CN110590087A - Treatment method of oily sludge - Google Patents

Treatment method of oily sludge Download PDF

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Publication number
CN110590087A
CN110590087A CN201910672589.2A CN201910672589A CN110590087A CN 110590087 A CN110590087 A CN 110590087A CN 201910672589 A CN201910672589 A CN 201910672589A CN 110590087 A CN110590087 A CN 110590087A
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China
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sludge
stage
collected
hot washing
oily sludge
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CN110590087B (en
Inventor
侯影飞
黄朝琦
秦志文
郭宁
尚绪敏
王刚
温燕军
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China University of Petroleum East China
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China University of Petroleum East China
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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
    • 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
    • C02F11/002—Sludge treatment using liquids immiscible with water
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
    • 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
    • C02F11/13—Treatment of sludge; Devices therefor by de-watering, drying or thickening by heating
    • C02F11/131—Treatment of sludge; Devices therefor by de-watering, drying or thickening by heating using electromagnetic or ultrasonic waves
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1003—Waste materials
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/40—Characteristics of the process deviating from typical ways of processing
    • C10G2300/4006—Temperature
    • 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

Abstract

The invention relates to a method for treating oily sludge. The method comprises the following steps: step a: carrying out hot washing treatment on the oily sludge by using a chemical agent, then layering the sludge after the hot washing to form an upper oil phase, a middle water phase and a lower layer of sludge, and respectively collecting the upper oil phase, the middle water phase and the lower layer of sludge after separation; step b: sequentially carrying out microwave heat treatment on the lower layer sludge in two stages; wherein, the first stage is heated to 150-220 ℃, and the evaporated gas phase is collected in the first stage; and in the second stage, the sludge is continuously heated to 580-600 ℃ for thermal decomposition, then the generated non-condensable gas and condensate are cooled and recovered, and finally the sludge residue after pyrolysis is collected. The invention realizes the aims of reduction, harmlessness and resource treatment of the oily sludge.

