CN115536134B - Treatment method and device for oily sewage - Google Patents

Treatment method and device for oily sewage Download PDF

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Publication number
CN115536134B
CN115536134B CN202110727797.5A CN202110727797A CN115536134B CN 115536134 B CN115536134 B CN 115536134B CN 202110727797 A CN202110727797 A CN 202110727797A CN 115536134 B CN115536134 B CN 115536134B
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aerogel
sewage treatment
oil
treatment system
concentration
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CN115536134A (en
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王刚
高会杰
陈明翔
孙丹凤
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Sinopec Dalian Petrochemical Research Institute Co ltd
China Petroleum and Chemical Corp
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Sinopec Dalian Petrochemical Research Institute Co ltd
China Petroleum and Chemical Corp
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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
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/30—Aerobic and anaerobic processes
    • C02F3/302—Nitrification and denitrification treatment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/08—Aerobic processes using moving contact bodies
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/10—Packings; Fillings; Grids
    • C02F3/104—Granular carriers
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/10—Packings; Fillings; Grids
    • C02F3/105—Characterized by the chemical composition
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/10—Packings; Fillings; Grids
    • C02F3/105—Characterized by the chemical composition
    • C02F3/106—Carbonaceous materials
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/10—Packings; Fillings; Grids
    • C02F3/109—Characterized by the shape
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/12—Activated sludge processes
    • C02F3/1236—Particular type of activated sludge installations
    • C02F3/1263—Sequencing batch reactors [SBR]
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/28—Anaerobic digestion processes
    • C02F3/282—Anaerobic digestion processes using anaerobic sequencing batch reactors
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F2003/001—Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms
    • C02F2003/003—Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms using activated carbon or the like
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)
    • 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
    • Y02W10/10—Biological treatment of water, waste water, or sewage

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Environmental & Geological Engineering (AREA)
  • Hydrology & Water Resources (AREA)
  • Biodiversity & Conservation Biology (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Biological Treatment Of Waste Water (AREA)

Abstract

The invention relates to a treatment method of oily sewage, in the starting stage, filler is added according to the effective volume of a sewage treatment system not lower than 50%, wherein the filler is activated carbon and an oil-resistant immobilized carrier, then activated sludge is inoculated and denitrifying bacteria agent is added for stewing and exposure treatment; starting water inflow, continuously running in a mode of gradually increasing water inflow load, and finishing starting when the ammonia nitrogen concentration of the system water outflow is less than 1mg/L, TN concentration and the ammonia nitrogen concentration of the system water outflow is less than 15mg/L, COD concentration and is less than 30mg/L when the system water outflow is in full-load running, and turning into a running stage; and in the operation stage, filling materials are added every 6-12 months. According to the invention, the oil-resistant immobilized carrier and the activated carbon are simultaneously added into the oily sewage treatment system, so that the rapid start and stable operation of the system are realized, and the oil-resistant immobilized carrier and the activated carbon integrated sewage treatment system have the advantages of good comprehensive treatment effect, clear effluent, good long-period operation stability and the like.

Description

Treatment method and device for oily sewage
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a method and a device for treating oily sewage.
Background
During petroleum exploitation, refining, processing and the like, a large amount of oily sewage is generated, and most of the oil in the sewage exists in the state of floating oil, dispersed oil, emulsified oil and dissolved oil. The sewage is treated by adopting a combined process generally because the sewage has the characteristics of large discharge amount, complex components, large water quality fluctuation and the like. Wherein, the floating oil and the dispersed oil can be removed by an oil separation floatation mode, and the dissolved oil and part of the emulsified oil which is not easy to remove often enter a biochemical unit at the tail end along with the wastewater. In order to meet stricter emission standards, three-stage biochemical treatment units mainly comprising a biological membrane reactor such as MBBR, BAF, FCBR are added. However, for oily sewage, the biological membrane reactor is adopted for treatment, and the ideal treatment effect cannot be achieved after long-period operation.
Yang Qiuyue (MBBR process treatment oil refining sewage operation analysis, middle and external energy sources, 2020,25 (1)) adopts a mode of properly adding nutrient salts and high-quality carbon sources at the water inlet of the MBBR tank to promote the normal growth and propagation of microorganisms, thereby improving the problem of difficult film formation. Sang Junjiang (research on fluidized composite carrier biological film technology for treating high-salt-content oil refining sewage, petroleum refining and chemical industry, 2017,48 (8)) adopts a novel biological film method biochemical treatment technology (FCBR) of a patent composite carrier, wherein one carrier is attached with microorganisms for propagation and growth to form a compact biological film, so that the treatment efficiency is improved, the other carrier is uniformly dispersed in water to fix pollutants, the impact resistance is improved, the carrier fluidization operation further strengthens the biological treatment capacity, and the treatment efficiency is improved.
At present, researchers mostly carry out a great deal of work on the aspects of carrier material selection, proportioning, carrier modification, immobilization method and the like.
