CN111039345A - High-added-value resource utilization method of oil sludge pyrolysis slag - Google Patents
High-added-value resource utilization method of oil sludge pyrolysis slag 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
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- C02F11/00—Treatment of sludge; Devices therefor
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- C02F2101/00—Nature of the contaminant
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- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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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
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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Abstract
The invention provides a high-added-value resource utilization method of oil sludge pyrolysis slag, and belongs to the technical field of resource secondary utilization. The method comprises the steps of grinding oil sludge pyrolysis slag, sieving the powder to be below 100 meshes, and then using the powder for heavy metal ion wastewater treatment, stabilization treatment of electroplating sludge and the like. When the wastewater and sludge containing heavy metal ions are treated, the oil sludge pyrolysis residue is added into the heavy metal ion wastewater or sludge, after the constant-temperature oscillation reaction, the filtrate and the residue are obtained through filtration, and the removal rate of the oil sludge pyrolysis residue on the heavy metal ions in the wastewater or sludge, the saturated adsorption capacity of the oil sludge on the heavy metals and the occurrence state of heavy metal adsorption are obtained. The method not only can effectively utilize the oil sludge pyrolysis residue, but also can replace lime and sodium sulfide in the treatment of heavy metal wastewater or sludge, and has wide source and low cost. The method promotes the development of the pyrolysis technology of the oily sludge and the high value-added utilization of the pyrolysis slag, and provides a high-efficiency and low-cost treatment raw material for the treatment of the wastewater or sludge containing heavy metal ions.
Description
Technical Field
The invention relates to the technical field of resource secondary utilization, in particular to a high-added-value resource utilization method of oil sludge pyrolysis slag.
Background
During the processes of oil exploration, exploitation, refining, tank cleaning, storage and transportation, a large amount of oily sludge is generated due to accidents, leakage, natural sedimentation and the like, and the oily sludge is mainly classified into three types, namely ground oil sludge, tank bottom oil sludge and refinery oil sludge. Because the oily sludge contains toxic and harmful substances such as sulfide, benzene series, phenols, anthracene, pyrene and the like, and some hydrocarbon substances contained in the crude oil have carcinogenic, teratogenic and mutagenic effects, the oily sludge in the oil field is listed as dangerous solid waste (HW08) by the state, is incorporated into dangerous waste for management, and must be subjected to harmless treatment and resource utilization according to the requirements of the solid waste pollution environment prevention and control law and the national clean production promotion law.
The developed technologies for harmless treatment of oily sludge include incineration, solidification, landfill, biological composting and the like, which play an important role in the harmless treatment of oily sludge, but secondary environmental pollution is generated by gas and ash generated by incineration, pollutants in solidified bodies are released to the environment again due to rainwater soaking, the problem that the pollutants leak to pollute soil and underground water after landfill still exists, and the risk of secondary pollution is also generated by volatile organic matters generated in the biological composting process. Therefore, the above-mentioned method for the harmless treatment of the oil-containing sludge is not optimal.
The resource utilization of the oily sludge is an important development direction in the future. At present, the resource utilization mainly focuses on the recovery of oil products, such as pyrolysis, solvent extraction, thermochemical cleaning, centrifugation, biological method, ultrasonic method, microwave method, etc. Research shows that pyrolysis is the most promising method for recovering oil from oily sludge because of more recovered oil and less residual residues, but the utilization of pyrolysis residues, residues generated by pyrolysis, is rarely reported. At present, a small amount of the waste cement is used for cooperative disposal of a cement kiln, and almost all the waste cement is subjected to landfill treatment, so that not only is the serious secondary pollution hidden danger existed, but also the waste of resources is caused. Finding a high value-added utilization method of oil sludge pyrolysis slag has become a hot point of interest in the petrochemical industry.