Description

Treatment method of oily sludge
Technical Field
The invention relates to the field of environmental protection, in particular to a method for treating oily sludge.
Background
The oily sludge is a common pollutant in the petroleum industry, and a large amount of oily sludge can be generated in various links such as petroleum exploitation, gathering and transportation, refining and the like. The oily sludge is a pollutant mainly mixed with petroleum, sewage, sludge and the like, generally contains a large amount of aged crude oil, oil extraction agents, salts, solid suspended matters, corrosives, bacteria and the like, has very complex composition, and is seriously harmful to the environmental safety when being directly discharged. At present, oily sludge is listed as dangerous solid waste (HW08) by the national records of dangerous waste.
With the increasing intensity of oil exploitation, the yield of oil-containing sludge is continuously increased every year. It is estimated that 1 ton of oily sludge is produced per 500 tons of crude oil processed, and at present, the yield of the oily sludge in China exceeds 300 ten thousand tons per year, and the global yield is about 6000 ten thousand tons per year. In the past, due to the reasons that the technology is relatively laggard, the treatment cost is high, the harmless treatment rate is low and the like, a mature, economical and efficient treatment process and technology are not formed, and a plurality of local treatment methods are simple open-air stacking and landfill. However, as environmental protection supervision becomes stricter and stricter, more severe requirements are provided for harmless treatment of oily sludge, a great amount of accumulated and newly increased oily sludge needs to be effectively treated, and oil production enterprises in various regions face huge pressure, so that efficient and economical oily sludge treatment methods are urgently sought. At present, the treatment methods for oily sludge at home and abroad mainly comprise an incineration method, a pyrolysis method, an extraction method, a biological method, a hot washing method and the like, and all the treatment methods have certain advantages, but have limitations and cannot fully utilize the beneficial value of the oily sludge.
Disclosure of Invention
The invention aims to provide a method for treating oily sludge, which can fully utilize oil phase in the sludge, improve the oil removal rate and the recovery value and solve the limitation of the prior art.
In order to achieve the above purpose, the invention provides the following technical scheme:
a method for treating oily sludge comprises the following steps:
step a: carrying out hot washing treatment on the oily sludge by using a chemical agent, then layering the sludge after the hot washing to form an upper oil phase, a middle water phase and a lower layer of sludge, and respectively collecting the upper oil phase, the middle water phase and the lower layer of sludge after separation;
step b: sequentially carrying out microwave heat treatment on the lower layer sludge in two stages; wherein, the first stage is heated to 150-220 ℃, and the evaporated gas phase is collected in the first stage; and in the second stage, the sludge is continuously heated to 580-600 ℃ for thermal decomposition, then the generated non-condensable gas and condensate are cooled and recovered, and finally the sludge residue after pyrolysis is collected.
Wherein, the step a can realize the layering by standing or centrifuging, or other feasible ways.
The above scheme of the invention achieves the following technical effects:
firstly, the invention organically combines the 'hot washing' with the 'microwave pyrolysis', and the oil in the sludge is removed and recovered at least twice, so that the oil is almost completely removed.
Secondly, the recovery of moisture from the sludge by the heating of the first stage of step b both dries the sludge and gains additional economic benefits in the process-since the recovered water vapour can release heat by condensation for any industrial process, such as the heating of step a and step b.
Thirdly, the middle water phase collected in the step a is rich in chemical agents and can be recycled in the hot washing stage. The solid-phase main component residue finally separated in the step b has the oil content of below 0.28 percent, meets the national emission standard (GB 4284-84), has the heavy metal content within the standard limit value (GB 15618-18), and can be used for paving or burying.
Fourthly, the second stage of the step b carries out thermal decomposition on the residual oil in the oily sludge to generate combustible gas (H2, CO, methane and the like) and pyrolysis oil with higher economic value, and the combustible gas and the pyrolysis oil can be further recycled, so that the resource purpose of the oily sludge is realized.
Fifth, microwave heating is different from conventional heating methods such as electric heating, and has the characteristics of integral heating, rapid temperature rise, energy conservation, high efficiency, easy control and the like. The microwave mode is adopted to carry out heat treatment on the oily sludge, so that the rapid heating rate and the good oil removing effect can be obtained in a short time.
In conclusion, the invention realizes the aims of reduction, harmlessness, resource utilization and high-efficiency treatment of the oily sludge.
The invention also optimizes the raw materials and treatment conditions of each step as follows.
The chemical agent of step a is mainly used for separating oil, water and solid phase by reducing interfacial tension, emulsification or changing wettability and rigid interfacial film, and can be replaced by other preferable formulas, and the preferable formula of the invention is mainly SDS, NP-10 and Na2SiO3Chemical agents of the composition.
Preferably, SDS, NP-10 and Na2SiO3The mass ratio of (a) to (b) is 1-2: 1-2, including but not limited to 1:1:1, 2:1:1, 1:2:1, 1:1:2, 2:2:1, 1:2:2, 2:1:2, 1.5:2:1, and the like.
The chemical agent is added to the oil-containing sludge in a solution state, and preferably, the chemical agent comprises SDS, NP-10 and Na2SiO3Is 2.5 to 3.5 wt%, including but not limited to 2.5 wt%, 2.6 wt%, 2.7 wt%, 2.8 wt%, 2.9 wt%, 3.0 wt%, 3.1 wt%, 3.5 wt%, etc.
Preferably, in the step a, the dosage of the chemical agent is 3-5 times of the mass of the oily sludge.
Preferably, the hot washing temperature in the step a is 80-100 ℃. For example, 80 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, 100 deg.C, etc.
Preferably, the step a is stirred for 150-250 r/min during hot washing.
Preferably, the heating temperature of the first stage in the step b is 150-200 ℃, and the continuously evaporated moisture is collected at the stage.
Preferably, the thermal decomposition time of the second stage in the step b is 30-90 min.
Preferably, the middle aqueous phase collected in step a is used for preparing the chemical agent;
preferably, the gas phase collected in the first stage of step b is used as a heat supply source in the hot washing of step a;
preferably, the non-condensable gas and condensed liquid collected in the second stage of step b can be used as the heating fuel for step a or step b.
Preferably, the heat released by the second stage cooling of step b is recovered for the hot wash.
In addition, in order to avoid oxidation of the cracked gas or oil at high temperature in step b, it is necessary to perform the process in an inert environment, such as purging a certain amount of inert gas (including but not limited to N) into the furnace2)。
In summary, compared with the prior art, the invention achieves the following technical effects:
(1) the oil removal rate of the oily sludge is improved;
(2) the water removal rate of the oily sludge is improved;
(3) the water phase, the oil phase, the water vapor, the pyrolysis gas and the like collected at each stage can be recycled and used as a heat supply source or a hot washing agent, so that the sludge is changed into valuable, the value of the sludge is fully utilized, and the sludge treatment cost is reduced;
(4) the method organically combines microwave heating and chemical hot washing, and achieves the aims of reduction, harmlessness, recycling and efficient treatment of the oily sludge.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings.
FIG. 1 is a flow chart of a method for treating oily sludge according to example 1 of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
As shown in FIG. 1, the oily sludge in a certain oil field is treated as follows:
the water content of the oily sludge before treatment is 54 wt%, the oil content is 26 wt% and the solid content is 20 wt%.
Firstly, chemical hot washing agents SDS, NP-10 and Na2SiO3Preparing a chemical hot washing medicament diluted solution with the concentration of 3 wt% according to the mass ratio of 1:1:1, mixing the oily sludge and the medicament solution according to the mass ratio of 1:4, and adding the mixture into a heating and stirring device.
And secondly, starting heating, setting the heating temperature to be 80 ℃, starting stirring after the temperature is reached, setting the stirring speed to be 200r/min, and setting the stirring time to be 50min, and carrying out chemical hot washing operation.
And thirdly, after the chemical heat washing is finished, taking out the materials and conveying the materials to a centrifugal device, wherein the centrifuged materials are layered into upper-layer floating oil, middle-layer sewage and lower-layer sludge. And respectively cutting and separating, recovering upper layer floating oil and middle layer sewage, and continuously treating the lower layer sludge serving as pre-deoiled sludge, wherein about 80% of oil content of the pre-deoiled sludge is separated compared with the original oily sludge. The upper layer floating oil is recycled, and the middle layer sewage contains medicament solution which is recycled for hot washing.
Fourthly, sending the pre-deoiled sludge to a microwave heating furnace, and introducing N2PurgingAnd starting microwave heating for 5min, and absorbing the steam generated before 200 ℃ with water as preheating water. And continuously heating to 600 ℃, and performing heat exchange condensation on oil gas generated after the temperature is 200 ℃ with water and recovering. The microwave pyrolysis treatment is completed after 50min (referring to the whole microwave heating time), and the oil content of the pyrolysis residue is only 0.28%, so that the national emission standard is met.
Example 2
Firstly, chemical hot washing agents AEO-9, LAS and Na2SiO33 wt% of chemical hot washing agent diluted solution is prepared according to the mass ratio of 1:1:1, and the oily sludge (the source is the same as that of the example 1) and the agent solution are mixed according to the mass ratio of 1:4 and added into a heating and stirring device.
And secondly, starting heating, setting the heating temperature to be 80 ℃, starting stirring after the temperature is reached, setting the stirring speed to be 200r/min, and setting the stirring time to be 50min, and carrying out chemical hot washing operation.
And thirdly, after the chemical heat washing is finished, taking out the materials and conveying the materials to a centrifugal device, wherein the centrifuged materials are layered into upper-layer floating oil, middle-layer sewage and lower-layer sludge. And respectively cutting and separating, recovering upper layer floating oil and middle layer sewage, and continuously treating the lower layer sludge serving as pre-deoiled sludge, wherein the oil content of the pre-deoiled sludge is about 70% removed compared with the original oily sludge. The upper layer floating oil is recycled, and the middle layer sewage contains medicament solution which is recycled for hot washing.
Fourthly, sending the pre-deoiled sludge to a microwave heating furnace, and introducing N2Purging for 5min, starting microwave heating, and absorbing the steam generated before 200 ℃ with water as preheating water. And continuously heating to 600 ℃, and performing heat exchange condensation on oil gas generated after the temperature is 200 ℃ with water and recovering. And (3) finishing microwave pyrolysis treatment after 60min (the whole microwave heating time), wherein the oil content of the pyrolysis residue is 0.26%, and the national emission standard is met.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (9)

