Method for preparing activated carbon powder using oil sludge

High-performance activated carbon powder was prepared by mixing calcining agent with oil sludge and activating it with red mud and phosphogypsum, which solved the problem of oil sludge resource utilization and achieved efficient oil sludge resource treatment and adsorption effect.

CN116692859BActive Publication Date: 2026-03-31ZHEJIANG HAOYU ECOLOGICAL TECH CO LTD +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-23
Publication Date
2026-03-31

AI Technical Summary

Technical Problem

Existing oil sludge treatment technologies are relatively limited, with generally poor treatment results, and cannot achieve the resource utilization of oil sludge.

Method used

Activated carbon powder is prepared by mixing a calcining agent with oil sludge, then activating the oil sludge with red mud and phosphogypsum, and finally carbonizing it. The specific steps include pre-activation, drying, carbonization, and filtration.

Benefits of technology

High-performance activated carbon powder with large adsorption capacity was prepared, realizing the resource utilization of oil sludge. The COD adsorption capacity was 689 mg/g, the ammonia nitrogen adsorption capacity was 463 mg/g, and the lead adsorption capacity was 35.93 mg/g.

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Abstract

The application relates to the technical field of efficient resource utilization of solid waste, and specifically discloses a method for preparing activated carbon powder from oil sludge, which comprises the following steps: respectively taking calcining agents and oil sludge, mixing and stirring to obtain pre-activated oil sludge; respectively taking red mud, phosphogypsum and the pre-activated oil sludge, mixing and uniformly stirring to obtain activated red oil paste; drying the activated red oil paste to obtain oil paste dry mud; placing the oil paste dry mud in a carbonization furnace for carbonization treatment to obtain first-stage oil sludge coarse carbon; grinding the first-stage oil sludge coarse carbon into powder, mixing, stirring, filtering, drying and obtaining the required high-performance activated carbon powder; the preparation method is simple, the preparation condition is mild, the prepared activated carbon powder has a large adsorption capacity, the maximum adsorption capacity of COD is 689 mg / g, the maximum adsorption capacity of ammonia nitrogen is 463 mg / g, and the maximum adsorption capacity of lead is 35.93 mg / g.
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Description

Technical Field

[0001] This application relates to the field of efficient resource utilization technology of solid waste, and more specifically, it relates to a method for preparing activated carbon powder using oil sludge. Background Technology

[0002] Oil sludge is an oily solid waste generated during oil extraction, transportation, refining, and oily wastewater treatment. It is a type of oily sludge, typically containing 10-40% oil and 20-70% water. Oil sludge has a complex composition, containing not only petroleum-based substances but also toxic compounds such as inorganic salts and heavy metals, posing a serious environmental hazard. Oil sludge dumping not only causes water and air pollution and poisons plants and animals, but also significantly affects the physical and chemical properties of the soil in the dumping area, reducing soil permeability and disrupting the ecological balance.

[0003] Currently, methods for disposing of oily sludge include pyrolysis, coking, incineration, and wet oxidation. Pyrolysis involves heating oily sludge with high oil content to recover gaseous and liquid phase products. Coking primarily targets heavy oil pollutants in oily sludge, achieving effective cracking of heavy oil through condensation and pyrolysis reactions. Incineration directly burns dehydrated oily sludge, reducing its volume. Wet oxidation involves high-temperature, high-pressure oxidation of suspended or dissolved organic matter in the presence of liquid water. These oily sludge disposal technologies are relatively limited, all exhibiting generally poor treatment effects and failing to achieve resource utilization. Given the current underdeveloped technology for oily sludge resource utilization, the research and development of efficient resource utilization technologies for oily sludge is urgently needed. Therefore, this application provides a method for preparing activated carbon powder from oily sludge. Summary of the Invention

[0004] To address the limitations of current oil sludge treatment technologies, their generally poor treatment results, and the inability to achieve resource utilization of oil sludge, this application provides a method for preparing activated carbon powder from oil sludge.