CN201210246151.6 discloses a coupling treatment method for oily sewage in oil field, firstly, the oily sewage is treated by two-stage biological contact oxidation treatment in a biochemical pool to obtain water body to be filtered, and then the water body to be filtered is filtered; in the biological contact oxidation treatment of each level, aeration is adopted at the lower bottom of the biochemical tank, hydrophilic fibrous filler with bacillus adsorbed thereon is adopted above the aeration, oily sewage is introduced into the biochemical tank, and the volume ratio of the aerated gas and the oily sewage, the pH value in the biochemical tank, the content ratio of C, N, P and the dissolved oxygen amount are controlled. The patent can thoroughly remove residual emulsified oil which is not completely removed in the front-end sewage system, improves the efficiency of the biochemical treatment system, and shortens the residence time of sewage in the biochemical treatment system from more than 12 hours to about 8 hours. However, the invention adopts hydrophilic fiber filler with bacillus adsorbed to realize grease removal, and requires matching of specific thalli and materials, and the filler and thalli are combined only through adsorption, so that the binding force needs to be further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method and a device for treating oily sewage. According to the invention, the oil-resistant immobilized carrier and the activated carbon are simultaneously added into the oily sewage treatment system, so that the rapid start and stable operation of the system are realized, and the oil-resistant immobilized carrier and the activated carbon integrated sewage treatment system have the advantages of good comprehensive treatment effect, clear effluent, good long-period operation stability and the like.
The invention provides a treatment method of oily sewage, which mainly comprises two stages of system starting and running, wherein in the starting stage, a filler is added according to the effective volume of a sewage treatment system not less than 50%, preferably 50% -70%, the filler is an activated carbon and oil-resistant immobilized carrier, then activated sludge is inoculated, and a denitrifying bacteria agent is added for stewing and exposure treatment; starting water inflow, wherein the water inflow is oil-containing nitrogen-containing sewage, and continuously running in a mode of gradually increasing water inflow load; when the full-load operation is performed, the system is started when the ammonia nitrogen concentration of the system effluent is less than 1mg/L, TN and less than 15mg/L, COD and less than 30mg/L, and the system is switched into an operation stage; and in the operation stage, filling materials are added every 6-12 months.
In the present invention, the sewage treatment system may employ a biochemical treatment reactor conventionally used in the art, such as A/O, SBR, BAF, and preferably a BAF reactor.
In the present invention, the activated carbon is granular activated carbon for sewage treatment systems, which is well known in the art, and has a particle size of 50-100 mesh.
In the present inventionThe oil-resistant immobilized carrier is prepared according to the following method: (1) Placing the aerogel into acetic acid solution for reaction, taking out and washing to neutrality; (2) Dissolving humic acid in Fe (OH) 3 Adding aerogel into the solution, reacting at 50-70 ℃, and washing to alkalescence to obtain modified aerogel; (3) Loading active metal on the modified aerogel to obtain a metal-loaded carrier; (4) Adsorbing the microorganism producing sugar ester on the carrier loaded with metal, and drying after the adsorption is finished to obtain the immobilized carrier.
The aerogel in the step (1) is at least one of carbon aerogel, silicon aerogel, cellulose aerogel and the like, and preferably the carbon aerogel. Is usually obtained by self-making or commercial purchase, and the specific surface area of the aerogel is 600-1100 m 2 The porosity per gram is 80% -98%.
The concentration of the acetic acid solution in the step (1) is 1.0-2.0 mol/L. Immersing the aerogel in acetic acid solution for reaction, wherein the reaction temperature is 30-50 ℃ and the reaction time is 1.0-2.0 h. The reaction can be carried out by direct heating or water bath heating, preferably water bath heating to 30-50 ℃. After the aerogel is taken out, the aerogel is washed to have neutral pH value, and the pH value is generally 6.5-7.5.
Step (2) the Fe (OH) 3 The concentration of the solution is 0.5 to 0.8mol/L, fe (OH) 3 The mass ratio of the solution to the humic acid is 1:1-3:1.
Step (2) immersing the aerogel in humic acid and Fe (OH) 3 In the mixed system of the solution, the water bath shock reaction is carried out for 3 to 5 hours at the temperature of 50 to 70 ℃. The mixture is taken out and washed until the pH value is slightly alkaline, and is generally 7.6 to 8.0.
The active metal in the step (3) is Cu 2+ 、Fe 2+ 、Mg 2+ At least one of the following, preferably Fe 2+ . The supported active metal may be impregnated using impregnation methods conventionally used in the art, for example, may be used in an equal volume, excess impregnation, etc. A soluble salt solution of the active metal is generally used, wherein the concentration of the metal ions is 1 to 4mol/L. For example, the modified aerogel may be immersed in the active metal solution at 60 to 70 ℃ for 6 to 10 hours.
And (4) immersing the metal-loaded carrier in fermentation liquor of the sugar ester-producing microorganism to perform adsorption growth of thalli, wherein the volume ratio of the metal-loaded carrier to the fermentation liquor is 1:1-3. The adsorption growth conditions are as follows: the temperature is 20-38 ℃, preferably 20-30 ℃, the pH is 6.0-8.5, preferably 6.0-7.0, and the reaction time is 12-36 h.