Disclosure of Invention
The invention aims to provide a high-added-value resource utilization method of oil sludge pyrolytic slag, which is used for treating heavy metal ion-containing wastewater (including industrial acid wastewater and mine wastewater) and electroplating sludge. Through the research on the composition and the performance of the oil sludge pyrolytic slag, the oil sludge pyrolytic slag is found to have a porous internal structure, and contains a large amount of S2-The compound has certain alkalinity, and provides a high-added-value resource utilization method for treating wastewater and sludge containing heavy metal ions by using oil sludge pyrolysis slag so as to realize 'treatment of waste by waste'.
Firstly, grinding and sieving oil sludge pyrolysis slag to be below 100 meshes, then adding the treated oil sludge pyrolysis slag into a material to be treated, uniformly stirring and reacting; wherein the materials to be treated comprise heavy metal ion wastewater (including industrial acid wastewater and mine wastewater) and electroplating sludge.
The oil sludge pyrolysis residue is residue obtained after oil products in the oil sludge are recovered by pyrolysis, wherein useful components comprise Fe, S, C, CaO and SiO2、Al2O3The content of the thermal decomposition residue is 23-28%, 15-23%, 18-25%, 10-15%, 8-15% and 8-10% respectively.
After the ground oil sludge pyrolysis slag reaches the required granularity, the ground oil sludge pyrolysis slag is directly added into the material to be treated, and the addition amount is determined according to the properties of different materials.
The utilization method of the oil sludge pyrolysis residue comprises the following steps:
(1) grinding the oil sludge pyrolysis residue, and sieving to 100 meshes (0.15mm) below for later use;
(2) weighing the oil sludge pyrolysis residue prepared in the step (1), adding the oil sludge pyrolysis residue into heavy metal ion wastewater or sludge, placing the mixture in a constant temperature oscillator, carrying out 150 r/m oscillation reaction for a certain time, and filtering to obtain filtrate and residue;
(3) determining the residual concentration of the heavy metal ions in the filtrate obtained in the step (2), and calculating the removal rate of the heavy metal;
(4) and (3) measuring the occurrence state of the heavy metal in the residue obtained in the step (2) by using an XRD and XPS combined measuring method.
Wherein, the oil sludge pyrolysis residue in the step (1) is residue left after oil products are recovered from oil-containing sludge in the petrochemical industry by adopting a pyrolysis technology, has a porous internal structure, and contains a large amount of S2-Compound and has certain alkalinity.
The proportion of the oil sludge pyrolysis residue to the heavy metal ion wastewater or sludge in the step (2) is 0.1-10 g/L.
In the step (2), the heavy metal ions in the heavy metal ion wastewater or sludge comprise Cr (VI), Cd2+、Pb2+、Cu2+、TI3+、Zn2+And the like.
In the step (2), the oscillating temperature is room temperature, and the oscillating reaction time is 30-75 min.
And (4) in the step (3), the removal rate of the heavy metal is (initial heavy metal concentration-residual heavy metal concentration)/initial heavy metal concentration.
The technical scheme of the invention has the following beneficial effects:
according to the scheme, the oily sludge pyrolysis residue in the petrochemical industry is used for replacing lime and sodium sulfide which are commonly used in the existing heavy metal wastewater or sludge treatment in the treatment process, the source is wide, the cost is low, and the wastewater with low heavy metal ion content can be treated. The pyrolysis slag is used for treating the wastewater containing the heavy metal ions, so that the development of the oil-containing sludge pyrolysis technology and the high-added-value resource utilization of the pyrolysis slag can be promoted, and a high-efficiency and low-cost treatment raw material can be provided for the treatment of the wastewater or sludge containing the heavy metal ions.
Drawings
FIG. 1 is a process flow chart of a method for treating heavy metal ion-containing wastewater or sludge by using oil sludge pyrolysis slag in an embodiment of the invention;
fig. 2 is an external view and an internal structure diagram of the oil sludge pyrolytic residue in the embodiment of the invention, wherein (a) is the external view of the oil sludge pyrolytic residue, and (b) is the internal structure.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides a high value-added resource utilization method of oil sludge pyrolysis slag.
