CN108579679A - A method of oil emulsion in the oil-in-water emulsion that removal surfactant is stablized - Google Patents

A method of oil emulsion in the oil-in-water emulsion that removal surfactant is stablized Download PDF

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CN108579679A
CN108579679A CN201810479415.XA CN201810479415A CN108579679A CN 108579679 A CN108579679 A CN 108579679A CN 201810479415 A CN201810479415 A CN 201810479415A CN 108579679 A CN108579679 A CN 108579679A
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oil
emulsion
stablized
water
mgo
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吴涛
刘文文
李玉江
孙德军
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Shandong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009Magnetic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/48Treatment of water, waste water, or sewage with magnetic or electric fields
    • C02F1/488Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation

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

Abstract

A method of oil emulsion in the oil-in-water emulsion that removal surfactant is stablized includes the following steps:(1) graphene oxide, ferric trichloride/ferrous sulfate mixing salt solution and layered double hydroxide colloidal sol are taken, it adds graphene oxide into ferric trichloride/ferrous sulfate mixing salt solution, the pH to 10 11 for adjusting solution, is persistently stirred at a temperature of 80 95 DEG C;Washing filtering, is dried in vacuo at 50 65 DEG C, obtains ferroso-ferric oxide graphene oxide hybrid;MGO is mixed with LDH colloidal sols, and is persistently stirred at 10 40 DEG C, filtering cleaning is magnetic adsorbent after dry;(2) ionic strength for the oil-in-water emulsion that surfactant is stablized is adjusted;(3) magnetic adsorbent is added in the O/W lotions stablized to surfactant, is stirred at 10 40 DEG C, then the Magneto separate in the case where adding magnetic fields outside.This method safety, easy to operate, equipment investment is few, floor space is small, and removal efficiency is high, is suitble to continuous extensive processing oily waste water.