The microorganism producing sugar ester in the step (4) is a microorganism producing at least one sugar ester of mouse Li Tangzhi, trehalose ester, sophorolipid, sucrose ester and the like by fermentation, for example, can be at least one of pseudomonas aeruginosa producing mouse Li Tangzhi, pseudomonas aeruginosa producing trehalose ester and the like. The preparation of the microbial fermentation broth for sugar ester production is conventional in the art.
And (3) drying in the step (4) at 35-50 ℃ for 24-48 hours to obtain the immobilized carrier. In the synthesized oil-resistant immobilized carrier, the metal content is 1-20% of the mass of the modified aerogel calculated by oxide, the humic acid is 0.1-10% of the mass of the modified aerogel, and the sugar-producing ester microorganism is 5-50% of the mass of the modified aerogel, preferably 10-30%. The synthesized immobilization carrier needs to be preserved in vacuum before use, and the preservation time is generally 1-3 months.
In the invention, the adding volume ratio of the active carbon to the oil-resistant immobilized carrier is 1:1-5.
In the invention, before filling, cobbles with different particle sizes are firstly filled in the reactor as supporting layers, and the height of the supporting layers is 10-50cm.
In the invention, the activated sludge is inoculated according to the proportion of 1000-2000mg/L of the mass of the activated sludge to the total volume of the sewage treatment system. The activated sludge is taken from a secondary sedimentation tank or a biochemical unit of a sewage treatment plant.
According to the invention, the denitrifying bacteria agent is inoculated according to the proportion of 0.01% -0.1% of the volume of the denitrifying bacteria agent to the total volume of the sewage treatment system. The denitrifying bacteria are well known to those skilled in the art and can be formed by combining single strains with conventional ammonia nitrogen removal and total nitrogen removal functions.
In the invention, after the filler, the activated sludge and the denitrifying bacteria are added, the mixture is subjected to stewing and exposure for 5 to 10 days under the condition of 2 to 6mg/L, pH to 7 to 9 dissolved oxygen.
In the invention, the water quality of the oil-containing and nitrogen-containing sewage is as follows: petroleum 15-25mg/L, ammonia nitrogen 50-100mg/L, total nitrogen 60-120mg/L, COD 300-400mg/L, and suspended matter 20-50mg/L.
In the invention, continuous operation is started according to 50% of the water inlet load, and the continuous operation is performed in a mode of gradually increasing the water inlet load until the water inlet load reaches 100% after the water inlet load reaches the standard.
In the invention, the operating conditions of the sewage treatment system in the starting stage and the operating stage are as follows: the dissolved oxygen is more than 2mg/L, the pH value is 7.5-8.5, and the temperature is 25-40 ℃.
In the invention, the filling material is added every 6-12 months in the running process, and the total amount of the filling material is not less than 50%, preferably 50% -70% of the effective volume of the sewage treatment system after the filling material is added.
In the invention, back flushing is carried out every 2-4 months in the operation stage.
The invention also provides a treatment device for the oily sewage treatment method, which mainly comprises a sewage treatment system and a monitoring system, wherein the sewage treatment system is filled with activated carbon and an oil-resistant immobilized carrier and is inoculated with activated sludge and a denitrifying bacteria agent for sewage treatment; the monitoring system is used for monitoring the system effluent, and when the system effluent is in full-load operation, the ammonia nitrogen concentration is less than 1mg/L, TN concentration and the ammonia nitrogen concentration is less than 15mg/L, COD concentration and is less than 30mg/L, the system is started, and the system is shifted to an operation stage.
In the present invention, the sewage treatment system may employ a biochemical treatment reactor conventionally used in the art, such as A/O, SBR, BAF, and preferably a BAF reactor.
Compared with the prior art, the invention has the following beneficial effects:
(1) The oil-resistant immobilized carrier and the activated carbon are added into the oily sewage treatment system simultaneously, and the activated sludge and the denitrifying bacteria agent are added in a combined way, so that the rapid start and stable operation of the system are realized, and the oil-resistant immobilized carrier and the activated carbon combined sewage treatment system has the advantages of good comprehensive treatment effect, clear effluent, good long-period operation stability and the like.
(2) The oil-resistant immobilized carrier has good oil resistance, can keep proper pore channel structure of the filler after being combined with the activated carbon according to a certain proportion, can keep the long-acting property of the filler application when being used in the oily sewage treatment process, avoid blocking oil substances and polluting the pore channel of the carrier, and prolong the back flushing time.
(3) The oil-resistant immobilized carrier has a pore canal structure suitable for adsorption and propagation of functional microorganisms in a treatment system, is favorable for initial adhesion of denitrifying microorganisms on the surface of a filler, can ensure adsorption capacity of decarbonizing and denitrifying microorganisms, and realizes deep treatment of oily sewage. The binding force of each component in the carrier is strong, active metal is not easy to run away, and long-term operation is stable.
Detailed Description
The process and effects of the present invention are described in further detail by the following examples. The embodiments and specific operation procedures are given on the premise of the technical scheme of the invention, but the protection scope of the invention is not limited to the following embodiments.
The experimental methods in the following examples, unless otherwise specified, are all conventional in the art. The experimental materials used in the examples described below, unless otherwise specified, were purchased from conventional biochemical reagent stores.
