irreversible, and drinking underground water polluted by organic matters can cause diarrhea and liver diseases, and long-term drinking can cause cancers; drinking groundwater contaminated with heavy metals can cause kidney diseases and damage to the nervous system of the human body, drinking groundwater contaminated with hormones can affect the endocrine system of the human body, and long-term drinking can cause cancers and deformities.
Advanced oxidation techniques (AOPs for short) are the most efficient known methods for degrading toxic, nonbiodegradable and persistent emerging organic pollutants. The basic principle is to use an oxidant (such as O)3，H2O2Etc.) generate radicals having strong oxidizing properties (e.g..OH, etc.) to oxidize organic substances into small molecular compounds and even completely mineralize the small molecular compounds into harmless substances (such as H)2O、CO2) The technique of (1). Persulfate is a common strong oxidizing agent for advanced oxidation, including Peroxymonosulfate (PMS) and Peroxydisulfate (PDS), which is relatively inexpensive and stable because of its ability to generate hydroxyl radicals.Similar or even higher OH (2.8V) sulfate radical SO4 -.,Has a ratio of.OH (less than 1. mu.s) longer half-life (4s) and, in certain cases, SO4 -.Has higher selectivity and is widely used for in-situ oxidation remediation of water pollution. However, the persulfate is directly thrown into water pollution, which has high cost and limited effect, and needs to be activated to activate an oxidant to generate an active substance ((ii)).OH、SO4 -.Superoxide radical O2 .-Singlet oxygen1O2). The conventional activation modes mainly comprise heat, radiation activation, alkali activation, transition metal and combined activation with carbon materials.
The traditional municipal sludge treatment method comprises dehydration, drying, anaerobic digestion, composting and the like; the disposal modes comprise landfill, sea filling, incineration, carbonization, building material utilization, land utilization and other novel resource utilization technologies, and the like, but researches show that the modes generate huge threats on the ecological environment and the human health to different degrees. The sludge is made into the biochar material in an efficient mode of carrying out reduction, stabilization and harmless treatment on the sludge, and the biochar surface of the sludge subjected to high-temperature pyrolysis contains rich organic functional groups such as carboxyl, phenolic hydroxyl, carbonyl and the like, is highly aromatic and has large specific surface areaThe porous carbon residue has strong material conversion and adsorption capacity, and because of adding the iron coagulant in the municipal sewage treatment, the calcined biochar contains a large amount of transition metal Fe and shows magnetism, and Fe and the carbon material can play an unexpected activation effect on the peroxydisulfate. However, although the raw biochar can be directly used as a general-purpose carbon-based material, the specific surface area and surface chemistry (e.g., defect level and sp) of the carbon material2Hybrid carbon backbone) is limited due to the non-stoichiometric nature of the original biomass. Therefore, researchers change the limitation of the original biochar by carrying out transition metal loading and heteroatom treatment on the carbon material, namely introducing hybridization modes of transition metal, nitrogen, S and the like. However, metal doping inevitably has the risks of metal leaching and passivation of metal in air after long-time exposure, and the activation and regeneration of metal parts requires extra energy cost, which affects the use efficiency and increases the money cost and also causes secondary pollution to the environment. Research shows that the nitrogen-doped biochar material can introduce ordered sp2The hybrid carbon skeleton changes the electrochemical capacity of the original pi electronic network and enhances the adsorption performance of the original carbon material, and can provide higher electrochemical catalytic activity for in-situ chemical remediation of soil and underground water.
In conclusion, the nitrogen-doped sludge biochar material obtained by high-temperature pyrolysis of sludge has rich specific surface area and functional groups, and can efficiently activate peroxydisulfate to generate SO4-.、.OH and1O2when the active substances degrade the organic pollutants, the heavy metal substances are reduced well. This patent aims at carrying out the resourceization to mud, allies oneself with organic pollutant and heavy metal in the removal water of peroxydisulfate efficient.
Disclosure of Invention
The invention aims to solve the problem that nitrogen-doped sludge biochar prepared by high-temperature pyrolysis efficiently activates peroxydisulfate to efficiently and jointly remove organic pollutants and heavy metals in water, and provides a new idea for removing the organic pollutants and the heavy metals in the water.
