CN112876041A - Treatment method of oily sludge - Google Patents

Treatment method of oily sludge Download PDF

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Publication number
CN112876041A
CN112876041A CN202110089142.XA CN202110089142A CN112876041A CN 112876041 A CN112876041 A CN 112876041A CN 202110089142 A CN202110089142 A CN 202110089142A CN 112876041 A CN112876041 A CN 112876041A
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beta
oil
water
precursor
oily sludge
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CN112876041B (en
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叶艳
宋瀚轩
李萌萌
周广旭
解涛
孙振玮
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China University of Petroleum Beijing
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
    • C02F11/148—Combined use of inorganic and organic substances, being added in the same treatment step
    • 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
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention provides a method for treating oily sludge, which comprises the following steps: mixing Fe3O4The @ beta-CD nano composite material is dissolved in water, prepared into nano fluid and then added into the oily sludge; stirring and/or ultrasonically vibrating for 15min-45 min; standing for 15-30 min, and separating solid phase, water phase and oil phase. Fe in the invention3O4The @ beta-CD nanocomposite can intelligently find an oil-water interface and an oil-solid interface to separate oil from water, oil and solid, and is high in oil removal efficiency; and, Fe3O4The @ beta-CD nanocomposite can be recycled for secondary utilization, and the oil removal rate of the @ beta-CD nanocomposite is still up to 85% during secondary utilization, so that the @ beta-CD nanocomposite has a good application prospect.

Description

Treatment method of oily sludge
Technical Field
The invention belongs to the field of oily sludge treatment, and particularly relates to Fe3O4The application of the @ beta-CD nanocomposite material in the oil-containing sludge.
Background
As one of the main energy pillars in China, the consumption of petroleum is increased year by year with the recent economic growth and rapid social development of the nation, and the consumption of petroleum energy occupies 1/5 of the total energy consumption in China in recent years, but the problem of environmental pollution is increasingly serious.
The oily sludge is a solid waste generated in the oil exploitation and transportation process, and the oily sludge is increased year by year along with the improvement of exploitation strength, so that the harmless and recycling treatment of the oily sludge becomes a hot spot concerned by current scholars. The oily sludge treatment method mainly comprises pyrolysis, solvent extraction, chemical cleaning, ultrasonic treatment, biological treatment and the like.
CN111333289A discloses an oily sludge treating agent calculated by taking the mass of oily sludge as a reference. The treating agent mainly comprises a viscosity reducer, petroleum sulfonate, sodium dodecyl benzene sulfonate, sodium silicate and an oxidant, the viscosity problem of the oily sludge after being placed for a long time can be reduced by the viscosity reducer in the method, the oily sludge can be efficiently cleaned by the oxidant, but the oxidant has to act under high temperature and ultrasonic conditions, and a large amount of energy consumption is caused. CN106520134A discloses an oily sludge treatment agent, which comprises the following main raw materials: the invention relates to a soil restoration agent for polluted soil, which comprises styrene sulfonic acid, sodium bentonite, polyacrylamide, waste bamboo leaves, maleic anhydride monoester, dimethyl malonate, 1-phenyl-3-methyl-4-benzoyl pyridinone, waste bagasse, fly ash, chitosan and polyaluminium chloride. CN107162360A discloses a high-efficiency oily sludge treatment agent, which is prepared from polyacrylamide, titanium carbonitride, gynostemma pentaphylla fruits, tangerine seeds, coconut peels, goosegrass, sodium bicarbonate, pelargonium graveolens, rosemary essential oil, basic magnesium carbonate, limonene, a fingered citron extract, chitosan and humic acid. CN111039526A discloses an efficient oily sludge treating agent with less material consumption, good treatment effect and stable performance, which mainly comprises saccharin sodium, montmorillonite, polyoxyethylene, humic acid, maleic anhydride, sodium bicarbonate, mozzie buster, polyaluminium chloride, waste coconut peel, mandarin orange and chitosan. Grinding the large substances into powder, synthesizing the powder into particles, and stirring for 2-3h at 40-55 ℃, wherein the treatment process is simple, but the treatment process has strict requirements on treatment equipment. CN107601797A discloses an oil-containing sludge treatment agent comprising a primary demulsifier and a secondary demulsifier, wherein the primary demulsifier is an organic acid salt comprising formate, acetate and glycolate, and the secondary demulsifier is a mixture of polyacrylamide and persulfate (or perphosphate).