In the embodiment of the invention, the COD concentration is measured by GB11914-89 'determination of water quality-chemical oxygen demand-dichromate method'; the ammonia nitrogen concentration is measured by using GB7478-87 method for measuring ammonium in water-distillation and titration; the total nitrogen concentration is measured by GB11894-89 water quality-total nitrogen measurement-ultraviolet spectrophotometry; the petroleum is measured by HJ970-2018 'determination of water quality-petroleum-ultraviolet spectrophotometry'; the metal ions are measured by adopting an inductively coupled plasma mass spectrometry; the effluent suspension is measured by GB11901-89 determination of aqueous suspension-gravimetric method.
Example 1
The preparation method of the oil-resistant immobilized carrier adopted by the invention comprises the following steps:
(1) Carbon aerogel (specific surface area 800m 2 Immersing/g with the porosity of 80%) in 1.5mol/L acetic acid solution for water bath reaction at the reaction temperature of 40 ℃, oscillating for 1.5h, taking out, and washing with deionized water to pH7.0 to obtain the pretreated carbon aerogel.
(2) According to Fe (OH) 3 The mass ratio of the solution to the humic acid is 2:1, and the humic acid is dissolved in 0.6mol/L Fe (OH) 3 Adding the pretreated carbon aerogel into the solution, oscillating for 4 hours in a water bath at 60 ℃, taking out, and washing with deionized water to pH8.0 to obtain the modified aerogel.
(3) Preparing ferrous sulfate solution with iron ion concentration of 1mol/L, adding modified aerogel, and soaking for 8 hours under the stirring condition at 65 ℃ to obtain the carrier loaded with active metal.
(4) Mixing the carrier loaded with active metal with the pseudomonas aeruginosa fermentation broth of a mouse Li Tangzhi, wherein the volume ratio of the carrier to the fermentation broth is 1:1. And (3) carrying out adsorption growth for 12 hours at the temperature of 30 ℃ and the pH value of 6.5 to obtain the carrier for adsorbing the pseudomonas aeruginosa. And taking out the carrier adsorbing the microorganisms, and drying at 45 ℃ for 24 hours to finally obtain the immobilized carrier.
The Pseudomonas aeruginosa of mouse Li Tangzhi used in this example was obtained according to the method provided in the literature screening for biosurfactant producer (Pan Bingfeng, microbiology report, 6/1996, 39 (3)). The strain with stable genetic characters and mouse Li Tangzhi is obtained through enrichment culture and screening by utilizing a blood plate, shaking, fermenting and rescreening, and is identified as pseudomonas aeruginosa through 16SrRNA and the like.
The preparation method of the pseudomonas aeruginosa fermentation broth comprises the following steps: the bacterial colony on the inclined plane is picked up and inoculated on LB culture medium, and is cultivated for 24 hours at 37 ℃ and 200rpm to obtain seed liquid, then the seed liquid is inoculated on fermentation culture medium according to 5 percent, and the fermentation liquid is obtained after the seed liquid is cultivated for 7 days at the pH of 6.5 and 35 ℃ and 200 rpm. The formula of the fermentation medium is as follows (in mass percent): glucose 5.0%, yeast extract 0.5%, KH 2 PO 4 、MgSO 4 、FeSO 4 ·7H 2 O and CaCL.2H 2 O was 0.02%.
The sewage treatment system adopts a BAF reactor, and cobbles with different particle sizes are firstly filled in the reactor as a supporting layer, and the height of the supporting layer is 15cm.
In the starting stage, a filler is added according to 60% of the effective volume of a sewage treatment system, the filler is activated carbon (100 meshes) and the oil-resistant immobilized carrier prepared by the invention, the volume ratio of the activated carbon to the oil-resistant immobilized carrier is 1:3, then activated sludge is inoculated according to the ratio of the mass of the activated sludge to the total volume of the sewage treatment system of 1500mg/L, and a denitrifying microbial inoculum is inoculated according to the ratio of the volume of the denitrifying microbial inoculum to the total volume of the sewage treatment system of 0.05% (microbial inoculum 1 prepared by adopting CN2016110729248 example 1) ＃ ) And (5) stewing and exposing for 5 days.
Starting water inflow, wherein petroleum in the water inflow is 20mg/L, ammonia nitrogen concentration is 80mg/L, total nitrogen is 100mg/L, COD concentration is 350mg/L, and suspended matters are 25mg/L.
The operation conditions of the sewage treatment system are as follows: the dissolved oxygen was 3mg/L, the pH was 7.8, and the temperature was 30 ℃.
Firstly, continuously running according to 50% of water inlet load, and continuously running in a mode of gradually increasing the water inlet load until the water inlet load reaches 100% after the water outlet reaches the standard. When the full load operation is carried out, the system effluent ammonia nitrogen concentration is less than 1mg/L, TN concentration and less than 15mg/L, COD concentration and less than 30mg/L, the starting is completed, and the operation stage is shifted; in the operation stage, the filler is added every 8 months, the filler composition is unchanged, and the total amount of the filler is 60% of the effective volume of the sewage treatment system after the filler is added. Back flushing is carried out every 3 months.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the outlet water is 0.6mg/L, the average total nitrogen concentration is 12.3mg/L, and the average COD concentration is 23.5mg/L.