[0005] This application provides a method for preparing activated carbon powder using oil sludge, employing the following technical solution:

[0006] A method for preparing activated carbon powder using oil sludge includes the following steps:

[0007] S1. Weigh out the calcining agent and the sludge separately, mix and stir to obtain pre-activated sludge;

[0008] S2. Weigh out red mud, phosphogypsum and pre-activated oil mud separately, mix them and stir evenly to obtain activated red oil paste;

[0009] S3. Dry the activated red oil paste to obtain dry oil paste mud. Place the dry oil paste mud in a carbonization furnace for carbonization treatment to obtain primary oil mud coarse carbon. Grind the primary oil mud coarse carbon into powder, add water, mix and stir, filter, and dry to obtain the required high-performance activated carbon powder.

[0010] Preferably, the mass ratio of calcining agent to sludge in step S1 is 0.5-5.5:100.

[0011] Preferably, the calcining agent in step S1 is at least one of sodium lauryl sulfate, ammonium fatty alcohol polyoxyethylene ether sulfate, and sodium fatty alcohol polyoxyethylene ether sulfate.

[0012] Preferably, the calcining agent is a compound of sodium lauryl sulfate and sodium fatty alcohol polyoxyethylene ether sulfate in a mass ratio of 1:1.

[0013] Preferably, in step S2, the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge is 0.5-7.5:0.5-5.5:100.

[0014] Preferably, the red mud in step S2 is Bayer process red mud.

[0015] Preferably, the phosphogypsum in step S2 is a solid waste generated in the wet phosphoric acid process, with a particle size of 16-22 μm.

[0016] Preferably, the drying temperature in step S3 is 75-175℃, and the moisture content of the dried oil paste is 5-15%.

[0017] Preferably, the carbonization temperature in step S3 is 350-750℃.

[0018] Preferably, the mixing ratio of water and coarse carbon powder in step S3 is 2-10:1 mL / g.

[0019] By adopting the above technical solution, during the mixing process of the calcining agent and the sludge, the hydrophobic end of the calcining agent dissolves into the oil-based substances of the sludge and is wedged into the sludge, while the hydrophilic end of the calcining agent dissolves in the pore liquid of the sludge, releasing sodium ions, ammonium ions, and hydroxide ions. Red mud and phosphogypsum enhance the flocculation and agglomeration effect of activated sludge through adsorption of free organic matter, hydroxyl bridge trapping and sweeping, and polar double charge layer compression, thus facilitating the subsequent transfer and carbonization of the sludge. During the drying process, the hydrophobic end of the calcining agent wedged into the sludge is guided through inverted wedge-shaped microchannels, while the hydrophilic end promotes mud-water separation through capillary attraction. Furthermore, by increasing the sludge's water secretion, it is beneficial to rapidly reduce the water content in the sludge, achieving rapid drying. During the carbonization process, the calcining agent releases... Sodium ions, ammonium ions, and hydroxide ions, along with aluminosilicates and metal cations in red mud, and phosphates, sulfates, fluorides, and chlorides in phosphogypsum, work synergistically to promote the scission of carbon chains in high-carbon chains and benzene ring-based oil-based substances in the sludge, as well as catalytic deoxygenation and hydrogenation, thus achieving rapid carbonization of the sludge. Simultaneous carbonization of the calcining agent during the carbonization process facilitates the rapid formation of pores and cracks in the carbonization products of the sludge. Simultaneously, under the carbonization environment, red mud, phosphogypsum, and pre-activated sludge react with each other. Under carbothermic chlorination, gases such as aluminum chloride, silicon chloride, and ferric chloride are released from the red mud and phosphogypsum, and sulfates, phosphates, and aluminosilicates are melted out. These substances are then incorporated into the carbon-based materials through gas-phase precipitation, crystal fusion, and electrochemical corrosion.