In order to solve the problems, the technical scheme of the invention is as follows: a method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate is characterized by comprising the following steps:
step 1): taking the sludge back, standing until mud and water are separated, pouring out supernatant, filtering the sludge, drying until the sludge is constant in weight, mixing the sludge with nitrogenous organic matters, putting the mixture into a tubular furnace for pyrolysis in a nitrogen atmosphere, taking out the mixture, washing the mixture with clear water until the mixture is neutral, and drying the mixture to obtain charcoal;
step 2): adding the biochar and the peroxydisulfate obtained in the step 1) into the sewage containing the organic pollutants and the heavy metals at normal temperature and normal pressure, and continuously stirring the whole system to remove the organic pollutants and the heavy metals in the sewage.
Preferably, the sludge in the step 1) is excess sludge in secondary sedimentation tank sludge of a sewage treatment plant; the nitrogen-containing organic matter is at least one of dicyandiamide, urea and melamine.
Preferably, the sludge in the step 1) is ground into powder and then mixed with the nitrogen-containing organic matter, and the mass ratio of the sludge to the nitrogen-containing organic matter is 1: 1-1: 3.
Preferably, the biochar obtained in the step 1) is dried, ground into powder and sieved by a 200-mesh sieve.
Preferably, the temperature for drying the sludge in the step 1) is 105 ℃; the pyrolysis is specifically as follows: introducing nitrogen for 20min to ensure the inert gas atmosphere in the tubular furnace, and then heating from room temperature to 800-1000 ℃ at the heating rate of 10 ℃/min, wherein the pyrolysis time is 2 h.
Preferably, the organic pollutants in the sewage are fluoroquinolone organic matters, and the heavy metal is chromium or/and antimony.
Preferably, the peroxydisulfate in step 2) is at least one of sodium peroxydisulfate and potassium peroxydisulfate.
Preferably, the system in the step 2) is adjusted by using a pH regulator, wherein the treatment condition of the organic pollutants is neutral or alkaline condition, and the treatment condition of the heavy metals is acidic condition.
More preferably, the pH regulator is 10mmol/L phosphate buffer solution.
Preferably, the adding amount of the biochar in the step 2) is 2g/L, and the adding amount of the peroxydisulfate is 0.4-2 mmol/L; the concentration of organic pollutants in the sewage is 20-50 mg/L, and the concentration of heavy metals is 1-10 mg/L. The amount of peroxodisulfate added is preferably 1 mmol/L; the concentration of the organic pollutants in the sewage is preferably 20mg/L, and the concentration of the heavy metals is preferably 1.4 mg/L.
The invention provides a method for jointly removing organic pollutants and heavy metals, which can be widely used for treating water bodies polluted by the organic pollutants and the heavy metals.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method has low technical cost, can jointly remove most organic pollutants and heavy metals in the polluted water body, and has high degradation speed and obvious removal effect.
(2) The invention realizes the removal of organic pollutants and heavy metals by combining the peroxodisulfate which has low price, stable property and easy transportation as an oxidant while recycling the sludge, and has higher value in the actual engineering application.
(3) Different from other Fenton reactions, the Fenton reaction has obvious effect under an acidic condition, has good removal effect on organic pollutants and heavy metals under neutral and alkaline conditions, has the best removal effect under the neutral condition, and can be efficiently used for actual wastewater treatment.
Drawings
FIG. 1 is a graph of removing enrofloxacin by using 2g/L of nitrogen-doped sludge biochar at a ratio of 0: 1-3: 1 and 1mM PDS in a combined manner;
FIG. 2 is a graph of enrofloxacin depletion with 1mM PDS, 2 g/L2N-BC and a combination thereof;
FIG. 3 is a graph of removal of enrofloxacin at different pH levels using 2 g/L2N-BC and 1mM PDS in combination.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
Method for removing organic pollutants and heavy metals in water by combining nitrogen-doped pyrolytic sludge biochar and peroxydisulfate
Respectively adding 20mg/L enrofloxacin into 4 parts of simulated water bodies containing 1.4mg/L chromium and antimony, adjusting the pH value of the system to be 7 by using a phosphate buffer solution, respectively adding 1mM PDS and nitrogen-doped sludge materials with dicyandiamide and sludge biochar doping ratio of 0: 1-3: 1, placing the materials into a magnetic stirrer for reaction, respectively sampling nitrogen for 0min, 1 min, 2 min, 5 min, 10 min, 15 min, 20min and 30min, observing the degradation condition of organic pollutants by using HPLC, and observing the removal condition of heavy metals by using 0min nitrogen and 30mi nitrogen in ICP-MS. After the reaction is found out for 30min, the combination of the nitrogen-doped sludge biochar material and the peroxydisulfate greatly accelerates the reaction rate of organic matters and heavy metals, and the removal effect of enrofloxacin and heavy metals can reach 100 percent. The specific removal effect of organic pollutants is shown in figure 1.