Therefore, there is a need to develop an oil-containing sludge treatment method which is environmentally friendly, low in cost, simple in production, and capable of being reused, so as to more efficiently perform treatment and disposal of oil-containing sludge.
Disclosure of Invention
An object of the present invention is to provide a method for treating oil-containing sludge.
The inventors of the present invention found Fe in their research3O4The @ beta-CD nanocomposite used as the oily sludge treatment agent can intelligently find an oil-water interface and an oil-solid interface, can reduce the interfacial tension between oil and water and oil-solid, and has the advantages of high oil removal efficiency, good effect and environmental friendliness.
Thus, the present invention provides a method for treating oily sludge, comprising:
mixing Fe3O4The @ beta-CD nano composite material is dissolved in water, prepared into nano fluid and then added into the oily sludge;
stirring and/or ultrasonic vibrating for 15min-45 min;
standing for 15-30 min, and separating solid phase, water phase and oil phase.
According to a specific embodiment of the present invention, the purpose of stirring and/or ultrasound after adding the nanofluid to the oily sludge in the present invention is to make Fe3O4The @ beta-CD nano composite material is fully contacted with the oily sludge, so that a better oil removing effect is realized.
According to a particular embodiment of the invention, the ultrasound has a frequency of 60Hz to 80 Hz.
According to a specific embodiment of the present invention, in the present invention, the Fe3O4The addition amount of the @ beta-CD nano composite material is 0.3-5 percent (mass fraction) of the oily sludge.
According to a particular embodiment of the invention, in the present invention, the nanofluid contains Fe3O4The mass fraction of the @ beta-CD nano composite material is 0.3-2%.
According to a specific embodiment of the present invention, in the present invention, the Fe3O4The grain size of the @ beta-CD nano composite material is 5nm-500 nm.
According to a specific embodiment of the present invention, in the present invention, the Fe3O4The @ beta-CD nanocomposite was prepared according to the following method:
uniformly dispersing an iron source and a surfactant in an alcohol solvent, adding an alkaline pH regulator to regulate the pH to 9-11, and reacting at 150-260 ℃ for 12-24 h to obtain Fe3O4A precursor;
mixing Fe3O4Uniformly dispersing the precursor, the modifier and the alkaline pH regulator in deionized water, and adding H2O2For Fe at pH 8-93O4Performing modification reaction on the precursor to obtain Fe3O4@ beta-CD nanocomposite; the modification reaction is carried out for 4 to 10 hours under the condition of 60 to 100Hz ultrasound at the temperature of between 40 and 60 ℃.
According to a specific embodiment of the present invention, the alcohol solvent includes one or more of methanol, ethanol, and ethylene glycol.
According to a specific embodiment of the present invention, the iron source is dispersed in the alcohol solvent at a concentration of 20g/L to 50 g/L.
According to a specific embodiment of the present invention, Fe3O4The mass fraction of the precursor dispersed in the deionized water is 3-5%.
According to a specific embodiment of the present invention, the iron source comprises one or more of ferric chloride hexahydrate, ferric sulfate and ferric nitrate.
According to a specific embodiment of the present invention, the alkaline pH adjuster comprises one or more of urea, sodium carbonate, ammonia water and sodium hydroxide.
According to a specific embodiment of the present invention, in the present invention, the surfactant includes a polyethylene glycol-based surfactant; the amount of the surfactant is 80-150% (mass fraction) of the iron source.
According to a specific embodiment of the present invention, in the present invention, the modifying agent includes cyclodextrin-based modifying agents, such as β -cyclodextrin; preferably, the modifier is used in an amount of Fe3O4The mass fraction of the precursor is 50-800%.
According to a specific embodiment of the present invention, in the present invention, said H2O2In an amount of Fe3O4The precursor accounts for 100-450 percent (mass fraction). Said H2O2The amount of (B) is H2O2H in solution2O2The content of (a). Said H2O2Can provide a reaction environment so that the cyclodextrin can react with Fe3O4And (4) successfully combining.
In the invention, Fe3O4The @ beta-CD nanocomposite material has the following beneficial technical effects when used for oil stain treatment: fe3O4The @ beta-CD nanocomposite can intelligently find an oil-water interface and an oil-solid interface to separate oil from water, oil and solid, and is high in oil removal efficiency; in addition, the ferroferric oxide magnetic nano composite material can be recycled for secondary utilization, and the oil removal rate of the ferroferric oxide magnetic nano composite material is still as high as 85% during secondary utilization, so that the ferroferric oxide magnetic nano composite material has a good application prospect; meanwhile, Fe in the present invention3O4The @ beta-CD nanocomposite is waterSynthesizing Fe at 150-260 deg.C by thermal method3O4Precursor, then cyclodextrin modifier is used as modifier, aqueous solution is used as dispersion medium, ultrasonic dispersion is carried out for modification; synthetic Fe3O4The @ beta-CD nanocomposite material has a nanometer-scale diameter and good magnetism.