[0020] In summary, this application has the following beneficial effects:

[0021] This application obtains the desired high-performance activated carbon powder by pre-activating it with a calcining agent, activating it with red mud and phosphogypsum, then drying and grinding the activated red mud paste, mixing it with water, filtering it, and drying it again. The preparation method of this application is simple and the preparation conditions are mild. The prepared activated carbon powder has a large adsorption capacity, and the maximum adsorption capacity achieved is 689 mg / g for COD, 463 mg / g for ammonia nitrogen, and 35.93 mg / g for lead. Attached Figure Description

[0022] Figure 1 This is a process flow diagram of a method for preparing activated carbon powder using oil sludge proposed in this application. Detailed Implementation

[0023] The present application will be further explained below with reference to specific embodiments.

[0024] This application provides a specific method for preparing activated carbon powder using oily sludge, wherein the oily sludge has an oil content of 32% and a water content of 51%; the red mud is Bayer process red mud, which, by mass percentage, includes the following main chemical components: Al2O3 18.4%, SiO2 38.2%, Fe2O3 21.8%, CaO 2.4%, Na2O 9.5%, K2O 0.8%, MgO 3.1%, TiO2 5.5%, and other components 0.3%; the phosphogypsum is a solid waste generated in the wet process of phosphoric acid, with a particle size of 20μm.

[0025] Examples 1-9 verified the effect of the mass ratio of calcining agent to sludge on the performance of the prepared activated carbon powder.

[0026] Example 1

[0027] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0028] The calcining agent and oil sludge were weighed out at a mass ratio of 0.25:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0029] Example 2

[0030] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0031] The calcining agent and oil sludge were weighed out at a mass ratio of 0.3:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0032] Example 3

[0033] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0034] The calcining agent and oil sludge were weighed out at a mass ratio of 0.4:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0035] Example 4

[0036] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0037] The calcining agent and oil sludge were weighed out at a mass ratio of 0.5:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0038] Example 5

[0039] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0040] The calcining agent and oil sludge were weighed out at a mass ratio of 3:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0041] Example 6

[0042] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0043] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0044] Example 7

[0045] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0046] The calcining agent and oil sludge were weighed out at a mass ratio of 6:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0047] Example 8

[0048] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0049] The calcining agent and oil sludge were weighed out at a mass ratio of 6.5:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0050] Example 9

[0051] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0052] The calcining agent and oil sludge were weighed out at a mass ratio of 7:100, mixed, and stirred for 0.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 5% moisture content at 75℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 2:1mL / g, stirred for 0.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0053] The high-performance activated carbon powder prepared in Examples 1-9 of this application was used to adsorb landfill leachate, and the performance parameters are shown in Table 1.

[0054] The leachate from this application was taken from a municipal solid waste sanitary landfill in Lianyungang City. The COD concentration of this batch of leachate was 1206 mg / L, the ammonia nitrogen concentration was 967 mg / L, and the heavy metal ion content was 24 mg / L for lead ions (Pb). 2 + ).

[0055] Adsorption test: Weigh 0.1g of activated carbon powder and mix it into 250mL of landfill leachate. Stir at 120rpm for 0.5 hours and centrifuge at 5000rpm for 5 minutes to obtain supernatant and separation slurry. The supernatant is used to detect pollutant concentration.

[0056] COD Concentration Detection and COD Adsorption Capacity Calculation: The concentration of chemical oxygen demand (COD) in landfill leachate and supernatant was determined according to the national standard "Determination of Chemical Oxygen Demand in Water - Dichromate Method" (GB 11914-1989); the COD adsorption capacity was calculated according to formula (1), where Q... COD COD adsorption capacity (mg / g), c0 and c t V represents the COD concentration (mg / L) in the landfill leachate and supernatant, respectively, V is the solution volume (L), and m is the mass of activated carbon (g).

