CN108373248B - Method for rapidly preparing porous magnetic activated coke based on dewatered sludge - Google Patents
Method for rapidly preparing porous magnetic activated coke based on dewatered sludge Download PDFInfo
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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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- 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
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L5/00—Solid fuels
- C10L5/40—Solid fuels essentially based on materials of non-mineral origin
- C10L5/46—Solid fuels essentially based on materials of non-mineral origin on sewage, house, or town refuse
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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
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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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
- C02F2303/00—Specific treatment goals
- C02F2303/06—Sludge reduction, e.g. by lysis
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Hydrology & Water Resources (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Sludge (AREA)
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Abstract
The invention provides a method for rapidly preparing porous magnetic activated coke based on dewatered sludge, which comprises the steps of air drying the dewatered sludge, and crushing the dried sludge into sludge particles; putting the dried sludge particles into a stainless steel reaction kettle, adding distilled water, sealing, magnetically stirring, heating and reacting; after the reaction is finished, cooling, cleaning and vacuum filtering to obtain a precursor product; immersing the precursor product into an activating agent and a catalyst solution, sealing, soaking, oscillating, vacuum-filtering, drying in air, heating and reacting; then cooling, cleaning and drying to obtain the porous magnetic active coke. The method has the advantages of simple and rapid process, good safety, mild reaction and low energy consumption, and the obtained active coke has a developed pore structure, good magnetism, is easy to recover and regenerate for reuse, can be widely applied to treatment of wastewater and waste gas, greatly expands the field of sludge resource utilization, and has obvious economic benefit and environmental benefit.
Description
Technical Field
The invention belongs to the technical field of waste recycling, and particularly relates to a method for quickly preparing porous magnetic activated coke based on dewatered sludge.
Background
According to statistics, the yield of excess sludge in 2016 urban sewage treatment in China is up to 4300 ten thousand tons (the water content is 80%), and the main treatment methods in the current stage comprise aerobic/anaerobic digestion, dehydration, drying and incineration, sanitary landfill and the like. However, the sludge production amount in China is huge, and the treatment capacity at the present stage is seriously insufficient, so that the safe treatment and disposal of the sludge become one of the environmental problems which are urgently needed to be solved in China, and the ecological environment safety and the human health are directly influenced.
In recent years, many researches and applications have been made on the aspects of harmlessness and reduction of excess sludge in sewage treatment, such as anaerobic/aerobic digestion of sludge, thermochemical hydrolysis, ultrasonic disintegration, microwave treatment, advanced oxidation technology and the like, but the research on the aspect of sludge resource utilization technology is relatively less. The hydrothermal carbonization technology is adopted to study the dewatering and reduction efficiency of the biological sludge in the earlier stage of the subject group of the applicant, and the discovery shows that the conversion of the biological sludge into the hydrothermal coke is a feasible resource-based way, the heat value can reach 15-18MJ/kg, and the biological sludge can be used as a derived solid fuel (patent No. ZL 201410143389.5). Nevertheless, because of its small specific surface area, it is difficult to use as an adsorbent in heavy metal and organic contaminated wastewater treatment, thereby limiting its resource utilization. Therefore, the method researches and expands the field of sludge resource utilization, develops a preparation technology of the porous structure magnetic activated coke which is rapid, low in consumption and easy to recover, and has important significance and application value for sludge reduction and resource additional value improvement.
Disclosure of Invention
The technical problem to be solved by the invention is how to prepare the magnetic active coke with a developed pore structure.
In order to solve the technical problems, the technical scheme of the invention is to provide a method for quickly preparing porous magnetic activated coke based on dewatered sludge, which is characterized by comprising the following steps:
step 1: air-drying the dewatered sludge, and crushing the dewatered sludge into sludge particles; putting the dried sludge particles into a stainless steel reaction kettle, adding distilled water, sealing, magnetically stirring, heating and reacting; after the reaction is finished, cooling, cleaning and vacuum filtering to obtain a precursor product;
step 2: immersing the precursor product prepared in the step 1 into an activating agent and a catalyst solution, sealing, soaking, oscillating, vacuum-filtering, drying by air, heating and reacting; then cooling, cleaning and drying to obtain the porous magnetic active coke.
Preferably, in the step 1, the water content of the dewatered sludge is 60-80%.
Preferably, in the step 1, the diameter of the sludge particles is 1-3 mm.
Preferably, in the step 1, the mass ratio of the dewatered sludge to the distilled water is 0.2-3.0.
Preferably, in the step 1, the magnetic stirring speed is 500-.
