CN113845286A - Method for co-pyrolysis of oil-containing sludge and aluminum slag - Google Patents

Method for co-pyrolysis of oil-containing sludge and aluminum slag Download PDF

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Publication number
CN113845286A
CN113845286A CN202111251246.2A CN202111251246A CN113845286A CN 113845286 A CN113845286 A CN 113845286A CN 202111251246 A CN202111251246 A CN 202111251246A CN 113845286 A CN113845286 A CN 113845286A
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pyrolysis
aluminum slag
oil
slag
aluminum
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赵慧慧
刘军
戴昕
郭燕
冉根柱
潘天琪
李钦钦
刘淦源
洪有成
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Nanjing Wondux Environmental Protection Technology Co ltd
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Nanjing Wondux Environmental Protection Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/10Treatment of sludge; Devices therefor by pyrolysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/318Preparation characterised by the starting materials
    • C01B32/324Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/40Valorisation of by-products of wastewater, sewage or sludge processing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Water Supply & Treatment (AREA)
  • Composite Materials (AREA)
  • Geology (AREA)
  • Hydrology & Water Resources (AREA)
  • Manufacturing & Machinery (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention provides a method for the collaborative pyrolysis of oil-containing sludge and aluminum slag, which comprises six steps of material crushing, component compounding, ventilation and exhaust, high-temperature pyrolysis, condensation and separation and residue resource utilization, wherein the pyrolysis efficiency of the oil-containing sludge is improved by utilizing the catalytic action of the aluminum slag, the effective components in the oil-containing sludge and the aluminum slag are fully excavated, and activated carbon nano aluminum oxide is prepared by using activated pyrolysis residues. The method realizes the cooperative pyrolysis treatment of the oily sludge and the aluminum slag, improves the pyrolysis efficiency of the oily sludge and the resource utilization efficiency of the aluminum slag, realizes the cooperative pyrolysis treatment of the oily sludge and the aluminum slag, and has wide application prospect.