Example 2
Method for removing organic pollutants and heavy metals in water by combining nitrogen-doped pyrolytic sludge biochar and peroxydisulfate
Respectively adding 20mg/L enrofloxacin into 3 parts of simulated water bodies respectively containing 1.4mg/L chromium and antimony, adjusting the pH value of the system to be 7 by using a phosphate buffer solution, respectively adding 1mM PDS, 2 g/L2 nitrogen-BC, 2g/L BC and 5mM PDS, placing the mixture into a magnetic stirrer, placing the mixture into the magnetic stirrer to react, respectively sampling at 0, 1, 2, 5, 10, 15, 20 and 30mi nitrogen, observing the degradation condition of organic pollutants by HPLC, and observing the removal condition of heavy metals by ICP-MS at 0 and 30mi nitrogen. The reaction finds that the single PDS has no obvious removal effect on the enrofloxacin and the heavy metals, the single nitrogen-doped sludge biochar has good adsorption performance on the organic pollutants and the heavy metals, the combination of the nitrogen-doped sludge biochar and the PDS greatly accelerates the reaction rate, and the removal rate of the organic pollutants and the heavy metals can reach nearly 100%. The specific removal effect of organic contaminants is shown in fig. 2.
Example 3
Method for removing organic pollutants and heavy metals in water by combining nitrogen-doped pyrolytic sludge biochar and peroxydisulfate
Respectively adding 20mg/L enrofloxacin into 4 parts of simulated water bodies respectively containing 1.4mg/L chromium and antimony, respectively adjusting the pH value of the solution to 3, 5, 7 and 9 by using a phosphate buffer solution, respectively adding 2 g/L2 nitrogen-BC and 1mM PDS into the simulated water bodies, placing the simulated water bodies in a magnetic stirrer for reaction, respectively sampling at 0, 1, 2, 5, 10, 15, 20 and 30mi nitrogen, observing organic pollutants by HPLC, and observing the removal condition of heavy metals by ICP-MS at the time of 0 and 30mi nitrogen. The reaction finds that the nitrogen-doped sludge biochar has the best effect of removing heavy metals under an acidic condition, the organic matter has the fastest removal efficiency under a neutral condition, and is alkaline, and the removal rate under the acidic condition can still be close to 95%. The specific removal effect of organic contaminants is shown in fig. 3.
Note that: and x nitrogen-BC represents that the doping ratio of dicyandiamide to sludge is x: 1.
Claims (10)
1. A method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate is characterized by comprising the following steps:
step 1): taking the sludge back, standing until mud and water are separated, pouring out supernatant, filtering the sludge, drying until the sludge is constant in weight, mixing the sludge with nitrogenous organic matters, putting the mixture into a tubular furnace for pyrolysis in a nitrogen atmosphere, taking out the mixture, washing the mixture with clear water until the mixture is neutral, and drying the mixture to obtain charcoal;
step 2): adding the biochar and the peroxydisulfate obtained in the step 1) into the sewage containing the organic pollutants and the heavy metals at normal temperature and normal pressure, and continuously stirring the whole system to remove the organic pollutants and the heavy metals in the sewage.
2. The method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate according to claim 1, wherein the sludge in step 1) is excess sludge from secondary sedimentation tank sludge of sewage treatment plants; the nitrogen-containing organic matter is at least one of dicyandiamide, urea and melamine.
3. The method for treating sewage by using the nitrogen-doped sludge biochar and the peroxydisulfate in combination as claimed in claim 1, wherein the sludge in the step 1) is ground into powder and then mixed with nitrogen-containing organic matters, and the mass ratio of the sludge to the nitrogen-doped organic matters is 1: 1-1: 3.
4. The method for treating sewage by using the nitrogen-doped sludge biochar and the peroxydisulfate in combination as claimed in claim 1, wherein the biochar obtained in the step 1) is dried, ground into powder and sieved by a 200-mesh sieve.
5. The method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate according to claim 1, wherein the temperature for drying sludge in the step 1) is 105 ℃; the pyrolysis is specifically as follows: introducing nitrogen for 20min to ensure the inert gas atmosphere in the tubular furnace, and then heating from room temperature to 800-1000 ℃ at the heating rate of 10 ℃/min, wherein the pyrolysis time is 2 h.
6. The method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate as claimed in claim 1, wherein the organic pollutants in the sewage are fluoroquinolone organic matters, and the heavy metals are chromium or/and antimony.
