CN105967388A - Method for removing emulsified oil in oil field oily wastewater - Google Patents

Method for removing emulsified oil in oil field oily wastewater Download PDF

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Publication number
CN105967388A
CN105967388A CN201610368916.1A CN201610368916A CN105967388A CN 105967388 A CN105967388 A CN 105967388A CN 201610368916 A CN201610368916 A CN 201610368916A CN 105967388 A CN105967388 A CN 105967388A
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oil
value
oil emulsion
waste water
oily wastewater
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吴涛
陈晓蕾
孙德军
李玉江
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Shandong University
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Shandong University
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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
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • 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
    • C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
    • 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
    • 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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • 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
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • 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
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/06—Controlling or monitoring parameters in water treatment pH

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Water Treatment By Sorption (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

A method for removing emulsified oil in oil field oily wastewater comprises the following steps that firstly, according to the proportion of 1-1.5 g of industrial waste residues and 10-20 mL of hydrochloric acid or diluted sulphuric acid, white mud is soaked in hydrochloric acid with the concentration of 1.2-1.5 mol/L or diluted sulphuric acid with the mass concentration of 15%-20% for 24 h, and filter liquor obtained after filtering is a treating agent; secondly, oily wastewater containing emulsified oil is subjected to pH value measuring, the oily wastewater is not treated when the pH value is 9.5-12.5, and otherwise the pH value of the oily wastewater is regulated to be 9.5-12.5 with a pH regulating agent; thirdly, the treating agent is added into the oily wastewater with the pH value being 9.5-12.5 at the adding amount of 0.5-6.0 g/L, the reaction temperature is controlled to be 10-70 DEG C, stirring is carried out for 0.5-10 min at the stirring speed of 150-200 turns/min, and then centrifugal sedimentation is carried out for 10-15 min. The method is simple, low in equipment investment, convenient to implement, suitable for enterprises to treat wastewater in a large scale and high in treatment efficiency.