Firstly, grinding and sieving oil sludge pyrolysis slag to be below 100 meshes, then adding the treated oil sludge pyrolysis slag into a material to be treated, uniformly stirring and reacting; wherein the materials to be treated comprise heavy metal ion wastewater (including industrial acid wastewater and mine wastewater) and electroplating sludge.
The following description is given with reference to specific examples.
When the treated material is wastewater or sludge containing heavy metal ions, the utilization method is shown in figure 1, and the method comprises the steps of firstly grinding the oil sludge pyrolysis residue and sieving the ground oil sludge pyrolysis residue to be below 100 meshes (0.15mm) for later use; then weighing the prepared oil sludge pyrolysis residue, adding the oil sludge pyrolysis residue into heavy metal ion wastewater or sludge, placing the heavy metal ion wastewater or sludge in a constant temperature oscillator for 150 r/m oscillation reaction for a certain time, and filtering to obtain filtrate and residue; determining the residual concentration of the heavy metal ions in the obtained filtrate, and calculating the removal rate of the heavy metal; and (3) measuring the occurrence state of heavy metals in the obtained residue by adopting an XRD and XPS combined measuring method.
The appearance and internal structure of the sludge pyrolytic slag used in the following examples are shown in fig. 2.
Example 1
Transferring 100ml of wastewater with Cr (VI) concentration of 40mg/L, pH of 2.0 into a 150ml conical flask, adding 0.1g of oil sludge pyrolysis residue, placing the wastewater into a 150 r/m constant-temperature shaking table for oscillation reaction for 60min, taking out and filtering, measuring the concentration and pH of the residual Cr (VI) in the filtrate, obtaining the filtrate with the residual Cr (VI) concentration of 1.8mg/L, pH of 2.3, wherein the removal rate of Cr (VI) is 95.5%, the saturated adsorption quantity of the pyrolysis residue on Cr (VI) is 46.71mg/g, and the Cr (VI) is reduced to Cr (III) on the surface of the pyrolysis residue and generates stable FeCr2O4。
Example 2
100ml of Cd2+Transferring the wastewater with the concentration of 20mg/L, pH of 6.9 into a 150ml conical flask, adding 80mg of oil sludge pyrolysis residue, placing the mixture into a 150 r/m constant-temperature shaking table for oscillation reaction for 60min, taking out and filtering, and measuring the residual Cd in the filtrate2+Concentration and pH to obtain Cd2+The remaining filtrate, Cd, at a concentration of 0.13mg/L, pH of 9.82+The removal rate is 99.35 percent, and the pyrolysis residue is Cd2+The saturated adsorption capacity of (b) is 78.78mg/g, Cd2+Stable CdS and a small amount of CdSiO are generated on the surface of the pyrolysis slag4、Cd(OH)2。
Example 3
100ml of Pb is added2+Transferring the wastewater with the concentration of 10mg/L, pH of 6.8 into a 150ml conical flask, adding 50mg of oil sludge pyrolysis residue, placing the mixture into a 150 r/m constant-temperature shaking table for oscillation reaction for 60min, taking out and filtering, and measuring the residual Pb in the filtrate2+Concentration and pH to obtain Pb2+9.5 filtrate at a residual concentration of 0.23mg/L, pH, Pb2+The removal rate is 97.66 percent, and the pyrolysis residue is Pb2+Has a saturated adsorption amount of 244.5mg/g and Pb2+Stable PbS and a small amount of PbSiO are generated on the surface of the pyrolysis slag4。
Example 4