Example 2
The preparation method of the oil-resistant immobilized carrier adopted by the invention comprises the following steps:
(1) Carbon aerogel (specific surface area 800m 2 Immersing/g with the porosity of 80%) in 1mol/L acetic acid solution for water bath reaction at the reaction temperature of 30 ℃, oscillating for 1h, taking out, washing with deionized water to pH6.5, and obtaining the pretreated carbon aerogel.
(2) According to Fe (OH) 3 The mass ratio of the solution to the humic acid was 1:1 and humic acid was added to 0.5mol/LFe (OH) 3 And adding the pretreated carbon aerogel into the solution, oscillating for 3 hours in a water bath at 50 ℃, taking out, and washing with deionized water to pH7.6 to obtain the modified aerogel.
(3) Preparing ferrous sulfate solution with iron ion concentration of 2mol/L, adding the modified aerogel into the solution, and soaking for 6 hours under the stirring condition at 60 ℃ to obtain the load metal carrier.
(4) Mixing the carrier loaded with metal with pseudomonas aeruginosa fermentation broth for producing trehalose grease, wherein the volume ratio of the carrier to the fermentation broth is 1:3. And (3) carrying out adsorption growth for 24 hours at the temperature of 25 ℃ and the pH value of 7.0 to obtain the carrier for adsorbing microorganisms. And taking out the carrier adsorbing the microorganisms, and drying at 35 ℃ for 48 hours to finally obtain the immobilized carrier.
The trehalose ester-producing Pseudomonas aeruginosa used in this example was obtained according to the method provided in the literature screening for biosurfactant-producing bacteria (Pan Bingfeng, microbiology report, 6 th 1996, 39 (3)). The strain which has stable genetic characters and produces the trehalose ester is obtained through enrichment culture and screening by utilizing a blood plate, shaking, fermenting and re-screening, and is identified as pseudomonas aeruginosa through 16SrRNA and the like.
The preparation method of the pseudomonas aeruginosa fermentation broth comprises the following steps: the bacterial colony on the inclined plane is picked up and inoculated on LB culture medium, and is cultivated for 24 hours at 37 ℃ and 200rpm to obtain seed liquid, then the seed liquid is inoculated on fermentation culture medium according to 5 percent, and the fermentation liquid is obtained after the seed liquid is cultivated for 7 days at the pH of 6.8 and 37 ℃ and 200 rpm. The formula of the fermentation medium is as follows (in mass percent): glucose 2.0%, yeast extract 0.5%, peptone 1.0%, KH 2 PO 4 、MgSO 4 、FeSO 4 ·7H 2 O and CaCL.2H 2 O was 0.02%.
The sewage treatment system adopts a BAF reactor, and cobbles with different particle sizes are firstly filled in the reactor as supporting layers, wherein the height of the supporting layers is 35cm.
In the starting stage, 60% of the effective volume of the sewage treatment system is added with filler which is activated carbon (100 meshes) and the sewage treatment systemThe oil-resistant immobilized carrier prepared by the invention has the volume ratio of 1:3, then the activated sludge is inoculated according to the ratio of the mass of the activated sludge to the total volume of the sewage treatment system of 1500mg/L, and the denitrifying bacteria agent (the bacteria agent 1 prepared in the embodiment 1 of CN 2016110729248) is inoculated according to the ratio of the volume of the denitrifying bacteria agent to the total volume of the system of 0.05 percent ＃ ) And (5) stewing and exposing for 5 days.
Starting water inflow, wherein petroleum in the water inflow is 20mg/L, ammonia nitrogen concentration is 80mg/L, total nitrogen is 100mg/L, COD concentration is 350mg/L, and suspended matters are 25mg/L.
The operation conditions of the sewage treatment system are as follows: the dissolved oxygen was 3mg/L, the pH was 7.8, and the temperature was 30 ℃.
Firstly, continuously running according to 50% of water inlet load, and continuously running in a mode of gradually increasing the water inlet load until the water inlet load reaches 100% after the water outlet reaches the standard. When the full load operation is carried out, the system effluent ammonia nitrogen concentration is less than 1mg/L, TN concentration and less than 15mg/L, COD concentration and less than 30mg/L, the starting is completed, and the operation stage is shifted; in the operation stage, the filler is added every 8 months, the filler composition is unchanged, and the total amount of the filler is 60% of the effective volume of the sewage treatment system after the filler is added. Back flushing is carried out every 3 months.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the effluent is 0.8mg/L, the average total nitrogen concentration is 13.6mg/L, and the average COD concentration is 28mg/L.
Example 3
The preparation method of the oil-resistant immobilized carrier is the same as in example 1.
The sewage treatment system adopts a BAF reactor, and cobbles with different particle sizes are firstly filled in the reactor as a supporting layer, and the height of the supporting layer is 15cm.
In the starting stage, filler is added according to 50% of the effective volume of the sewage treatment system, wherein the filler is activated carbon (50 meshes) and the oil-resistant immobilized carrier prepared in the embodiment 1, the volume ratio of the activated carbon to the oil-resistant immobilized carrier is 1:1, then the activated sludge is inoculated according to the ratio of the mass of the activated sludge to the total volume of the sewage treatment system of 1000mg/L, and the volume of the denitrifying bacteria agent to the total volume of the system is adopted0.1% of the denitrifying bacteria (bacteria 1 prepared in example 1 of CN 2016110729248) ＃ ) And (5) stewing and exposing for 10 days.