Description

A kind of remove the method for oil emulsion in oil-containing wastewater
Technical field
The present invention relates to a kind of for removing the method for oil emulsion in oil-containing wastewater, belong to technical field of sewage.
Background technology
Oil exploitation is one of main path obtaining the energy.In recent years, along with the lasting rising of oil demand amount, research worker Develop many technology strengthening oil exploitation.Along with the fast development of tertiary oil recovery technology, the increasing reinforcement displacement of reservoir oil and increasing The technology adding oil recovery factor is applied to each elephant, meets national economy to oil day by day with the oil production rate of steady growth The dependence increased and demand.High oil recovery factor stems from the improvement to displacing fluid character of the various chemical substances of interpolation, adds Chemical substance include alkali, surfactant and polymer.Be added to and the organic acid in crude oil of alkali (Alkali) are sent out Raw reaction, in-situ preparation has the petroleum soap of surface activity to reduce oil-water interfacial tension；Surfactant (Surfactant) Use partly in order to improve the wettability of rock surface, on the other hand improve crude oil mobility in the earth formation, be permissible Substantially reduce oil-water interfacial tension；The effect of polymer (Polymer) is then to increase the viscosity of displacing fluid, improves oil-water Flowing ratio, improves " volume is swept " effect.The use if Alkali, Surfactant and Polymer three combines, crude oil Recovery ratio can be further improved, this technology is referred to as " ternary composite driving " technology (Alkali/Surfactant /Polymer flooding,ASP flooding).ASP flooding is to strengthen the displacement of reservoir oil and increase the weight of oil recovery factor Want one of technology.After ASP flooding drilling technology completes, thus produce the substantial amounts of liquid wastes containing oil emulsion, Possibly together with surfactant, polymer, the clay particle of suspension and the Organic substance of residual in liquid wastes.These refuses have good Good hydrophilic, under pressure, they are uniformly dispersed in aqueous phase and form stable O/w emulsion, this emulsion It is referred to as output water or oily waste water.In the presence of having surfactant and polymer, oil emulsion (crude oil after emulsifying) It is difficult to remove from output water；Meanwhile, the biological degradability of oil is very poor, needs to expend the very long time and just has the probability of degraded. If this kind of discharge of wastewater enters reclaims water body, the existence of oil emulsion can cause the detergent power of water body, solubilising power and transmittability It is decreased obviously, and BOD (BOD) and COD (COD) substantially rise, make recovery water body be extremely difficult to re-injection With the requirement reused.Under normal circumstances, oil can be present in water body water environment generation pollution in two kinds of modes: freely oil And oil emulsion.Free oil is not a big problem, because the freest oil can float to the top of water body, passes through Oil scraper just can remove；But oil emulsion is but a real big problem, because oil emulsion is all with oil-in-water in water body (O/W) or presented in Water-In-Oil (W/O) emulsion, it is difficult to accomplish oil-water separation.The content of oil emulsion is reduced to certain After standard, output water just can be recycled into underground and reuse.So, output water is before re-injection, and oil emulsion must quickly have Removing from output water of effect, otherwise oil emulsion not only produces harm to water environment, and also brings along infringement to running facility.
In traditional removal output water or oily waste water, the method for oil emulsion includes biological treatment, gas flotation, coagulation and electrochemistry Coagulation, filter bed and filter membrane isolation technics.But, existing treatment technology generally exist process excessive cycle, removal efficiency low, Equipment investment is big, filter bed and filter membrane are easily contaminated needs repeatedly to rinse and the shortcoming such as replacing, and be not suitable for oil emulsion content high, Oily field produced water that water yield is big or the process of oily waste water.
Summary of the invention
The present invention is directed to the shortcoming and defect that in existing oil field produced water or oily waste water, oil emulsion treatment technology exists, it is provided that one The method of oil emulsion in the removal oil-containing wastewater that the process of kind is simple, low cost, treatment effeciency are high.
The present invention removes the method for oil emulsion in oil-containing wastewater, comprises the following steps:
(1) inorganic agent is prepared:
The dilute sulfuric acid taking industrial residue white clay and the hydrochloric acid of concentration 1.2mol/L-1.5mol/L or mass concentration 15%-20% is former material Material, in 1g-1.5g white clay and 10mL-20mL hydrochloric acid or the ratio of dilute sulfuric acid, soaks 24 in hydrochloric acid or dilute sulfuric acid by white clay Hour, after filtration, gained filtrate is inorganic agent (LSWM, the leachate of white clay)；
(2) oily waste water containing oil emulsion is carried out pH value mensuration, do not enter when the pH value of oily waste water is 9.5-12.5 Row processes, and the pH value otherwise regulating oily waste water reaches 9.5-12.5；
The regulator of regulation pH value is hydrochloric acid (HCl), sodium hydroxide (NaOH) and calcium hydroxide (Ca (OH)2One in).
(3) co-precipitation-adsorption process:
In the oily waste water that pH value is 9.5-12.5, inorganic agent, reaction temperature is added according to the dosage of 0.5g/L-6.0g/L Control at 10 DEG C-70 DEG C, stir 0.5 minute-10 minutes under the mixing speed of 150-200 rev/min；It is then centrifuged for sedimentation 10-15 minute.