[0057]

[0058] Ammonia nitrogen concentration detection and ammonia nitrogen adsorption capacity calculation: The concentration of ammonia nitrogen in landfill leachate and supernatant was determined according to the "Determination of Ammonia Nitrogen in Water Quality - Salicylic Acid Spectrophotometric Method" (HJ536-2009); the ammonia nitrogen adsorption capacity was calculated according to formula (2), where Q N c is the ammonia nitrogen adsorption capacity (mg / g). N0 and c Nt The initial concentrations of ammonia nitrogen in the landfill leachate and supernatant are (mg / L), respectively. V is the solution volume in L, and m is the mass of activated carbon in g.

[0059]

[0060] Heavy metal ion concentration detection and adsorption capacity calculation: The lead concentration in landfill leachate and supernatant was determined according to the "Determination of 32 Elements in Water Quality by Inductively Coupled Plasma Atomic Emission Spectrometry" (HJ 776-2015). The adsorption capacity of heavy metal Pb ions was calculated according to formula (3), where Q Pb The adsorption capacity of heavy metals (mg / g), c Pb0 and c Pbt The values ​​are the initial concentrations (mg / L) of heavy metal Pb ions in the landfill leachate and supernatant, respectively, where V is the solution volume in L and m is the mass of activated carbon in g.

[0061]

[0062] The experimental results are shown in Table 1.

[0063] Table 1. Effect of the mass ratio of calcining agent to sludge on the performance of the prepared activated carbon.

[0064]

[0065]

[0066] As shown in Table 1, when the mass ratio of calcining agent to sludge is less than 0.5:100 (as shown in Table 1, when the mass ratio of calcining agent to sludge is 0.4:100, 0.3:100, 0.25:100, and even lower ratios not listed in Table 1), the amount of calcining agent added is relatively small, resulting in reduced dehydration and carbonization performance of the sludge. Consequently, the adsorption capacity of the prepared activated carbon for COD, ammonia nitrogen, and lead decreases significantly as the mass ratio of calcining agent to sludge decreases. When the mass ratio of calcining agent to sludge is equal to 0.5-5.5:100 (as shown in Table 1, when the mass ratio of calcining agent to sludge is 0.5:100, 3:100, and 5.5:100), during the mixing process of the calcining agent and sludge, the hydrophobic end of the calcining agent dissolves into the oil-based substances of the sludge and weds into the sludge, while the hydrophilic end of the calcining agent dissolves in the pore fluid of the sludge, releasing sodium ions, ammonium ions, and hydroxide ions. During the drying process, the hydrophobic end of the calcining agent, embedded in the sludge, promotes mud-water separation through the inverted wedge-shaped microchannels and the capillary attraction of the hydrophilic end. This also increases water exudation from the sludge, thus rapidly reducing its moisture content and achieving rapid drying. Simultaneous carbonization of the calcining agent during the carbonization process facilitates the rapid formation of pores and cracks in the carbonization products of the sludge. Ultimately, the prepared activated carbon exhibited COD adsorption capacities greater than 645 mg / g, ammonia nitrogen adsorption capacities greater than 452 mg / g, and lead adsorption capacities greater than 28 mg / g. When the mass ratio of calcining agent to sludge was greater than 5.5:100 (as shown in Table 1, when the mass ratio of calcining agent to sludge was 6:100, 6.5:100, 7:100, and higher ratios not listed in Table 1), excessive calcining agent was added. This led to an imbalance in the reactions among the materials during the carbonization process, resulting in a significant decrease in the adsorption capacities of the prepared activated carbon for COD, ammonia nitrogen, and lead as the mass ratio of calcining agent to sludge further increased. Therefore, considering both benefits and costs, a mass ratio of calcining agent to sludge of 0.5-5.5:100 is most conducive to improving the adsorption performance of activated carbon powder prepared from sludge.

[0067] Examples 10-30 verified the effect of the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge on the performance of the prepared activated carbon.