Drawings
FIG. 1 is an XRD pattern for example 1-example 4; wherein the horizontal axis represents diffraction angle and the vertical axis represents intensity.
FIG. 2 shows Fe obtained in example 13O4SEM image of @ beta-CD nanoparticles.
FIG. 3 shows Fe obtained in example 23O4SEM image of @ beta-CD nanoparticles.
FIG. 4 shows Fe obtained in example 33O4SEM image of @ beta-CD nanoparticles.
FIG. 5 shows Fe obtained in example 43O4SEM image of @ beta-CD nanoparticles.
FIG. 6 shows Fe obtained in example 13O4Infrared spectrum of @ beta-CD nano particle.
FIG. 7 shows Fe obtained in example 13O4The oil removal efficiency diagram of the @ beta-CD nano particles is characterized in that Fe is added under the ultrasonic action3O4The oil removal efficiency of the @ beta-CD nano particles is improved by 40.24 percent.
FIG. 8 shows Fe obtained in example 13O4The intelligent oil finding graph of the @ beta-CD nano particles.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
According to Fe3O4The chemical formula is that 1.15g of ferric chloride hexahydrate is used as an iron source, 30mL of ethylene glycol is used as a solvent and a reducing agent, 1g of polyethylene glycol 4000 is used as a surfactant, 2g of urea provides an alkaline environment, the pH value is about 10-11, and the product is subjected to heat preservation for 18 hours at 200 ℃ by a hydrothermal methodWashing with deionized water and ethanol, drying at 90 deg.C for 30min to obtain a certain amount of nanoscale Fe3O4A precursor; taking dried Fe3O4Adding 1g of precursor and 1g of beta-cyclodextrin into 30mL of deionized water, adjusting the pH to be about 8-9 by adopting 15% ammonia water, and adding 5mL of 30% H every 1H for three times2O2. Performing ultrasonic treatment at 60 deg.C under 60Hz for 8 hr, cooling to room temperature, sequentially cleaning with ionized water and ethanol, and drying at 90 deg.C for 30min to obtain Fe3O4@β-CD。
Fe obtained in this example3O4The @ beta-CD nanoparticles have a spherical structure with a particle size of about 200nm to 300nm, as shown in XRD (X-ray diffraction) diagram) and SEM (scanning Electron microscope) diagram of FIG. 1 and SEM diagram of FIG. 2.
Example 2
According to Fe3O4The chemical formula is that 1.15g of ferric chloride hexahydrate is used as an iron source, 30mL of ethylene glycol is used as a solvent and a reducing agent, 1g of polyethylene glycol 4000 is used as a surfactant, 2g of urea provides an alkaline environment, the pH value is about 10-11, a hydrothermal method is adopted, the temperature is kept at 200 ℃ for 20 hours, then a product is cleaned by deionized water and ethanol, and the product is dried at 90 ℃ for 30 minutes to obtain a certain amount of nanoscale Fe3O4A precursor; taking dried Fe3O4Adding 1g of precursor and 1.5g of beta-cyclodextrin into 30mL of deionized water, adjusting the pH to 8-9 by adopting 15% ammonia water, and adding 5mL of 30% H every 1H for three times2O2. Performing ultrasonic treatment at 60 deg.C under 70Hz for 8 hr, cooling to room temperature, sequentially cleaning with ionized water and ethanol, and drying at 90 deg.C for 30min to obtain Fe3O4@β-CD。
Fe obtained in this example3O4The XRD pattern of the @ beta-CD nanoparticles is shown in FIG. 1, the SEM pattern is shown in FIG. 3, the particle size is about 200nm-300nm, the spherical structure is shown in FIG. 6, and the infrared spectrum is shown in FIG. 6.