Inorganic agent once contacts with oily waste water, soluble metallic salt (CaCO in inorganic agent3,Mg(OH)2,Al2O3, FeO etc.) The M dissociateed2+/M3+Metal cation and OH-Ion collides under the effect of stirring, gradually forms sepia cotton-shaped Precipitation.Containing substantial amounts of Ca in inorganic agent2+、Mg2+、Fe2+、Al3+Deng metal cation, contain when inorganic agent joins alkalescence In oil waste water, M2+/M3+With OH-Chemical reaction is occurred to generate MOH+、M(OH)2+With M (OH)2 +Compound ion； When the concentration of these compound ions reaches to a certain degree, they will form little nucleus, becomes M (OH)2/M(OH)3 The center of precipitation growth, constantly nucleation and growth, gradually grow into the M (OH) of large-size2/M(OH)3Precipitation；? M(OH)2/M(OH)3In precipitation growth course, due to MOH+、M(OH)2+With M (OH)2 +Compound ion has ratio M(OH)2/M(OH)3Higher positive charge, therefore these compound ions and the emulsified oil droplet of oppositely charged The strongest electrostatic attraction effect is there is between (Emulsified Oil Droplets, EOs)；Meanwhile, M(OH)2/M(OH)3Precipitation granule also has the strongest adhesive attraction with EOs；Therefore, generate in position M(OH)2/M(OH)3During precipitation, EOs does not adsorb only on the surface of precipitation granule, and directly embeds entrance Main M (OH)2/M(OH)3Precipitation, defines M (OH)2/M(OH)3-EOs sediment composite； M(OH)2/M(OH)3-EOs sediment composite is by electrostatic, hydrogen bond and adhesive attraction and surrounding M(OH)2/M(OH)3Proceeding reaction with EOs, gradually formed big cotton-shaped aggregation, aggregation is the biggest, just The easiest separate from water body, thus reach to remove the purpose of oil emulsion, here it is co-precipitation-adsorption process.
Separate and collect the cotton-shaped aggregation after step (3) centrifugal sedimentation, the supernatant after co-precipitation-adsorption process is processed Carrying out remaining the mensuration of oil emulsion concentration, in oily waste water, the oil emulsion of residual can be by carbon tetrachloride, gasoline, petroleum ether and three Any one of chloromethanes organic solvent extracts, and the color of extract is linear with the concentration of oil content, therefore can use The method of colorimetric is measured；Waste water process up to standard after discharge, otherwise adjust inorganic agent dosage until up to standard.
For oily waste water, time of contact is an important influence factor, selects not only improve place a suitable time of contact Reason agent and oily waste water mix homogeneously, be also beneficial to the chemical reaction of inorganic agent and oil emulsion, also, it helps big gathering The generation of body.The length of time of contact directly affects oil emulsion content in water outlet, and relatively short period of time is not enough to remove oil emulsion, but It is difficult to accept in holdup time long technological process；Secondly, inorganic agent dosage, pH value, reaction temperature are also to affect oily waste water One of key factor that in water, oil emulsion is removed.
The present invention uses the leachate of cheap industrial residue white clay as inorganic agent, uses co-precipitation-adsorption process to tie mutually The one-step method closed, as main technique operating process, is suitable for the extensive line production of enterprise, easy and simple to handle, to different water project situation With being well adapted for property of temperature range.There is the highest efficiency for the removal of oil emulsion in oily waste water, decrease underground The pollution of water；The oil emulsion that what is more important is separated can reclaim, and re-uses as a kind of regenerative resource.
Accompanying drawing explanation
Fig. 1 is the M (OH) that situ of the present invention generates2/M(OH)3Precipitate (Fig. 1 (a)) and through co-precipitation-adsorption process The M (OH) formed with EOs afterwards2/M(OH)3-EOs the sediment composite (Fig. 1 (b)) electricity under high-resolution-ration transmission electric-lens Mirror photo (amplification 20000 times).
Fig. 2 is M in the present invention (OH)2/M(OH)3Precipitation with simulated oily wastewater change with system pH time precipitation granule and Change (excursion of pH value the is 9.5-12.5) schematic diagram of EOs surface charge density.
Fig. 3 is the schematic diagram that in embodiment 1, the clearance of oil emulsion changes with the change of inorganic agent dosage.
Fig. 4 is the schematic diagram that in embodiment 2, the clearance of oil emulsion changes with the change of system pH.
Fig. 5 is the schematic diagram that in embodiment 3, the clearance of oil emulsion changes with the change of time of contact.Wherein Fig. 5 (a) is The clearance of oil emulsion is with the visual effect photo changed time of contact；Fig. 5 (b) is that the clearance of oil emulsion became with time of contact The curve chart changed.
Fig. 6 is that (range of temperature is the schematic diagram that in embodiment 4, the clearance of oil emulsion changes with the change of reaction temperature 10-70℃)。
Fig. 7 is EOs fluorescent microscopy images (amplification 800 times) in simulated oily wastewater in embodiment 5.
Detailed description of the invention
Simulated oily wastewater used by each embodiment is prepared by procedure below:
Sodium hydroxide, crude oil and mineralized water is taken in the ratio of 1g:3g:1997mL.Described mineralized water is according to Shengli Oil field The composition of lower water mineral is prepared, and the total salinity of mineralized water is 3380mg/L, and wherein the concentration of NaCl is 1600mg/L, NaHCO3Concentration be 1600mg/L, Na2CO3Concentration be 100mg/L, CaCl2Concentration be 40mg/L, MgCl2 Concentration be 40mg/L.Mineralized water contains the surfactant (dodecylbenzene sodium sulfonate, SDBS) of mass percent 0.2% With 0.1% polymer (PAMA, HPAM).
Being joined by crude oil in mineralized water, on magnetic stirring apparatus, the rotating speed with 150-200 rev/min stirs 15-20 minute, Add sodium hydroxide, become mixed system.Then, under the rotating speed of 8000-10000 rev/min, above-mentioned mixed system is put Emulsifying 30-40 minute in mulser, is allowed to form stable O/W emulsion, and this emulsion is simulated oily wastewater, oil content For 1500mg/L.