100ml of Cu2+Transferring the wastewater with the concentration of 40mg/L, pH of 6.2 to a 150ml conical flask, adding 75mg of oil sludge pyrolysis residue, placing the mixture into a 150 r/m constant-temperature shaking table for oscillation reaction for 60min, taking out and filtering, and measuring the residual Cu in the filtrate2+Concentration and pH to obtain Cu2+Filtrate with residual concentration of 0.31mg/L, pH of 7.2, Cu2+The removal rate is 99.23 percent, and the pyrolytic slag is Cu2+Has a saturated adsorption amount of 65.40mg/g and Cu2+Stable CuS and a small amount of CuSiO are generated on the surface of the pyrolysis slag4、Cu(OH)2。
Example 5
100ml of Zn is added2+Transferring the wastewater with the concentration of 40mg/L, pH of 4.2 to a 150ml conical flask, adding 70mg of oil sludge pyrolysis residue, placing the mixture into a constant temperature shaking table with 150 revolutions per minute for oscillation reaction for 60min, taking out the mixture for filtration, and measuring the residual Zn in the filtrate2+Concentration and pH to obtain Zn2+Filtrate with residual concentration of 0.43mg/L, pH of 6.6, Zn2+The removal rate is 98.9 percent, and the pyrolytic slag is Zn2+Has a saturated adsorption amount of 56.33mg/g and Zn2+Stable ZnS and a small amount of ZnSiO are generated on the surface of the pyrolysis slag4、Zn(OH)2。
Example 6
100ml of Cd2+、Pb2+Transferring the wastewater with the concentration of 457.5mg/L and the concentration of 5.95mg/L and the solution pH of 2.0 into a 150ml conical flask, adding 70mg of oil sludge pyrolysis residue, placing the mixture into a 150-rpm constant-temperature shaking table for oscillation reaction for 60min, taking out and filtering, and measuring the residual Cd in the filtrate2+、Pb2+Concentration and pH of filtrate to obtain Cd2+、Pb2+The residual concentrations are 0.07mg/L and 0.19mg/L respectively, the pH of the filtrate is 6.1, and Cd is2+、Pb2+The removal rates were 99.98% and 99.22%, respectively.
Example 7
100ml of TI3+、Cd2+Transferring the wastewater with the concentration of 1.60 and the concentration of 45.27mg/L, pH of 4.4 into a 150ml conical flask, adding 30mg of oil sludge pyrolysis residue, placing the mixture into a constant temperature shaking table with 150 revolutions per minute for oscillation reaction for 60min, taking out the mixture for filtration, and determining the residual TI in the filtrate3+、Cd2+Concentration and pH to obtain TI3+、Cd2+The filtrate, TI, had residual concentrations of 0.24 and 1.43mg/L, pH, respectively, of 7.93+、Cd2+The removal rates were 84.9 and 96.6%, respectively.
Example 8
100ml of TI3+、Cd2+Transferring the wastewater with the concentration of 1.60 and the concentration of 45.27mg/L, pH of 4.4 into a 150ml conical flask, adding 40mg of oil sludge pyrolysis residue, placing the mixture into a constant temperature shaking table with 150 revolutions per minute for oscillation reaction for 60min, taking out the mixture for filtration, and determining the residual TI in the filtrate3+、Cd2+Concentration and pH to obtain TI3+、Cd2+The filtrate with residual concentrations of 0.06 and 0.045mg/L, pH being 8.6 respectively, TI3 +、Cd2+The removal rates were 96.3 and 99.9%, respectively.
Example 9
100ml of Pb is added2+、Zn2+Lead-zinc flotation waste with the concentration of 11.2 and the concentration of 2.8mg/L, pH of 11.4 respectivelyTransferring water to a 150ml conical flask, adding 25mg of oil sludge pyrolytic residue, placing in a 150 r/m constant temperature shaking table for oscillation reaction for 60min, taking out and filtering, and measuring the residual Pb in the filtrate2+、Zn2+Concentration and pH to obtain Pb2+、Zn2+The remaining concentrations were 0.034 and 0.025mg/L, pH, respectively, were 11.8 for the filtrate, Pb2+、Zn2+The removal rates were 99.7 and 99.1%, respectively.