Starting water inflow, wherein petroleum in the water inflow is 15mg/L, ammonia nitrogen concentration is 50mg/L, total nitrogen is 60mg/L, COD concentration is 300mg/L, and suspended matters are 20mg/L.
The operation conditions of the sewage treatment system are as follows: the dissolved oxygen content was 3.5mg/L, the pH was 8.0, and the temperature was 28 ℃.
Firstly, continuously running according to 50% of water inlet load, and continuously running in a mode of gradually increasing the water inlet load until the water inlet load reaches 100% after the water outlet reaches the standard. When the full load operation is carried out, the system effluent ammonia nitrogen concentration is less than 1mg/L, TN concentration and less than 15mg/L, COD concentration and less than 30mg/L, the starting is completed, and the operation stage is shifted; in the operation stage, the filler is added every 6 months, the filler composition is unchanged, and the total amount of the filler is 50% of the effective volume of the sewage treatment system after the filler is added. Back flushing is carried out every 2 months.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the effluent is 0.91mg/L, the average total nitrogen concentration is 14.1mg/L, and the average COD concentration is 27.1mg/L.
Example 4
The preparation method of the oil-resistant immobilized carrier is the same as in example 1.
The sewage treatment system adopts a BAF reactor, and cobbles with different particle sizes are firstly filled in the reactor as a supporting layer, and the height of the supporting layer is 50cm.
In the starting stage, filling materials are added according to 70% of the effective volume of a sewage treatment system, wherein the filling materials are activated carbon (80 meshes) and an oil-resistant immobilized carrier prepared in the embodiment 1, the volume ratio of the activated carbon to the oil-resistant immobilized carrier is 1:5, then activated sludge is inoculated according to the ratio of the mass of the activated sludge to the total volume of the sewage treatment system of 2000mg/L, and a denitrifying bacterial agent is inoculated according to the ratio of the volume of the denitrifying bacterial agent to the total volume of the system of 0.01% (bacterial agent 1 prepared in the embodiment 1 of CN2016110729248 is adopted) ＃ ) And (5) carrying out stewing and exposure treatment for 7 days.
Starting water inflow, wherein petroleum in the water inflow is 25mg/L, ammonia nitrogen concentration is 100mg/L, total nitrogen is 120mg/L, COD concentration is 400mg/L, and suspended substances are 50mg/L.
The operation conditions of the sewage treatment system are as follows: the dissolved oxygen was 4mg/L, the pH was 7.5, and the temperature was 30 ℃.
Firstly, continuously running according to 50% of water inlet load, and continuously running in a mode of gradually increasing the water inlet load until the water inlet load reaches 100% after the water outlet reaches the standard. When the full load operation is carried out, the system effluent ammonia nitrogen concentration is less than 1mg/L, TN concentration and less than 15mg/L, COD concentration and less than 30mg/L, the starting is completed, and the operation stage is shifted; in the operation stage, the filler is added every 12 months, the filler composition is unchanged, and the total amount of the filler is 70% of the effective volume of the sewage treatment system after the filler is added. Back flushing is carried out every 4 months.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the effluent is 0.89mg/L, the average total nitrogen concentration is 14.4mg/L, and the average COD concentration is 27.8mg/L.
Example 5
The difference from example 1 is that: in the preparation method of the oil-resistant immobilized carrier, silicon aerogel is adopted to replace carbon aerogel, and the specific surface area of the silicon aerogel is 1000m 2 And/g, wherein the porosity is 85%, and finally the oil-resistant immobilized carrier is prepared.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the outlet water is 0.98mg/L, the average total nitrogen concentration is 14.7mg/L, and the average COD concentration is 28.5mg/L.
Example 6
The difference from example 1 is that: in the preparation method of the oil-resistant immobilized carrier, cellulose aerogel is adopted to replace carbon aerogel, and the specific surface area of the cellulose aerogel is 900m 2 And/g, wherein the porosity is 95%, and finally the immobilized carrier is prepared.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the outlet water is 0.96mg/L, the average total nitrogen concentration is 13.3mg/L, and the average COD concentration is 28.1mg/L.
Example 7
The difference is that in example 1In the following steps: in the preparation method of the oil-resistant immobilized carrier, cu is adopted as metal ions 2+ Preparing a copper chloride solution with the concentration of 3mol/L to replace the ferric sulfate solution, and finally preparing the immobilized carrier.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the outlet water is 0.95mg/L, the average total nitrogen concentration is 13.6mg/L, and the average COD concentration is 28.7mg/L.
Example 8
The difference from example 1 is that: in the preparation method of the oil-resistant immobilized carrier, the metal ion adopts Mg 2+ A magnesium sulfate solution of 4mol/L was prepared instead of the ferric sulfate solution. Finally, the immobilized carrier is prepared.
After one year of operation, the system treatment effect is stable, the average ammonia nitrogen concentration of the outlet water is 0.98mg/L, the average total nitrogen concentration is 14.3mg/L, and the average COD concentration is 29.3mg/L.