Inorganic agent in each embodiment is to be prepared by procedure below:
Take the industrial residue white clay of aluminium manufacturer and the hydrochloric acid of concentration 1.2mol/L-1.5mol/L or the dilute sulfuric acid of mass concentration 15%-20% For raw material, in 1g-1.5g white clay and 10mL 20mL hydrochloric acid or the ratio of dilute sulfuric acid, by white clay in hydrochloric acid or dilute sulfuric acid Soaking 24 hours, after filtration, gained filtrate is inorganic agent (LSWM, the leachate of white clay).
Embodiment 1
Taking simulated oily wastewater 1000mL, the initial concentration of oil emulsion is 1500mg/L, temperature 30 DEG C.Employing pH adjusting agent is adjusted The pH=12.5 of joint simulated oily wastewater, pH adjusting agent is HCl, NaOH and Ca (OH)2In one.By 0.5-6.0g/L's Dosage adds inorganic agent in simulated oily wastewater, maintains mixing speed 150-200 rev/min, stirs 0.5-10 minute, It is then centrifuged for sedimentation 10-15 minute, collects the supernatant, carry out remaining the mensuration of oil emulsion concentration.
Result of implementation shows: the clearance of oil emulsion increases, as it is shown on figure 3, work as inorganic agent with the increase of inorganic agent dosage When dosage is 4.0g/L, the clearance of oil emulsion has reached 98.58%, along with the further increase of inorganic agent dosage, breast The clearance of carburetion the most significantly rises.Therefore, the optimum dosage of inorganic agent is 4.0g/L.Oil emulsion does not adsorbs only on M(OH)2/M(OH)3The surface of granule, and embed the main M of entrance (OH)2/M(OH)3, precipitation generates M(OH)2/M(OH)3-EOs sediment composite, as shown in Figure 1.
Embodiment 2
Take simulated oily wastewater 1000mL, the initial concentration 1500mg/L of oil emulsion, temperature 30 DEG C.Employing pH adjusting agent regulates The pH value of simulated oily wastewater is respectively 9.5,10.0,10.5,11.0,11.5,12.0 and 12.5；PH adjusting agent be HCl, NaOH and Ca (OH)2In one.In oily waste water, add inorganic agent by the dosage of 4.0g/L, maintain mixing speed 150-200 rev/min, stir 0.5-10 minute, be then centrifuged for sedimentation 10-15 minute, collect the supernatant, remain The mensuration of oil emulsion concentration.
Result of implementation shows: the clearance of oil emulsion increases with the increase of pH value, as shown in Figure 4.As pH=12.5, The clearance of oil emulsion reaches maximum.Therefore, pH=12.5 is Optimal pH condition.This is with M (OH)2/M(OH)3Precipitation and The surface charge density of emulsified oil droplet changes relevant with the change of pH.As in figure 2 it is shown, at temperature 30 DEG C, pH value model When enclosing for 9.5-12.5, M (OH)2/M(OH)3Precipitation electropositive increasing always, be when pH=12.5 slightly under Fall；And the negative charge density on emulsified oil droplet surface is increasing the most always, i.e. elecrtonegativity strengthens, as shown in Figure 2.Deposit between them In the strongest electrostatic attraction effect, adding the synergism of hydrogen bond and adhesion, the removal of oil emulsion can reach gratifying Effect.
Embodiment 3
Take simulated oily wastewater 1000mL, the initial concentration 1500mg/L of oil emulsion, pH=12.5, temperature 30 DEG C.By 4.0g/L Dosage in oily waste water, add inorganic agent, maintain mixing speed 150-200 rev/min, control at 0.5-10 time of contact Minute, it is then centrifuged for sedimentation 10-15 minute, collects the supernatant, carry out remaining the mensuration of oil emulsion concentration.
Result of implementation shows: when time of contact is 1 minute, and the removal effect of oil emulsion is the most clearly；Increase between when contacting It is added to the close balance of the removal of oil emulsion when 6 minutes.As it is shown in figure 5, wherein Fig. 5 (a) is that the clearance of oil emulsion is with connecing The visual effect photo of the time of touching change；Fig. 5 (b) is the curve chart that the clearance of oil emulsion changed with time of contact.
Co-precipitation-adsorption process is one method fast and effectively for the removal of oil emulsion in oily waste water.
Embodiment 4
Take simulated oily wastewater 1000mL, the initial concentration 1500mg/L of oil emulsion, pH=12.5, reaction temperature control 10 DEG C, 30 DEG C, 50 DEG C and 70 DEG C.In oily waste water, add inorganic agent by the dosage of 4.0g/L, maintain mixing speed 150-200 Rev/min, mixing time 0.5-10 minute, it is then centrifuged for sedimentation 10-15 minute, collects the supernatant, carry out remaining emulsifying The mensuration of oil concentration.
Result of implementation shows: reduces temperature, contributes to the removal of oil emulsion, determine the process removing oil emulsion from oily waste water It it is exothermic reaction.As shown in Figure 6.Removing of oil emulsion is closely related with its dissolubility in aqueous phase.Temperature raises and adds O/W emulsion intercalation method, it is meant that oil emulsion dissolubility in aqueous phase with temperature raise and raise, cause oil emulsion be more difficult to from Oily waste water is removed.
Embodiment 5
Taking 4 parts of simulated oily wastewater, every part of oily waste water 200mL respectively, the initial concentration of oil emulsion is 1500mg/L, PH=12.5.The temperature of 4 parts of oily waste waters controls respectively 10 DEG C, 30 DEG C, 50 DEG C and 70 DEG C.Use fluorescence microscope Oil droplet existence in oily waste water under different temperatures.
Result shows: at a lower temperature such as 10 DEG C and 30 DEG C, and oil droplet size becomes greatly and is gathered into bigger bunch, easily from water Separate in mutually；Such as 50 DEG C at a temperature of higher, oil droplet size diminishes, and dissolubility increases；It is warmed up to 70 DEG C, oil droplet grain It is the least that footpath has become, and has been substantially dissolved in aqueous phase, defines highly stable emulsion.The clearance of this oil emulsion just The reason raised with temperature and decline.Fig. 7 gives EOs fluorescent microscopy images in simulated oily wastewater in the present embodiment (amplification 800 times).