Description

Method for co-pyrolysis of oil-containing sludge and aluminum slag
Technical Field
The invention belongs to the field of solid waste disposal, and particularly relates to a method for the collaborative pyrolysis of oil-containing sludge and aluminum slag.
Background
The aluminum slag and the oily sludge are solid wastes generated in energy chemical industries such as petrochemical industry, metallurgy and the like, and are stacked or buried in the open air for a long time, so that heavy metal elements and toxic substances in the solid wastes enter soil to pollute crops, and the food safety and the health safety of people are finally influenced through continuous enrichment.
The source, sludge composition and properties of the oily sludge are different, and thus the disposal of the oily sludge is different. Wherein, the oil-containing sludge pyrolysis is a chemical decomposition thermal reaction process for decomposing the oil-containing sludge into gas, liquid and solid phases under the inert gas atmosphere or the vacuum state. The oily sludge can be recycled by pyrolysis treatment, and the generated combustible gas and pyrolysis oil can be used as energy. In addition, the carbon content in the pyrolysis residue of the oily sludge is sharply reduced by the catalytic action of metallic aluminum, alumina, and the like. The aluminum slag is solid waste generated in the electrolytic smelting process, contains a large amount of toxic heavy metal substances such as aluminum, iron and the like, and can cause soil and water environment to be damaged when being randomly stacked or buried. How to improve the pyrolysis efficiency of the oil-containing sludge by utilizing the catalytic action of the aluminum slag and fully excavate effective components in the oil-containing sludge and the aluminum slag is a problem to be solved urgently.
Disclosure of Invention
Aiming at how to improve the pyrolysis efficiency of the oily sludge by utilizing the catalytic action of the aluminum slag and fully excavate the effective components in the oily sludge and the aluminum slag, the invention provides a method for the collaborative pyrolysis of the oily sludge and the aluminum slag. The invention comprises the following steps:
(1) crushing materials, wherein the material crushing is to crush oily sludge and aluminum slag of the materials respectively to form small particles;
(2) compounding components, wherein the compounding of the components is to add aluminum slag into the oily sludge to form a mixed component;
(3) ventilating and exhausting, wherein after the pyrolysis furnace is sealed, high-purity nitrogen is introduced to exhaust oxygen in the furnace;
(4) performing high-temperature pyrolysis, namely putting the mixed components in a high-temperature oxygen-free environment for calcination and activation, and performing high-temperature pyrolysis on the oily sludge to obtain a pyrolysis product; calcining the aluminum slag at high temperature to form activated aluminum slag;
(5) condensing and separating, namely separating gas and liquid generated by pyrolysis, drying the gas and collecting the gas;
(6) and (3) carrying out resource utilization on the residues, wherein the resource utilization of the residues is to prepare the activated carbon nano-alumina by using the oily sludge and the aluminum residue pyrolysis residues as raw materials.
Further, in the step (1), the crushed particle size of the material is not more than 50 mm.
Further, in the step (2), the components compounded by the components are mixed in a ratio of aluminum slag to sludge containing 1: 3, the mixture is uniformly mixed.
In the step (3), the ventilation and the exhaust are performed in such a way that the inside of the pyrolysis furnace is in an oxygen-insulated environment, and nitrogen is used as a protective gas.
Further, in the step (4), the temperature in the pyrolysis furnace is increased to a corresponding pyrolysis temperature by means of external heating, and the temperature range is 750-900 ℃.
Further, in the step (5), the carrier gas (nitrogen) drives the pyrolysis product to pass through a condensing device, the heavy component is liquefied and enters an oil component collecting bottle, and the gas component enters a gas collecting device through a drying device and is collected.
Further, in the step (6), the step of recycling the residue includes: soaking the activated slag sample in deionized water, and taking supernatant to adjust the pH value to be more than 13 so as to remove iron and silicon in the solution; adding calcium oxide, standing for a period of time, and removing precipitated impurities by centrifugation; adding ammonium bicarbonate solution with the same concentration as the aluminum ions into the filtrate until the solution completely generates white colloidal precipitate, standing the precipitate, sucking out the supernatant, and keeping the colloidal solution uniform; repeatedly pickling the obtained solid slag sample, and drying the slag sample in an oven after pickling; mixing and stirring the dried slag sample after acid cleaning and white colloid, performing solid-liquid separation on the stirred solution by using a screen, retaining the separated solution, drying the loaded slag sample, and calcining for 4 hours in a furnace; and stirring the calcined sample and the filtrate obtained by centrifugation, and repeating the steps to obtain the activated carbon nano aluminum oxide material.
The invention has the beneficial effects that:
according to the invention, through the cooperative treatment of the oily sludge and the aluminum slag, the pyrolysis efficiency of the oily sludge is improved by utilizing the catalytic action of the aluminum slag, the effective components in the oily sludge and the aluminum slag are fully excavated, and the activated carbon nano-alumina is prepared by taking pyrolysis residues as raw materials, so that the cooperative pyrolysis treatment of the oily sludge and the aluminum slag is realized. The invention improves the pyrolysis efficiency of the oily sludge by utilizing the catalytic action of aluminum, realizes the resource utilization of the aluminum slag, and has high energy-saving and environment-friendly benefits.
Drawings
FIG. 1 is a process flow diagram of a method for the co-pyrolysis of oil-containing sludge and aluminum dross.
Detailed Description
The present invention will be further explained with reference to the drawings and examples, and it should be noted that the present embodiment is a detailed description of the technical method of the present invention, and does not limit the technical method of the present invention in any way, and all pyrolysis pretreatment and residue recycling methods in the field and the similar field of the present invention should be protected by the present invention.
Examples
As shown in figure 1, a process flow chart of a method for the synergistic pyrolysis of oil-containing sludge and aluminum slag.
In the embodiment, the oil-containing sludge and the aluminum slag are subjected to synergistic pyrolysis, and the aluminum slag plays a role of a catalyst in a catalytic cracking reaction of the oil-containing sludge, so that the rate of the pyrolysis reaction is greatly increased. The chloride ions in the aluminum slag are extracted by an alkali fusion method, and then the aluminum hydroxide colloid prepared by ammonium bicarbonate is further purified by drying, acid washing, ultrasonic cleaning and the like. The concrete process comprises five steps of material crushing, component compounding, ventilation and exhaust, high-temperature pyrolysis, condensation separation and residue resource utilization, and the concrete steps are as follows.
The oil content of the oily sludge in this example was 30%, the water content was 28%, and the solid content was 35%. Crushing the oily sludge and the aluminum slag to be less than 50mm, uniformly mixing the crushed oily sludge and the aluminum slag according to the mass ratio of 3:1, then feeding the mixed materials into a high-temperature pyrolysis furnace, sealing the high-temperature pyrolysis furnace, introducing high-purity nitrogen into the high-temperature pyrolysis furnace at the speed of 200mL/min for 30min, and heating the high-temperature pyrolysis furnace after exhausting oxygen in the furnace; the furnace temperature is kept at about 750 ℃; the nitrogen drives the pyrolysis product to pass through a condensing device, the heavy component is liquefied and enters an oil content collecting device, and the gas component enters a gas collecting device through a drying device and is collected; and the residues generated by pyrolysis are activated residues and enter a subsequent residue resource utilization system.
Soaking the activated residue in deionized water, stirring for 30min, collecting supernatant, adding a certain amount of sodium hydroxide to adjust pH to be higher than 13, adding 0.01g of calcium oxide, standing for 24 hr, and centrifuging to remove precipitate impurities; adding an ammonium bicarbonate solution with the same concentration as the aluminum ions of the filtrate into the filtrate until the solution completely generates white colloidal precipitate, standing the precipitate, sucking out supernatant, and stirring to keep the colloidal solution uniform; taking the solid residue value generated by pyrolysis, repeatedly pickling with acid liquor, and drying the residue after pickling; then mixing and stirring the residue after acid cleaning and drying with uniform colloid for 1h, then carrying out solid-liquid separation by using a screen, drying the separated residue, then continuously feeding into a pyrolysis furnace, and calcining for 4h at 750 ℃; and stirring the calcined solid and the filtrate obtained by centrifugation, and then repeatedly calcining to obtain the activated carbon nano aluminum oxide material.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.