[0068] Example 10

[0069] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0070] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.25:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0071] Example 11

[0072] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0073] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.3:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0074] Example 12

[0075] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0076] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.4:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0077] Example 13

[0078] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0079] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.25:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0080] Example 14

[0081] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0082] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.3:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0083] Example 15

[0084] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0085] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.4:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0086] Example 16

[0087] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0088] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0089] Example 17

[0090] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0091] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 4:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0092] Example 18

[0093] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0094] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:0.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, and mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0095] Example 19

[0096] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0097] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:3:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, and mixed with water at a ratio of 6:1 mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0098] Example 20

[0099] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0100] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 4:3:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1 mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0101] Example 21

[0102] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0103] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:3:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0104] Example 22

[0105] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0106] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 0.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, and mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0107] Example 23

[0108] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0109] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 4:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0110] Example 24

[0111] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0112] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0113] Example 25

[0114] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0115] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 8:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0116] Example 26

[0117] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0118] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 8.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0119] Example 27

[0120] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0121] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 9:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1 mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0122] Example 28

[0123] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0124] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:6:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1 mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0125] Example 29

[0126] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0127] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:6.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0128] Example 30

[0129] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0130] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 2.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:7:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 10% moisture content at 125℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 6:1mL / g, stirred for 0.75 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0131] The high-performance activated carbon powder prepared in Examples 10-30 of this application was used to adsorb landfill leachate (adsorption test, COD concentration detection and COD adsorption capacity calculation, ammonia nitrogen concentration detection and ammonia nitrogen adsorption capacity calculation, heavy metal ion concentration detection and adsorption capacity calculation are the same as in Examples 1-9), and the performance parameters are shown in Table 2.

[0132] Table 2. Effect of the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge on the performance of the prepared activated carbon.

[0133]

[0134]

[0135] As shown in Table 2, when the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge is less than 0.5:0.5:100 (as shown in Table 2, when the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge is 0.5:0.4:100, 0.5:0.3:100, 0.5:0.25:100, 0.4:0.5:100, 0.3:0.5:100, 0.25:0.5:100, and even lower ratios not listed in Table 2), the amount of red mud and phosphogypsum added is relatively small, and the flocculation, agglomeration, and carbonization effects of the oil sludge become worse. As a result, the adsorption capacity of the prepared activated carbon for COD, ammonia nitrogen, and lead decreases significantly as the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge decreases. When the mass ratio of red mud, phosphogypsum, and pre-activated sludge is equal to 0.5-7.5:0.5-5.5:100 (as shown in Table 2, where the mass ratios of red mud, phosphogypsum, and pre-activated sludge are 0.5:0.5:100, 4:0.5:100, 7.5:0.5:100, 0.5:3:100, 4:3:100, 7.5:3:100, 0.5:5.5:100, 4:5.5:100, and 7.5:5.5:100), during the carbonization process, the sodium ions, ammonium ions, and hydroxide ions released by the calcining agent, the aluminosilicates and metal cations contained in the red mud, and the phosphates, sulfates, fluorides, and chlorides in the phosphogypsum synergistically promote the scission of carbon chains in high-carbon chains and benzene ring oil-based substances in the sludge and catalytic deoxygenation and hydrogenation, thereby achieving rapid carbonization of the sludge. Simultaneously, under carbonization conditions, red mud, phosphogypsum, and pre-activated sludge react with each other. Under carbothermic chlorination, gases such as aluminum chloride, silicon chloride, and ferric chloride are released from the red mud and phosphogypsum, along with sulfates, phosphates, and aluminosilicates. These substances are incorporated into the carbon-based materials through gas-phase precipitation, crystal fusion, and electrochemical corrosion. Ultimately, the prepared activated carbon exhibits COD adsorption capacities greater than 667 mg / g, ammonia nitrogen adsorption capacities greater than 457 mg / g, and lead adsorption capacities greater than 32 mg / g. When the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge is greater than 7.5:5.5:100 (as shown in Table 2, where the mass ratios are 8:5.5:100, 8.5:5.5:100, 9:5.5:100, 7.5:6:100, 7.5:6.5:100, 7.5:7:100, and higher ratios not listed in Table 2), excessive addition of red mud and phosphogypsum leads to an imbalance in the reactions among the materials during the carbonization process. This results in a significant decrease in the adsorption capacity of the prepared activated carbon for COD, ammonia nitrogen, and lead as the mass ratio of red mud, phosphogypsum, and pre-activated oil sludge further increases. Therefore, considering both efficiency and cost, a mass ratio of red mud, phosphogypsum, and pre-activated oil sludge of 0.5-7.5:0.5-5.5:100 is most beneficial for improving the adsorption performance of activated carbon powder prepared using oil sludge.