Claims (1)

1. remove a method for oil emulsion in oil-containing wastewater, it is characterized in that, comprise the following steps:
(1) inorganic agent is prepared:
The dilute sulfuric acid taking industrial residue white clay and the hydrochloric acid of concentration 1.2mol/L-1.5mol/L or mass concentration 15%-20% is former material Material, in 1g-1.5g white clay and 10mL-20mL hydrochloric acid or the ratio of dilute sulfuric acid, soaks 24 little in hydrochloric acid or dilute sulfuric acid by white clay Time, after filtration, gained filtrate is inorganic agent；
(2) oily waste water containing oil emulsion is carried out pH value mensuration, do not carry out when the pH value of oily waste water is 9.5-12.5 Processing, the pH value otherwise regulating oily waste water reaches 9.5-12.5；
(3) co-precipitation-adsorption process:
In the oily waste water that pH value is 9.5-12.5, inorganic agent, reaction temperature is added according to the dosage of 0.5g/L-6.0g/L Control at 10 DEG C-70 DEG C, stir 0.5 minute-10 minutes under the mixing speed of 150-200 rev/min；It is then centrifuged for sedimentation 10-15 minute.
CN201610368916.1A 2016-05-27 2016-05-27 Method for removing emulsified oil in oil field oily wastewater Pending CN105967388A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1605374A (en) * 2004-09-09 2005-04-13 上海交通大学 Fluid cavitation and emulsion breaking method
CN101428877A (en) * 2008-12-10 2009-05-13 周才华 Method for removing roily oil from degreasing waste liquor in coating wastewater
CN101659482A (en) * 2009-09-27 2010-03-03 山东大学 Method for treating alkaline surfactant polymer flooding oil-field wastewater
CN101665289A (en) * 2009-09-27 2010-03-10 山东大学 Treatment method of polymer flooding water of oil field

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1605374A (en) * 2004-09-09 2005-04-13 上海交通大学 Fluid cavitation and emulsion breaking method
CN101428877A (en) * 2008-12-10 2009-05-13 周才华 Method for removing roily oil from degreasing waste liquor in coating wastewater
CN101659482A (en) * 2009-09-27 2010-03-03 山东大学 Method for treating alkaline surfactant polymer flooding oil-field wastewater
CN101665289A (en) * 2009-09-27 2010-03-10 山东大学 Treatment method of polymer flooding water of oil field

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