Preferably, in the step 1, the reaction is carried out for 0.5-2h after heating to 160-260 ℃.
Preferably, in the step 1, the cleaning comprises hydrochloric acid washing, ethanol or acetone soaking and distilled water washing, wherein the hydrochloric acid concentration is 0.1-0.5mol/L, and the volume fraction of ethanol or acetone is 50% -85%.
Preferably, in the step 2, the activating agent is zinc chloride, potassium hydroxide, potassium carbonate, phosphoric acid or sodium dihydrogen phosphate; the mass ratio of the activating agent to the dewatered sludge is 0.05-0.20.
Preferably, in the step 2, the catalyst is nascent ferric hydroxide or ferrous hydroxide; the mass ratio of the catalyst to the dewatered sludge is 0.1-0.5.
Preferably, in the step 2, the sealed soaking is performed for 2-8h, and the oscillation rate is 100-300 r/min; air drying and reacting at 500-700 deg.c for 30-120 min.
The magnetic active coke prepared by the invention can be used as an adsorbent for treating waste water and waste gas, an advanced oxidation free radical activator and a solid fuel.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation process method is simple and rapid, has good safety, mild reaction and low energy consumption, the obtained active coke has developed pore structure and good magnetism, overcomes the defects of small specific surface area and pore volume of hydrothermal coke obtained by single hydrothermal carbonization, is easy to recycle and can be widely applied to treatment of wastewater and waste gas.
(2) The invention utilizes the special physicochemical property and solvation effect of distilled water in a subcritical state to realize the carbonization and forming processes of sludge, not only has lower energy consumption than the traditional pyrolysis method, but also can greatly shorten the reaction time.
(3) The method can not only carry out harmless and reduction treatment on the sludge, but also obtain the magnetic activated coke with a developed pore structure, greatly expands the field of sludge resource utilization, and has obvious economic benefit and environmental benefit.
Detailed Description
The invention will be further illustrated with reference to the following specific examples.
Example 1
Air-drying the dewatered sludge with the water content of 80%, crushing the dewatered sludge into particles with the diameter of about 1mm, putting 5g of the particles into a stainless steel reaction kettle with the volume of 100mL, adding 5mL of distilled water, sealing, controlling the magnetic stirring speed to be 500r/min, heating to 160 ℃ for reaction for 0.5h, after the reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out a solid-liquid mixture obtained by the reaction in a beaker, washing the solid-liquid mixture with 10mL of hydrochloric acid with the concentration of 0.1mol/L, soaking the solid-liquid mixture with 10mL of ethanol with the volume fraction of 85%, washing the solid-liquid mixture with 50mL of distilled water, carrying out vacuum filtration, and finally weighing to obtain 2.9g of precursor product.
Weighing 2.5g of the precursor product obtained in the previous step into a conical flask filled with 50mL of distilled water, then respectively adding 0.5g of nascent state ferric hydroxide and 0.25g of zinc chloride, sealing, soaking and oscillating at the speed of 100r/min for 2h, then carrying out vacuum filtration, reacting at 500 ℃ for 30min after air drying, cooling to room temperature, washing with 10mL of hydrochloric acid with the concentration of 0.1mol/L and 10mL of distilled water, and then drying at 105 ℃ for 24h to obtain the porous magnetic active coke. The heat value of the active coke is 14.6MJ/kg and the specific surface area is 167m2The saturation magnetization is 6.58emu/g, and the saturation adsorption capacity of the magnetic material to tetracycline antibiotics in water can reach 52.7 mg/g.
Example 2
Air-drying dehydrated sludge with the water content of 60%, crushing the dehydrated sludge into particles with the diameter of about 3mm, putting 10g of the particles into a 100mL stainless steel reaction kettle, adding 20mL distilled water, sealing, controlling the magnetic stirring speed to be 800r/min, heating to 260 ℃ for reaction for 2h, naturally cooling the reaction kettle to room temperature after the reaction is finished, pouring out a solid-liquid mixture obtained by the reaction in a beaker, washing the solid-liquid mixture with 20mL hydrochloric acid with the concentration of 0.1mol/L, soaking the solid-liquid mixture with 20mL acetone with the volume fraction of 50%, washing the solid-liquid mixture with 40mL distilled water, vacuum-filtering, and weighing to obtain 4.5g of precursor product.