[0136] Examples 31-39 verified the effect of carbonization temperature on the performance of the prepared activated carbon.

[0137] Example 31

[0138] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0139] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 15% moisture content at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 275℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0140] Example 32

[0141] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0142] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to a moisture content of 15% at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 300℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0143] Example 33

[0144] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0145] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 15% moisture content at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 325℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0146] Example 34

[0147] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0148] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 15% moisture content at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 350℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0149] Example 35

[0150] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0151] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to a moisture content of 15% at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 550℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0152] Example 36

[0153] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0154] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to a moisture content of 15% at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 750℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0155] Example 37

[0156] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0157] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 15% moisture content at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 775℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0158] Example 38

[0159] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0160] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to a moisture content of 15% at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 800℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0161] Example 39

[0162] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0163] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to a moisture content of 15% at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 825℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0164] The high-performance activated carbon powder prepared in Examples 31-39 of this application was used to adsorb landfill leachate (adsorption test, COD concentration detection and COD adsorption capacity calculation, ammonia nitrogen concentration detection and ammonia nitrogen adsorption capacity calculation, heavy metal ion concentration detection and adsorption capacity calculation are the same as in Examples 1-9), and the performance parameters are shown in Table 3.

[0165] Table 3 Effect of carbonization temperature on the properties of the prepared activated carbon

[0166] carbonization temperature <![CDATA[Q COD (mg / g)]]> <![CDATA[Q N (mg / g)]]> <![CDATA[Q Pb (mg / g)]]> 275℃ 631.06 415.51 20.37 300℃ 653.89 433.45 26.88 325℃ 671.26 442.39 30.52 350℃ 684.58 459.88 33.16 550℃ 686.73 461.36 34.81 750℃ 689.32 463.47 35.93 775℃ 687.19 457.73 32.45 800℃ 675.34 451.08 28.29 825℃ 646.74 442.62 24.74