7. The method for treating wastewater using nitrogen-doped sludge biochar in combination with peroxydisulfate according to claim 1, wherein the peroxydisulfate in step 2) is at least one of sodium peroxydisulfate and potassium peroxydisulfate.
8. The method for treating sewage by combining nitrogen-doped sludge biochar and peroxydisulfate according to claim 1, wherein the system in the step 2) is adjusted by a pH regulator, wherein the treatment condition of the organic pollutants is neutral or alkaline condition, and the treatment condition of the heavy metals is acidic condition.
9. The method for treating sewage by using the combination of nitrogen-doped sludge biochar and peroxydisulfate as claimed in claim 8, wherein said pH regulator is 10mmol/L phosphate buffer solution.
10. The method for treating sewage by using the nitrogen-doped sludge biochar and the peroxydisulfate in combination as claimed in claim 1, wherein the adding amount of the biochar in the step 2) is 2g/L, and the adding amount of the peroxydisulfate is 0.4-2 mmol/L; the concentration of organic pollutants in the sewage is 20-50 mg/L, and the concentration of heavy metals is 1-10 mg/L.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113304770A (en) * | 2021-06-28 | 2021-08-27 | 四川大学 | Method for preparing nitrogen-rich metal catalyst by using nitrogen-modified chromium-containing leather scraps and application of nitrogen-rich metal catalyst |
| CN114433167A (en) * | 2022-02-25 | 2022-05-06 | 天津科技大学 | Preparation and use method of iron-based heterogeneous catalyst |
| CN114768779A (en) * | 2022-04-18 | 2022-07-22 | 武汉理工大学 | Preparation method of nitrogen-doped magnetic iron sludge biochar applied to tetracycline removal in water |
| CN114887663A (en) * | 2022-05-03 | 2022-08-12 | 东华大学 | Catalytic system for generating singlet oxygen and application thereof |
| CN115043479A (en) * | 2022-05-17 | 2022-09-13 | 山西财经大学 | Nitrogen-doped biochar as well as preparation method and application thereof |
| CN115532226A (en) * | 2022-09-29 | 2022-12-30 | 广东工业大学 | Efficient adsorption remover for cadmium ions as well as preparation method and application of efficient adsorption remover |
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| CN113304770A (en) * | 2021-06-28 | 2021-08-27 | 四川大学 | Method for preparing nitrogen-rich metal catalyst by using nitrogen-modified chromium-containing leather scraps and application of nitrogen-rich metal catalyst |
| CN113304770B (en) * | 2021-06-28 | 2022-04-12 | 四川大学 | Method for preparing nitrogen-rich metal catalyst by using nitrogen-modified chromium-containing leather scraps and application of nitrogen-rich metal catalyst |
| CN114433167A (en) * | 2022-02-25 | 2022-05-06 | 天津科技大学 | Preparation and use method of iron-based heterogeneous catalyst |
| CN114433167B (en) * | 2022-02-25 | 2024-04-23 | 天津科技大学 | Preparation and use methods of iron-based heterogeneous catalyst |
| CN114768779A (en) * | 2022-04-18 | 2022-07-22 | 武汉理工大学 | Preparation method of nitrogen-doped magnetic iron sludge biochar applied to tetracycline removal in water |
| CN114887663A (en) * | 2022-05-03 | 2022-08-12 | 东华大学 | Catalytic system for generating singlet oxygen and application thereof |
| CN115043479A (en) * | 2022-05-17 | 2022-09-13 | 山西财经大学 | Nitrogen-doped biochar as well as preparation method and application thereof |
| CN115043479B (en) * | 2022-05-17 | 2024-02-27 | 山西财经大学 | Nitrogen-doped biochar as well as preparation method and application thereof |
| CN115532226A (en) * | 2022-09-29 | 2022-12-30 | 广东工业大学 | Efficient adsorption remover for cadmium ions as well as preparation method and application of efficient adsorption remover |
| CN115532226B (en) * | 2022-09-29 | 2023-12-12 | 广东工业大学 | Efficient adsorption remover for cadmium ions and preparation method and application thereof |
| CN115814758A (en) * | 2022-11-15 | 2023-03-21 | 昆明理工大学 | Papermaking sludge biochar, application thereof and method for degrading organic matters |
| CN116139901A (en) * | 2022-11-28 | 2023-05-23 | 武汉理工大学 | Ball milling nitrogen-doped sludge biochar and preparation method and application thereof |
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