Weighing 2.5g of the obtained precursor product into a conical flask filled with 50mL of distilled water, then respectively adding 0.25g of nascent state ferrous hydroxide and 0.75g of potassium hydroxide, sealing, soaking and oscillating at the speed of 300r/min for 8h, then carrying out vacuum filtration, reacting at 700 ℃ for 120min after air drying, cooling to room temperature, washing with 10mL of hydrochloric acid with the concentration of 0.1mol/L and 10mL of distilled water, and then drying at 105 ℃ for 24h to obtain the porous magnetic active coke. The heat value of the active coke is measured to be 18.6MJ/kg, and the specific surface area is 421m2The saturation magnetization is 7.08emu/g, and the saturation adsorption capacity of the magnetic material to tetracycline antibiotics in water can reach 98.4 mg/g.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (7)
1. A method for rapidly preparing porous magnetic activated coke based on dewatered sludge is characterized by comprising the following steps:
step 1: air-drying the dewatered sludge, and crushing the dewatered sludge into sludge particles; putting the dried sludge particles into a stainless steel reaction kettle, adding distilled water, sealing, magnetically stirring, heating and reacting; after the reaction is finished, cooling, cleaning and vacuum filtering to obtain a precursor product; the cleaning sequentially comprises hydrochloric acid washing, ethanol or acetone soaking and distilled water washing, wherein the concentration of hydrochloric acid is 0.1-0.5mol/L, and the volume fraction of ethanol or acetone is 50% -85%;
step 2: immersing the precursor product prepared in the step 1 into an activating agent and a catalyst solution, sealing, soaking, oscillating, vacuum-filtering, drying by air, heating and reacting; then cooling, cleaning and drying to obtain porous magnetic active coke; the activating agent is zinc chloride, potassium hydroxide, potassium carbonate, phosphoric acid or sodium dihydrogen phosphate; the mass ratio of the activating agent to the dewatered sludge is 0.05-0.20; the catalyst is nascent state ferric hydroxide or ferrous hydroxide; the mass ratio of the catalyst to the dewatered sludge is 0.1-0.5.
2. The method for rapidly preparing the porous magnetic activated coke based on the dewatered sludge as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the water content of the dewatered sludge is 60-80%.
3. The method for rapidly preparing the porous magnetic activated coke based on the dewatered sludge as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the diameter of the sludge particles is 1-3 mm.
4. The method for rapidly preparing the porous magnetic activated coke based on the dewatered sludge as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the mass ratio of the dewatered sludge to the distilled water is 0.2-3.0.
5. The method for rapidly preparing the porous magnetic activated coke based on the dewatered sludge as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the magnetic stirring speed is 500-800 r/min.
6. The method for rapidly preparing the porous magnetic activated coke based on the dewatered sludge as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the reaction is carried out for 0.5-2h after heating to 160-260 ℃.
7. The method for rapidly preparing the porous magnetic activated coke based on the dewatered sludge as claimed in claim 1, wherein the method comprises the following steps: in the step 2, the sealed soaking and the oscillation are carried out for 2 to 8 hours, and the oscillation rate is 100-300 r/min; air drying and reacting at 500-700 deg.c for 30-120 min.
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| CN109876770A (en) * | 2019-03-13 | 2019-06-14 | 重庆大学 | The preparation method and application of magnetic hydro-thermal carbon adsorbent |
| CN110577219A (en) * | 2019-09-29 | 2019-12-17 | 南京工程学院 | Magnetic sludge straw-based activated carbon and preparation method thereof |
| CN113251422B (en) * | 2021-06-21 | 2022-02-15 | 中国环境科学研究院 | Non-pollution low-energy-consumption garbage recycling treatment method and system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103521180A (en) * | 2013-09-29 | 2014-01-22 | 福建工程学院 | Method for preparing sludge-based formed magnetic active carbon |
| CN106744952A (en) * | 2016-11-29 | 2017-05-31 | 中冶华天南京工程技术有限公司 | The method that sewage sludge prepares modified active coke |
| CN107572524A (en) * | 2017-09-15 | 2018-01-12 | 华中科技大学 | A kind of method that activated carbon is prepared using sludge |
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| KR20150001001A (en) * | 2013-06-26 | 2015-01-06 | 대전대학교 산학협력단 | Adsorption Characteristics of H2S on Adsorbent Made by Drinking Water Treatment Sludge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103521180A (en) * | 2013-09-29 | 2014-01-22 | 福建工程学院 | Method for preparing sludge-based formed magnetic active carbon |
| CN106744952A (en) * | 2016-11-29 | 2017-05-31 | 中冶华天南京工程技术有限公司 | The method that sewage sludge prepares modified active coke |
| CN107572524A (en) * | 2017-09-15 | 2018-01-12 | 华中科技大学 | A kind of method that activated carbon is prepared using sludge |
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