[0167] As shown in Table 3, when the carbonization temperature is below 350℃ (as shown in Table 3, carbonization temperatures = 325℃, 300℃, 275℃, and even lower values ​​not listed in Table 3), the low carbonization temperature leads to insufficient reaction between raw materials and incomplete carbonization, resulting in a significant decrease in the adsorption capacity of the prepared activated carbon for COD, ammonia nitrogen, and lead as the carbonization temperature decreases. When the carbonization temperature is between 350℃ and 750℃ (as shown in Table 3, carbonization temperatures = 350℃, 550℃, and 750℃), during the carbonization process, the sodium ions, ammonium ions, and hydroxide ions released by the calcining agent, the aluminosilicates and metal cations contained in the red mud, and the phosphates, sulfates, fluorides, and chlorides in phosphogypsum synergistically promote the chain breaking of high-carbon chains and benzene ring oil-based substances in the sludge and catalytic deoxygenation and hydrogenation, achieving rapid carbonization of the sludge. The simultaneous carbonization of the calcining agent during the carbonization process is beneficial for the rapid formation of pores and cracks in the carbonization products of the sludge. Simultaneously, under carbonization conditions, red mud, phosphogypsum, and pre-activated sludge react with each other. Under carbothermic chlorination, gases such as aluminum chloride, silicon chloride, and ferric chloride are released from the red mud and phosphogypsum, and sulfates, phosphates, and aluminosilicates are melted out. These substances are incorporated into the carbon-based materials through gas-phase precipitation, crystal phase fusion, and electrochemical corrosion. Ultimately, the prepared activated carbon exhibits COD adsorption capacities greater than 684 mg / g, ammonia nitrogen adsorption capacities greater than 459 mg / g, and lead adsorption capacities greater than 33 mg / g. When the carbonization temperature exceeds 750℃ (as shown in Table 3, carbonization temperatures = 775℃, 800℃, 825℃, and higher values ​​not listed in Table 3), the excessively high carbonization temperature leads to over-calcination of the material and collapse of the carbon structure. Consequently, the adsorption capacities of the prepared activated carbon for COD, ammonia nitrogen, and lead decrease significantly with further increases in carbonization temperature. Therefore, considering both benefits and costs, a carbonization temperature of 350℃-750℃ is most conducive to improving the adsorption performance of activated carbon powder prepared from oil sludge.

[0168] Examples 40-45 verified the effect of the type of calcining agent on the performance of the prepared activated carbon.

[0169] Example 40

[0170] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0171] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium lauryl sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to a moisture content of 15% at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 750℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0172] Example 41

[0173] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0174] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was fatty alcohol polyoxyethylene ether ammonium sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 15% moisture content at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 750℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0175] Example 42

[0176] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0177] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge, wherein the calcining agent was sodium fatty alcohol polyoxyethylene ether sulfate. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to 15% moisture content at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 750℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm, mixed with water at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0178] Example 43

[0179] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0180] The calcining agent and sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated sludge. The calcining agent was a compound of sodium lauryl sulfate and sodium fatty alcohol polyoxyethylene ether sulfate at a mass ratio of 1:1. Red mud, phosphogypsum, and pre-activated sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red mud paste. The activated red mud paste was dried to 15% moisture content at 175℃ to obtain dried sludge paste. The dried sludge paste was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 750℃ to obtain primary sludge coarse carbon. The primary sludge coarse carbon was ground into sludge coarse carbon powder with a particle size of 100μm. Water and sludge coarse carbon powder were mixed at a mass ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0181] Example 44

[0182] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0183] The calcining agent and sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated sludge. The calcining agent was a compound of sodium lauryl sulfate and fatty alcohol polyoxyethylene ether ammonium sulfate at a mass ratio of 1:1. Red mud, phosphogypsum, and pre-activated sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red mud paste. The activated red mud paste was dried to 15% moisture content at 175℃ to obtain dried sludge paste. The dried sludge paste was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 750℃ to obtain primary sludge coarse carbon. The primary sludge coarse carbon was ground into sludge coarse carbon powder with a particle size of 100μm. Water and sludge coarse carbon powder were mixed at a ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0184] Example 45

[0185] This application discloses a method for preparing activated carbon powder using oil sludge, comprising the following steps:

[0186] The calcining agent and oil sludge were weighed out at a mass ratio of 5.5:100, mixed, and stirred for 4.5 hours to obtain pre-activated oil sludge. The calcining agent was a compound of fatty alcohol polyoxyethylene ether ammonium sulfate and fatty alcohol polyoxyethylene ether sodium sulfate at a mass ratio of 1:1. Red mud, phosphogypsum, and pre-activated oil sludge were weighed out at a mass ratio of 7.5:5.5:100, mixed, and stirred evenly to obtain activated red oil paste. The activated red oil paste was dried to a moisture content of 15% at 175℃ to obtain dried oil paste sludge. The dried oil paste sludge was placed in a carbonization furnace for carbonization treatment at a carbonization temperature of 750℃ to obtain primary oil sludge coarse carbon. The primary oil sludge coarse carbon was ground into oil sludge coarse carbon powder with a particle size of 100μm. Water and oil sludge coarse carbon powder were mixed at a mass ratio of 10:1 mL / g, stirred for 1.25 hours, filtered, and dried to obtain high-performance activated carbon powder.