Example 3
According to Fe3O4The chemical formula is that 1.15g of ferric chloride hexahydrate is used as an iron source, 30mL of ethylene glycol is used as a solvent and a reducing agent, 1g of polyethylene glycol 4000 is used as a surfactant, 2g of urea provides an alkaline environment, the pH value is about 10-11, and the hydrothermal method is carried out for heat preservation at 200 ℃ for 22 hoursWashing the product with deionized water and ethanol, and drying at 90 deg.C for 30min to obtain a certain amount of nanoscale Fe3O4A precursor; taking dried Fe3O4Adding 1g of precursor and 2g of beta-cyclodextrin into 30mL of deionized water, adjusting the pH to be 8-9 by adopting ammonia water with the concentration of 15%, and adding 5mL of H with the concentration of 30% every 1H for three times2O2. Ultrasonic treating at 60 deg.C under 80Hz for 8 hr, cooling to room temperature, washing with ionized water and ethanol sequentially, drying at 90 deg.C for 30min to obtain Fe3O4@β-CD。
Fe obtained in this example3O4The @ beta-CD nanoparticles have a spherical structure with a particle size of about 200nm to 300nm as shown in FIG. 1 in an XRD pattern and as shown in FIG. 4 in an SEM pattern.
Example 4
According to Fe3O4The chemical formula is that 1.15g of ferric chloride hexahydrate is used as an iron source, 30mL of ethylene glycol is used as a solvent and a reducing agent, 1g of polyethylene glycol 4000 is used as a surfactant, 2g of urea provides an alkaline environment, the pH value is about 10-11, the product is washed and dried by deionized water and ethanol at the temperature of 200 ℃ for 24 hours by a hydrothermal method, and the product is dried at the temperature of 90 ℃ for 30 minutes to obtain a certain amount of nanoscale Fe3O4A precursor; taking dried Fe3O4Adding 1g of precursor and 2.5g of beta-cyclodextrin into 30mL of deionized water, adjusting the pH to be 8-9 by adopting ammonia water with the concentration of 15%, and adding 5mL of H with the concentration of 30% every 1 hour for three times2O2. Performing ultrasonic treatment at 60 deg.C under 100Hz for 8 hr, cooling to room temperature, washing with ionized water and ethanol sequentially, drying at 90 deg.C for 30min to obtain Fe3O4@β-CD。
Fe obtained in this example3O4The @ beta-CD nanoparticles have an XRD pattern as shown in FIG. 1 and an SEM pattern as shown in FIG. 5, and have a particle size of about 5nm to 100 nm.
Example 5
Taking 3g of oily sludge in a beaker, taking 0.15g of the sample obtained in the example 1, preparing the sample into 0.5% nano liquid, adding the nano liquid into the beaker, placing the beaker in ultrasonic for 70Hz ultrasonic oscillation for 45min, then standing for 30min, carrying out three-phase separation of a solid phase, a water phase and an oil phase, drying the separated solid phase, measuring the oil removed solid phase, and then measuring the oil removed solid phaseOil content of solid phase, without addition of Fe in the present invention3O4The experimental results are shown in FIG. 7 with respect to @ β -CD as a blank control, and it can be seen from FIG. 7 that Fe was added3O4After @ beta-CD, the oil removal efficiency can reach 90.17 percent, and is improved by 40.24 percent compared with the blank control without adding. And, through carrying out the secondary deoiling experiment after the magnetism is retrieved, discover the Fe after the secondary recovery3O4The oil removal efficiency of @ beta-CD is still as high as about 85 percent, which indicates that Fe3O4@ beta-CD can be reused.
Example 6
Taking 0.5 percent of Fe3O420mL of @ beta-CD dispersion liquid is added into 40mL of oil-water mixed liquid, the mixture is subjected to 80Hz ultrasonic oscillation for 15min, the mixture is kept stand for 15min after the ultrasonic oscillation is finished, oil-water separation is carried out, and Fe3O4@ beta-CD is enriched at the oil-water interface. The results of the experiment are shown in FIG. 8. As can be seen from the figure, the addition of Fe3O4Before the @ beta-CD nano particles, the oil-water interface is not clear, the emulsification phenomenon is serious, and the oil-water separation is difficult, but Fe is added3O4After @ beta-CD nanoparticles, the oil-water interface was clearly visible by simply shaking and standing, enabling separation treatment. The experimental result shows that Fe3O4The @ beta-CD nano particles can efficiently search an oil-water interface to separate oil from water.

Claims (10)

1. A method for treating oily sludge, comprising:
mixing Fe3O4The @ beta-CD nano composite material is dissolved in water, prepared into nano fluid and then added into the oily sludge;
stirring and/or ultrasonic vibrating for 15min-45 min;
standing for 15-30 min, and separating solid phase, water phase and oil phase.