Claims (7)

1. The method for the collaborative pyrolysis of the oil-containing sludge and the aluminum slag is characterized by comprising the following steps of:
step 1: respectively crushing the oily sludge and the aluminum slag to form small particles;
step 2: adding aluminum slag into the oily sludge to form a mixed component;
and step 3: after the pyrolysis furnace is sealed, high-purity nitrogen is introduced, so that oxygen in the furnace is exhausted;
and 4, step 4: calcining and activating the mixed components in a high-temperature oxygen-free environment in a pyrolysis furnace, pyrolyzing the oily sludge at high temperature to obtain a pyrolysis product, and calcining the aluminum slag at high temperature to form activated aluminum slag;
and 5: the activated carbon nano-alumina is prepared by using oily sludge and aluminum slag pyrolysis residues as raw materials.
2. The method for the co-pyrolysis of the oil-containing sludge and the aluminum slag according to claim 1, wherein in the step 1, the particle size of the small particles is not more than 50 mm.
3. The method for the co-pyrolysis of the oil-containing sludge and the aluminum slag according to claim 1, wherein the ratio of the aluminum slag to the oil-containing sludge in the step 2 is 1: 3, the mixture is uniformly mixed.
4. The method for the synergic pyrolysis of the oil-containing sludge and the aluminum slag as claimed in claim 1, wherein in the step 4, the temperature in the pyrolysis furnace is raised to 750-900 ℃ by means of external heating.
5. The method for the collaborative pyrolysis of the oil-containing sludge and the aluminum slag as claimed in claim 1, wherein in the step 4, the carrier gas generated by the high-temperature pyrolysis drives the pyrolysis product to pass through a condensing device, the heavy component is liquefied and enters an oil collecting bottle, and the gas component passes through a drying device and enters a gas collecting device to be collected.
6. The method for the collaborative pyrolysis of the oil-containing sludge and the aluminum slag according to claim 1, wherein in the step 5, the step of preparing the activated carbon nano alumina comprises the following steps: step 5.1: soaking the pyrolysis residue in deionized water, and taking supernatant to adjust the pH value to be more than 13;
step 5.2: adding calcium oxide into the supernatant, standing for a period of time, and removing precipitated impurities by centrifugation;
step 5.3: 5.2, adding an ammonium bicarbonate solution with the same concentration as the aluminum ions into the filtrate obtained by centrifugation until the solution completely generates white colloidal precipitate, standing the precipitate, sucking out the supernatant, and keeping the colloidal solution uniform;
step 5.4: repeatedly pickling the solid slag sample obtained in the step 5.1, and drying the slag sample in an oven after pickling;
step 5.5: mixing and stirring the dried solid slag sample after acid cleaning and white colloid, performing solid-liquid separation on the stirred solution by using a screen, retaining the separated solution, drying the separated slag sample, and then feeding the slag sample into a pyrolysis furnace for calcination;
step 5.6: and (3) stirring the calcined slag sample and the filtrate obtained by centrifuging in the step 5.5, and repeating the steps to obtain the activated carbon nano aluminum oxide material.
7. The method for the collaborative pyrolysis of the oil-containing sludge and the aluminum slag according to claim 6, wherein in the step 5.5, the calcination time is 4 hours, and the calcination temperature is 750-900 ℃.
CN202111251246.2A 2021-10-27 2021-10-27 Method for co-pyrolysis of oil-containing sludge and aluminum slag Pending CN113845286A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115010337A (en) * 2022-05-19 2022-09-06 中南大学 Oil sludge pyrolysis method
WO2023193419A1 (en) * 2022-04-08 2023-10-12 天津大学 Oil-containing sludge treatment method, soil remediation method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20130045644A (en) * 2011-10-26 2013-05-06 한국에너지기술연구원 A pyrolysis process and its operation method producing fuel oil from plastic materials
CN107117787A (en) * 2017-07-07 2017-09-01 中国石油大学(华东) A kind of process of oily sludge addition microalgae biomass collaboration pyrolysis
CN110724547A (en) * 2019-04-10 2020-01-24 湖南顶立科技有限公司 Method for drying and pyrolyzing sludge and medicine residues cooperatively

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20130045644A (en) * 2011-10-26 2013-05-06 한국에너지기술연구원 A pyrolysis process and its operation method producing fuel oil from plastic materials
CN107117787A (en) * 2017-07-07 2017-09-01 中国石油大学(华东) A kind of process of oily sludge addition microalgae biomass collaboration pyrolysis
CN110724547A (en) * 2019-04-10 2020-01-24 湖南顶立科技有限公司 Method for drying and pyrolyzing sludge and medicine residues cooperatively

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王军: "铝渣和含油污泥协同处理可行性实验研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023193419A1 (en) * 2022-04-08 2023-10-12 天津大学 Oil-containing sludge treatment method, soil remediation method
CN115010337A (en) * 2022-05-19 2022-09-06 中南大学 Oil sludge pyrolysis method
CN115010337B (en) * 2022-05-19 2023-12-22 中南大学 Oil sludge pyrolysis method

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Application publication date: 20211228