[0187] The high-performance activated carbon powder prepared in Examples 40-45 of this application was used to adsorb landfill leachate (adsorption test, COD concentration detection and COD adsorption capacity calculation, ammonia nitrogen concentration detection and ammonia nitrogen adsorption capacity calculation, heavy metal ion concentration detection and adsorption capacity calculation are the same as in Examples 1-9), and the performance parameters are shown in Table 4.

[0188] Table 4. Effect of calcining agent type on the properties of prepared activated carbon

[0189]

[0190] As shown in Table 4, when the calcining agent is any one of sodium lauryl sulfate, fatty alcohol polyoxyethylene ether ammonium sulfate, or sodium lauryl sulfate, or a 1:1 mass ratio of sodium lauryl sulfate and fatty alcohol polyoxyethylene ether ammonium sulfate, or a 1:1 mass ratio of fatty alcohol polyoxyethylene ether ammonium sulfate and sodium lauryl sulfate, the COD, ammonia nitrogen, and lead adsorption capacities of the prepared activated carbon powder are relatively close. When a 1:1 mass ratio of sodium lauryl sulfate and fatty alcohol polyoxyethylene ether sulfate is used, the COD, ammonia nitrogen, and lead adsorption capacities of the prepared activated carbon powder are significantly improved.

[0191] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A method for producing activated carbon powder using oil sludge, characterized by, The method comprises the following steps: S1, respectively, take calcined agent and oil sludge, mix and stir to obtain pre-activated oil sludge; S2, respectively, take red mud, phosphogypsum and pre-activated oil sludge, mix and stir uniformly to obtain activated red oil paste; S3, the activated red oil paste is dried to obtain oil paste dry mud, the oil paste dry mud is placed in a carbonization furnace for carbonization treatment to obtain first-stage oil sludge coarse carbon, the first-stage oil sludge coarse carbon is ground into powder and then mixed with water, stirred, filtered, dried to obtain the required high-performance activated carbon powder; The mass ratio of the calcined agent to the oil sludge in the step S1 is (0.5-5.5):100; the calcined agent in the step S1 is at least one of sodium lauryl sulfate, fatty alcohol polyoxyethylene ether ammonium sulfate and fatty alcohol polyoxyethylene ether sodium sulfate; the mass ratio of the red mud, the phosphogypsum and the pre-activated oil sludge in the step S2 is (0.5-7.5):(0.5-5.5):

100.

2. The method for preparing activated carbon powder using oil sludge according to claim 1, characterized in that, The calcined agent is a compound of sodium lauryl sulfate and fatty alcohol polyoxyethylene ether sodium sulfate with a mass ratio of 1:

1.

3. The method for preparing activated carbon powder using oil sludge according to claim 1, characterized in that, The red mud in the step S2 is Bayer process red mud.

4. The method for preparing activated carbon powder using oil sludge according to claim 1, characterized in that, The phosphogypsum in the step S2 is a solid waste produced in the wet-process phosphoric acid process, and the particle size is 16-22 μm.

5. The method for preparing activated carbon powder using oil sludge according to claim 1, characterized in that, The drying temperature in the step S3 is 75-175 ℃, and the water content of the oil paste dry mud is 5-15%.

6. The method for preparing activated carbon powder using oil sludge according to claim 1, characterized in that, The carbonization temperature in the step S3 is 350-750 ℃.

7. The method for preparing activated carbon powder using oil sludge according to claim 1, characterized in that, The mixing ratio of water to oil sludge coarse carbon powder in the step S3 is (2-10):1 mL / g.