Comparative example 1
The difference from example 1 is that: the sewage treatment system does not adopt the oil-resistant immobilized carrier prepared by the application, and only adopts granular activated carbon. After one year operation, the average ammonia nitrogen concentration of the system output water is 16.9mg/L, the average total nitrogen concentration is 29.7mg/L and the average COD concentration is 39.3mg/L due to the influence of petroleum substances.
Comparative example 2
The difference from example 1 is that: the sewage treatment system does not adopt activated carbon and only adopts the immobilized carrier prepared by the application. After one year operation, the average ammonia nitrogen concentration of the system outlet is 10.6mg/L, the average total nitrogen concentration is 20.9mg/L and the average COD concentration is 35.5mg/L because the proper pore canal structure of the filler cannot be maintained.
Comparative example 3
The difference from example 1 is that: volcanic rock filler is adopted in the BAF reactor to replace the combined filler of the activated carbon and the immobilized carrier. After one year of operation, the average ammonia nitrogen concentration of the system outlet water is 23.4mg/L, the average total nitrogen concentration is 29.8mg/L, and the average COD concentration is 45.5mg/L.
Comparative example 4
The difference from example 1 is that: only activated sludge is inoculated in the sewage treatment system, and no denitrifying bacteria agent is inoculated. After one year of operation, the average ammonia nitrogen concentration of the system outlet water is 11.7mg/L, the average total nitrogen concentration is 23.5mg/L, and the average COD concentration is 37.6mg/L.
Comparative example 5
The difference from example 1 is that: in the preparation process of the immobilization carrier, the step (3) is to modify aerogel without loading metal ions, and finally obtain the immobilization carrier. After one year of operation, the average ammonia nitrogen concentration of the system outlet water is 12.3mg/L, the average total nitrogen concentration is 24.7mg/L, and the average COD concentration is 36.9mg/L.
Comparative example 6
The difference from example 1 is that: in the preparation process of the immobilized carrier, the step (4) adopts rhamnolipid to replace pseudomonas aeruginosa fermentation broth for producing rhamnolipid, and finally the immobilized carrier is prepared. After one year operation, the average ammonia nitrogen concentration of the system outlet water is 14.3mg/L, the average total nitrogen concentration is 28.8mg/L, the average suspended matter concentration is 67mg/L, and the average COD concentration is 46.3mg/L.

Claims (35)

1. The treatment method of the oily sewage is characterized by comprising two stages of starting and running, wherein in the starting stage, a filler is added according to the effective volume of a sewage treatment system of not less than 50%, the filler is an activated carbon and an oil-resistant immobilized carrier, then activated sludge is inoculated, a denitrifying bacteria agent is added, and stewing and exposure treatment are carried out; starting water inflow, wherein the water inflow is oil-containing nitrogen-containing sewage, and continuously running in a mode of gradually increasing water inflow load; when the full-load operation is performed, the system is started when the ammonia nitrogen concentration of the system effluent is less than 1mg/L, TN and less than 15mg/L, COD and less than 30mg/L, and the system is switched into an operation stage; in the operation stage, filling materials are added every 6-12 months;
the oil-resistant immobilized carrier is prepared according to the following steps: (1) Placing the aerogel into acetic acid solution for reaction, taking out and washing to neutrality; (2) Dissolving humic acid in Fe (OH) 3 Adding aerogel into the solution, reacting at 50-70 ℃, and washing to alkalescence to obtain modified aerogel; (3) Loading active metal on modified aerogel to obtain loadA metal support; (4) Adsorbing the microorganism producing sugar ester on the carrier loaded with metal, and drying after the adsorption is finished to obtain the immobilized carrier.
2. The method according to claim 1, characterized in that: adding filler according to the effective volume of the sewage treatment system of 50% -70%.
3. The method according to claim 1, characterized in that: the sewage treatment system adopts an A/O, SBR, BAF biochemical treatment reactor.
4. A method according to claim 3, characterized in that: the sewage treatment system adopts a BAF reactor.
5. The method according to claim 1, characterized in that: the active carbon is granular active carbon with the grain diameter of 50-100 meshes.
6. The method according to claim 1, characterized in that: the aerogel in the step (1) is at least one of carbon aerogel, silicon aerogel and cellulose aerogel.
7. The method according to claim 6, wherein: the aerogel in the step (1) is carbon aerogel.
8. The method according to claim 6 or 7, characterized in that: the specific surface area of the aerogel is 600-1100 m 2 The porosity per gram is 80% -98%.
9. The method according to claim 1, characterized in that: the concentration of the acetic acid solution in the step (1) is 1.0-2.0 mol/L; immersing the aerogel in acetic acid solution for reaction, wherein the reaction temperature is 30-50 ℃ and the reaction time is 1.0-2.0 h.
10. The method according to claim 1, characterized in that: step by stepStep (2) the Fe (OH) 3 The concentration of the solution is 0.5 to 0.8mol/L, fe (OH) 3 The mass ratio of the solution to the humic acid is 1:1-3:1.