2. The method of claim 1, wherein the Fe3O4The addition amount of the @ beta-CD nano composite material is 0.3-5% of the mass of the oily sludge.
3. The method of claim 1, wherein the nanofluid is Fe3O4The mass fraction of the @ beta-CD nano composite material is 0.3-2%.
4. The method of claim 1, wherein the Fe3O4The grain size of the @ beta-CD nano composite material is 5nm-500 nm.
5. The method of claim 1, wherein the ultrasound has a frequency of 60Hz-80 Hz.
6. The method of any one of claims 1-5, wherein the Fe3O4The @ beta-CD nanocomposite was prepared according to the following method:
uniformly dispersing an iron source and a surfactant in an alcohol solvent, adding an alkaline pH regulator to regulate the pH to 9-11, and reacting at 150-260 ℃ for 12-24 h to obtain Fe3O4A precursor;
mixing Fe3O4Uniformly dispersing the precursor, the modifier and the alkaline pH regulator in deionized water, and adding H2O2For Fe at pH 8-93O4Performing modification reaction on the precursor to obtain Fe3O4@ beta-CD nanocomposite; the modification reaction is carried out for 4 to 10 hours under the condition of 60 to 100Hz ultrasound at the temperature of between 40 and 60 ℃.
7. The method of claim 6, wherein the iron source comprises one or more of ferric chloride hexahydrate, ferric sulfate, and ferric nitrate;
the alcohol solvent comprises one or more of methanol, ethanol and glycol;
the alkaline pH regulator comprises one or more of urea, sodium carbonate, ammonia water and sodium hydroxide.
8. The method of claim 6, wherein the surfactant comprises a polyethylene glycol-based surfactant; the amount of the surfactant is 80-150% of the mass of the iron source.
9. The method of claim 6, wherein the modifying agent comprises a cyclodextrin-based modifying agent, such as β -cyclodextrin; preferably, the modifier is used in an amount of Fe3O4The mass fraction of the precursor is 50-800%.
10. The method of claim 5, wherein the H2O2In an amount of Fe3O4The precursor accounts for 100-450 percent (mass fraction).
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09176659A (en) * 1995-12-25 1997-07-08 Shimizu Corp Method for purifying oil-containing sludge
CN103819631A (en) * 2014-02-28 2014-05-28 西南石油大学 Oil suction high-molecular material based on host-guest interaction and preparation method
US20140175015A1 (en) * 2011-06-20 2014-06-26 Fujifilm Corporation Water purification method
CN106336067A (en) * 2016-04-21 2017-01-18 浙江海洋学院 Domestic wastewater purifying treatment method
CN106830248A (en) * 2017-03-14 2017-06-13 长江大学 For the preparation method of the magnetic Nano water treatment agent of oilfield sewage
CN110272174A (en) * 2019-06-28 2019-09-24 陕西欧菲德环保科技有限公司 A kind of alkalinity release agent and the application in oil sludge processing
CN110550666A (en) * 2019-09-27 2019-12-10 陕西科技大学 Monodisperse and superparamagnetic ferroferric oxide nanoflower and preparation method thereof
CN111234049A (en) * 2018-11-28 2020-06-05 天津大学 Self-assembly type cyclodextrin functionalized magnetic-gold composite material and preparation method and application thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09176659A (en) * 1995-12-25 1997-07-08 Shimizu Corp Method for purifying oil-containing sludge
US20140175015A1 (en) * 2011-06-20 2014-06-26 Fujifilm Corporation Water purification method
CN103819631A (en) * 2014-02-28 2014-05-28 西南石油大学 Oil suction high-molecular material based on host-guest interaction and preparation method
CN106336067A (en) * 2016-04-21 2017-01-18 浙江海洋学院 Domestic wastewater purifying treatment method
CN106830248A (en) * 2017-03-14 2017-06-13 长江大学 For the preparation method of the magnetic Nano water treatment agent of oilfield sewage
CN111234049A (en) * 2018-11-28 2020-06-05 天津大学 Self-assembly type cyclodextrin functionalized magnetic-gold composite material and preparation method and application thereof
CN110272174A (en) * 2019-06-28 2019-09-24 陕西欧菲德环保科技有限公司 A kind of alkalinity release agent and the application in oil sludge processing
CN110550666A (en) * 2019-09-27 2019-12-10 陕西科技大学 Monodisperse and superparamagnetic ferroferric oxide nanoflower and preparation method thereof

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