Example 10
Mixing 100ml of Cu2+、Pb2+、Zn2+Transferring the underground copper-lead-zinc mine wastewater with the concentrations of 0.173, 1.142 and 1.582mg/L, pH of 4.5 into a 150ml conical flask, adding 20mg of oil sludge pyrolysis residue, placing the mixture into a 150 r/m constant-temperature shaking table for oscillation reaction for 60min, taking out and filtering, and measuring the residual Cu in the filtrate2+、Pb2+、Zn2+Concentration and pH to obtain Cu2+、Pb2+、Zn2+The residual concentrations of the filtrate and Cu are respectively 0.031, 0.108 and 0.043mg/L, pH which are 5.82+、Pb2+、Zn2+The removal rates were 82.1, 90.5, and 97.3%, respectively.
Example 11
83% of water, Cr (VI) and Zn2+、Ni2+Transferring 100ml of chromium-based electroplating sludge with concentrations of 20.8, 26.6 and 47.8mg/L, pH of 10.0 into a 150ml conical flask, adding 150mg of oil sludge pyrolysis residue, placing into a 150 r/m constant temperature shaking table for oscillation reaction for 60min, taking out, filtering, and measuring the residual Cr (VI) and Zn in the filtrate2+、Ni2+Concentration and pH to obtain Cr (VI), Zn2+、Ni2+The filtrate with the residual concentrations of 4.431, 3.878 and 3.043mg/L, pH of 10.8 respectively, Cr (VI) and Zn2+、Ni2+The removal rates were 78.7, 85.4, and 93.6%, respectively.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A high value-added resource utilization method of oil sludge pyrolysis slag is characterized by comprising the following steps: firstly, grinding and sieving oil sludge pyrolytic slag to be below 100 meshes, then adding the treated oil sludge pyrolytic slag into a material to be treated, uniformly stirring and reacting; wherein the material to be treated comprises wastewater containing heavy metal ions and electroplating sludge.
2. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 1, which is characterized in that: the wastewater containing heavy metal ions comprises industrial acid wastewater and mine wastewater.
3. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 1, which is characterized in that: the oil sludge pyrolysis residue is residue obtained after oil products in the oil sludge are recovered by pyrolysis, wherein useful components comprise Fe, S, C, CaO and SiO2、Al2O3The content of the useful components in the pyrolysis residue is 23-28%, 15-23%, 18-25%, 10-15%, 8-15% and 8-10% respectively.
4. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 1, which is characterized in that: after the ground oil sludge pyrolysis slag reaches the required granularity, the ground oil sludge pyrolysis slag is directly added into the material to be treated, and the addition amount is determined according to the properties of different materials.
5. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 1, which is characterized in that: the method comprises the following steps:
(1) grinding the oil sludge pyrolysis residue, and sieving to be below 100 meshes for later use;
(2) weighing the oil sludge pyrolysis residue prepared in the step (1), adding the oil sludge pyrolysis residue into a material to be treated, placing the material into a constant temperature oscillator, carrying out oscillation reaction at 150 rpm for a certain time, and filtering to obtain filtrate and residue;
(3) determining the residual concentration of the heavy metal ions in the filtrate obtained in the step (2), and calculating the removal rate of the heavy metal;
(4) and (3) measuring the occurrence state of the heavy metal in the residue obtained in the step (2) by using an XRD and XPS combined measuring method.
6. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 5, which is characterized in that: the proportion of the oil sludge pyrolysis residue to the heavy metal ion wastewater or sludge in the step (2) is 0.1-10 g/L.
7. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 5, which is characterized in that: the heavy metal ions contained in the material to be treated in the step (2) comprise Cr (VI), Cd2+、Pb2+、Cu2+、TI3+、Zn2+。
8. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 5, which is characterized in that: the oscillating temperature in the step (2) is room temperature, and the oscillating reaction time is 30-75 min.
9. The high value-added resource utilization method of the oil sludge pyrolysis residue according to claim 5, which is characterized in that: and (4) in the step (3), the removal rate of the heavy metal is (initial heavy metal concentration-residual heavy metal concentration)/initial heavy metal concentration.
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