11. The method according to claim 1, characterized in that: step (2) immersing the aerogel in humic acid and Fe (OH) 3 In the mixed system of the solution, carrying out water bath oscillation reaction for 3-5 h at 50-70 ℃; and taking out and washing until the pH value is alkalescent.
12. The method according to claim 11, wherein: taking out and washing until the pH value is 7.6-8.0.
13. The method according to claim 1, characterized in that: the active metal in the step (3) is Cu 2+ 、Fe 2+ 、Mg 2+ At least one of them.
14. The method according to claim 13, wherein: the active metal in the step (3) is Fe 2+ 。
15. The method according to claim 1 or 13 or 14, characterized in that: and (3) adopting a soluble salt solution of active metal, wherein the concentration of metal ions is 1-4 mol/, and soaking for 6-10 h at 60-70 ℃.
16. The method according to claim 1, characterized in that: and (4) immersing the metal-loaded carrier in fermentation liquor of the sugar ester-producing microorganism to perform adsorption growth of thalli, wherein the volume ratio of the metal-loaded carrier to the fermentation liquor is 1:1-3.
17. The method according to claim 1 or 16, characterized in that: the adsorption growth conditions in the step (4) are as follows: the temperature is 20-38 ℃, the pH is 6.0-8.5, and the reaction time is 12-36 h.
18. The method according to claim 17, wherein: the temperature is 20-30 ℃, and the pH is 6.0-7.0.
19. The method according to claim 1, characterized in that: the sugar ester-producing microorganism in the step (4) is a microorganism which ferments and produces at least one sugar ester of mouse Li Tangzhi, trehalose ester, sophorolipid and sucrose ester.
20. The method according to claim 19, wherein: the sugar ester-producing microorganism in the step (4) is at least one of Pseudomonas aeruginosa producing mice Li Tangzhi and Pseudomonas aeruginosa producing trehalose esters.
21. The method according to claim 1, characterized in that: and (3) drying in the step (4) at 35-50 ℃ for 24-48 hours to obtain the immobilized carrier.
22. The method according to claim 1, characterized in that: in the synthesized oil-resistant immobilized carrier, the metal content is 1-20% of the mass of the modified aerogel calculated by oxide, the humic acid is 0.1-10% of the mass of the modified aerogel, and the sugar-ester-producing microorganism is 5-50% of the mass of the modified aerogel.
23. The method as claimed in claim 22, wherein: the sugar ester-producing microorganisms account for 10% -30% of the mass of the modified aerogel.
24. The method according to claim 1, characterized in that: the adding volume ratio of the activated carbon to the oil-resistant immobilized carrier is 1:1-5.
25. The method according to claim 1, characterized in that: before filling, cobbles with different particle sizes are filled in the reactor as supporting layers with the height of 10-50cm.
26. The method according to claim 1, characterized in that: inoculating the activated sludge according to the proportion of 1000-2000mg/L of the mass of the activated sludge to the total volume of the sewage treatment system.
27. The method according to claim 1, characterized in that: inoculating the denitrifying bacteria agent according to the ratio of 0.01% -0.1% of the volume of the denitrifying bacteria agent to the total volume of the sewage treatment system.
28. The method according to claim 1, characterized in that: after the filler, the activated sludge and the denitrifying bacteria agent are added, the mixture is subjected to stewing and exposure for 5 to 10 days under the condition of 2 to 6mg/L, pH to 9 of dissolved oxygen.
29. The method according to claim 1, characterized in that: the water quality of the oil-containing and nitrogen-containing sewage is as follows: petroleum 15-25mg/L, ammonia nitrogen 50-100mg/L, total nitrogen 60-120mg/L, COD 300-400mg/L, and suspended matter 20-50mg/L.
30. The method according to claim 1, characterized in that: firstly, starting continuous operation according to 50% of water inlet load, and continuously operating in a mode of gradually increasing the water inlet load until the water inlet load reaches 100% after the water outlet reaches the standard.
31. The method according to claim 1, characterized in that: the operating conditions of the sewage treatment system are as follows: the dissolved oxygen is more than 2mg/L, the pH value is 7.5-8.5, and the temperature is 25-40 ℃.
32. The method according to claim 1, characterized in that: and filling materials are added every 6-12 months in the operation process, wherein the adding amount is that the total amount of the filling materials is not less than 50% of the effective volume of the sewage treatment system after the adding.
33. The method as claimed in claim 32, wherein: the adding amount is that the total amount of the filling material is 50% -70% of the effective volume of the sewage treatment system after adding.
34. The method according to claim 1, characterized in that: and in the operation stage, back flushing is carried out every 2-4 months.
35. A treatment device for the oily sewage treatment method of any one of claims 1 to 34, the treatment device comprising a sewage treatment system and a monitoring system, the sewage treatment system being filled with activated carbon and an oil-resistant immobilized carrier and being inoculated with activated sludge and a denitrifying bacteria agent for sewage treatment; the monitoring system is used for monitoring the system effluent, and when the system effluent is in full-load operation, the ammonia nitrogen concentration is less than 1mg/L, TN concentration and the ammonia nitrogen concentration is less than 15mg/L, COD concentration and is less than 30mg/L, the system is started, and the system is shifted to an operation stage.
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