1. The method for treating the oily sludge is characterized by comprising the following steps of:
step a: carrying out hot washing treatment on the oily sludge by using a chemical agent, then layering the sludge after the hot washing to form an upper oil phase, a middle water phase and a lower layer of sludge, and respectively collecting the upper oil phase, the middle water phase and the lower layer of sludge after separation;
step b: sequentially carrying out microwave heat treatment on the lower layer sludge in two stages; wherein, the first stage is heated to 150-220 ℃, and the evaporated gas phase is collected in the first stage; and in the second stage, the sludge is continuously heated to 580-600 ℃ for thermal decomposition, then the generated non-condensable gas and condensate are cooled and recovered, and finally the sludge residue after pyrolysis is collected.
2. The process of claim 1, wherein the chemical agent consists essentially of SDS, NP-10, and Na2SiO3Composition is carried out;
preferably, SDS, NP-10 and Na2SiO3The mass ratio of (A) to (B) is 1-2: 1-2.
3. The method of claim 2, wherein the chemical agent comprises SDS, NP-10, and Na2SiO3The total concentration of (A) is 2.5-3.5 wt%.
4. The treatment method according to claim 2, wherein in the step a, the dosage of the chemical agent is 3-5 times of the mass of the oily sludge.
5. The treatment method according to claim 2, wherein the temperature of the hot washing in the step a is 80 to 100 ℃.
6. The treatment method according to claim 1, wherein the step a is carried out by stirring at 150-250 r/min during hot washing.
7. The process according to claim 1, wherein the heating temperature in the first stage in the step b is 150 to 200 ℃.
8. The treatment method according to claim 1, wherein the thermal decomposition time of the second stage in the step b is 30 to 90 min.
9. The process of claim 1, wherein the middle aqueous phase collected in step a is used for the preparation of the chemical agent;
preferably, the gas phase collected in the first stage of step b is used as one of the heat sources for the hot washing in step a;
preferably, the non-condensable gas and condensed liquid collected in the second stage of the step b can be used as the heat supply fuel for the step a or the step b;
preferably, the heat released by the second stage cooling of step b is recovered for the hot wash.
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CN111908752A (en) * 2020-08-12 2020-11-10 陈贝 Treatment method of oily sludge
CN113003922A (en) * 2021-03-04 2021-06-22 山东科技大学 Integrated efficient hot washing-advanced oxidation combined oily sludge treatment system and oily sludge treatment method
CN113698065A (en) * 2021-08-20 2021-11-26 常州大学 Environment-friendly separation method of refined oil sludge
CN114477586A (en) * 2022-01-25 2022-05-13 安尔达技术(北京)有限责任公司 Comprehensive utilization and treatment method for oily wastewater

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