Description

A method of oil emulsion in the oil-in-water emulsion that removal surfactant is stablized
Technical field
The present invention relates to a kind of methods of oil emulsion in oil-in-water emulsion that removal surfactant is stablized, and belong at sewage Manage technical field.
Background technology
The processing of oil-in-water (oil-in-water, O/W) lotion that oiliness sewage treatment, especially surfactant are stablized It is a global challenge.Surfactant (surfactant) is a major class organic compound, they can change system Interface composition and structure, become people and change that liquid-liquid, liquid-solid and solid-solid interface interfacial property to be to adapt to the weight of various requirement Want means.Surfactant often by technical staff as auxiliary agent or additive application in industrial quarters.Engine used in automobile Drilling mud or oil displacement agent used in oil, laundry detergent used when taking and doing housework, petroleum industry, people take when sick Drug and when ore dressing flotation agent used in have surfactant.Surfactant is primarily present in liquid phase medium In oil-in-water emulsion and play a role.It, will be with liquid wastes once these oil-in-water emulsions lose original function and property Form be discharged into surface water body or enter sewage treatment plant, therefore, the oil-in-water that oily waste water or surfactant are stablized Lotion is mainly derived from our daily life and various industrial process, for example, daily-use chemical industry, cosmetics, pesticide, automobile making, Intermetallic composite coating and cleaning, oil exploitation (surfactant flooding and ternary composite driving), petrochemical industry refining etc..Due to surfactant Stable oil-in-water emulsion be present in water body can block sunlight injection, reduce the light transmittance of water body, reduction organism in water and The photosynthesis of plant, therefore aquatic ecosystem can be caused greatly to damage and injure, and it is discharged into pipeline and sewage When processing equipment, easily causes to corrode and block.So the oil-in-water emulsion that oily waste water or surfactant are stablized is discharging Into before surface water body or sewage treatment plant, it is necessary to effectively remove oil emulsion.
Up to the present, various methods include electrochemical treatment, settling methods, Bubble-floating Method, membrane separation process and coagulation- Flocculence is all used for handling oily waste water.However, these methods are only effective to oil slick and dispersed oil.When oil is emulsified simultaneously well And oil droplet size be less than 10 μm when, these methods are invalid.When containing oil emulsion in waste water, absorption method, which is considered as one kind, to be had The method of effect, because its safety and technological design are simple, energy expenditure is low, acceptable discharge quality and at low cost.In order to Meet the needs of fast-developing water technology, the adsorbent in ideal must have some basic properties, such as big table Face region, environmental-friendly, high adsorption capacity, outstanding biological degradability, good cyclicity.Various adsorbents such as zeolite glues Native mineral, metal oxide and mixed-metal oxides are all used to processing emulsified oil-containing waste water.However, these adsorbents are still It there are problems that some such as low selectivity, poor extracting power, not satisfactory Oil-water separation efficiency and adsorbent again It is raw difficult.In this situation, promote us to design and develop new sorbent material and be used for handling emulsification oil content height, oil droplet grain Diameter is less than 10 μm, the processing of the oil-in-water emulsion of the big surfactant stabilization of water yield.
Invention content
Oil processing technology is emulsified in the oil-in-water emulsion that the present invention stablizes for existing oily waste water or surfactant Present in shortcoming and defect, provide a kind for the treatment of effeciency height, small investment, removal easy to operate, adsorbent regenerating easily The method of oil emulsion in the oil-in-water emulsion that surfactant is stablized.
The method of oil emulsion, includes the following steps in the oil-in-water emulsion that the removal surfactant of the present invention is stablized:
(1) magnetic adsorbent is prepared:
1. taking graphene oxide (GO), ferric trichloride and ferrous sulfate mixing salt solution and layered double hydroxide (Layered double hydroxide, LDH), by 0.15g graphene oxides and 200-220mL ferric trichlorides and ferrous sulfate The ratio of mixing salt solution, adds graphene oxide into mixing salt solution, is heated to 80-90 DEG C and is passed through N2Protection;
2. concentration 1.5mol/L NaOH solutions are added, pH to the 10-11 of regulation system stirs 30-40 at 80-90 DEG C Minute;Then, it is filtered, washed, is dried in vacuo 20-24 hours at 50-65 DEG C, obtain black MGO (Fe3O4- GO) hybrid;
3. a concentration of 5mg/L of fixed MGO hybrids, respectively according to MGO hybrids and layered double hydroxide matter Amount compares MGO:LDH is 5:1~1:5 ratio, the two is mixed, and is persistently stirred at 10-40 DEG C 1-2 hours, filtering Sediment, and be magnetic adsorbent after being cleaned and dried;
The ferric trichloride and Fe in ferrous sulfate mixing salt solution3+With Fe2+Mass ratio is 2:1.
The step (1) 2. in mixing speed be 100-130 revs/min.
3. middle drying precipitate temperature is 50-65 DEG C to the step (1).
(2) oil-in-water emulsion that Surfactant (for anion surfactant) is stablized carries out ionic strength adjusting, The ionic strength of the oil-in-water emulsion of surfactant stabilization is set to reach 0.001-0.1mol/L;
The conditioning agent for adjusting ionic strength is sodium chloride (NaCl) or sodium carbonate (Na2CO3)。
(3) adsorption process:
According to 0.1g/L-0.4g/L dosage to pH be 6-8, ionic strength be 0.001-0.1mol/L surface-active Magnetic adsorbent is added in the oil-in-water emulsion that agent is stablized, 10-40 DEG C is stirred 10-15 minutes, then in the effect of externally-applied magnetic field Lower Magneto separate.
100-130 revs/min of the mixing speed.
The Magneto separate time is 2-4 minutes.
The tan precipitate after Magneto separate in step (3) is separated and collected, remaining emulsification is carried out to the supernatant liquor after Magneto separate The measurement of oil concentration, remaining oil emulsion can use carbon tetrachloride (CCl in supernatant liquor4) extracted, the color of extract liquor It is in a linear relationship with the concentration of oil content, therefore can be measured by Infrared Oil Determination Instrument;Treated, and oily waste water reaches Reuse requirement, can be with reuse.Mass ratio, magnetic suck agent dosage, temperature and the ionic strength of MGO and LDH is all to influence surface The key factor that oil emulsion removes in the oil-in-water emulsion that activating agent is stablized.
The present invention uses absorption method.Absorption method handles the crucial skill of oil emulsion in the oil-in-water emulsion that surfactant is stablized Art is the selection of adsorbent, and an outstanding and ideal adsorbent must have big surface region, high adsorption capacity good Bio-compatibility and outstanding renewable ability.
The present invention prepares graphene oxide using natural graphite that is cheap and being easy to get as raw material, uses Fe3O4Particle is to oxygen Graphite alkene is modified, and MGO hybrids are obtained;Then LDH and MGO is carried out nano combined, obtain containing multi-functional group and Positively charged MGO/LDH nano-complexes, reaction condition is simple and easy to control, small investment, and treatment effeciency is high, be suitble to enterprise it is continuous, Extensive processing oily waste water, the oil emulsion isolated can be recycled, can be reused as a kind of regenerated resources;Magneto separate Adsorbent afterwards repeated multiple times can recycle.
Description of the drawings
Fig. 1 be prepare MGO/LDH nano-complexes each raw material observed under transmission electron microscope it is microcosmic Structure and pattern (15000 times of amplification factor).Wherein:(a) GO, (b) Fe3O4Particle, (c) MGO, (d) LDH, (e) MGO/LDH3 (MGO:LDH=1:And 4 (MGO of (f) MGO/LDH 1):LDH=1:3).
Fig. 2 is the song that the Zeta electric potential of 4 two kinds of nano-complexes of MGO/LDH 3 and MGO/LDH changes with pH value variation Line.
Fig. 3 is the schematic diagram that the removal efficiency of oil emulsion in embodiment 1 changes with the change of MGO and LDH mass ratioes.
Fig. 4 is the schematic diagram that the removal efficiency of oil emulsion in embodiment 2 changes with the change of temperature.
Fig. 5 is the schematic diagram that the removal efficiency of oil emulsion in embodiment 3 changes with the change of ionic strength.
Fig. 6 is the schematic diagram that the removal efficiency of oil emulsion in embodiment 4 changes with the change of sorbent circulation number.
Fig. 7 is that the oil-in-water emulsion that surfactant is stablized is added that magnetic adsorbent is front and back and effect in externally-applied magnetic field Issue the digital photograph of raw Oil-water separation.Wherein:(a) crude oil, the left side:Original crude oil-in-water lotions;It is intermediate: Original crude oil-in-water lotions+MGO/LDH 3;The right:Oil-hydromagnetic separation.(b) white oil, the left side:Original white Oil-in-water lotions;It is intermediate:Original white oil-in-water lotions+MGO/LDH 4;The right:Oil-hydromagnetic separation. (c) n-decane, the left side:Original decane-in-water lotions;It is intermediate:Original decane-in-water lotions+MGO/LDH4; The right:Oil-hydromagnetic separation.
Specific implementation mode
The oil-in-water emulsion that surfactant used in each embodiment is stablized is prepared by following procedure:
By 2g:The ratio of 1000mL takes oil and aqueous surfactant solution.Oil used in it selected three kinds it is different Product, i.e. crude oil, white oil and n-decane.Surfactant (detergent alkylate containing 40mg/L in aqueous surfactant solution Sodium sulfonate, SDBS).
2g crude oil (crude oil), white oil (white oil) and n-decane (decane) are added separately to containing surface In the aqueous solution of activating agent, is stirred 10-15 minutes on magnetic stirring apparatus, form uniform mixed system, then, by mixture System is placed on mulser, and under the rotating speed of 13000-18000, emulsification pretreatment 1-2 hours is allowed to form stable oil-in-water breast The average content of the oil-in-water emulsion that liquid, as surfactant are stablized, oil emulsion is 2000mg/L.
Magnetic adsorbent in each embodiment is pressed following procedure and is prepared:
Take graphite oxide (GO), ferric trichloride/ferrous sulfate mixing salt solution (Fe3+/Fe2+=2:1, w/w) and stratiform is double Metal hydroxides (Layered double hydroxide, LDH) colloidal sol is raw material, the mass percent concentration of LDH colloidal sols For 10-15%.In the ratio of 0.15g GO and 200-220mL ferric trichloride/ferrous sulfate mixing salt solution, GO is dispersed in three In iron chloride/ferrous sulfate mixing salt solution, the pH value of 1.5mol/L NaOH regulation systems is added to 10-11, at 80-95 DEG C It persistently stirs 30-40 minutes down;It is filtered, washed, is dried in vacuo 20-24 hours at 50-65 DEG C, obtain black Fe3O4-GO (MGO) hybrid;Then, a concentration of 5mg/L of fixed MGO, according to MGO:LDH mass ratioes are 5:1,3:1,1:1,1:3 and 1:5 Ratio, MGO is mixed with LDH colloidal sols, and is persistently stirred at 10-40 DEG C 1-2 hours, filtering, cleaning after, drying precipitate It is magnetic adsorbent, abbreviation MGO/LDH afterwards.
Five kinds of MGO:LDH mass ratioes (5:1,3:1,1:1,1:3 and 1:5) MGO/LDH 1, MGO/LDH 2, MGO/ obtained LDH3, MGO/LDH 4 and MGO/LDH 5 can be used as adsorbent;
Fig. 1 gives GO (a), Fe3O4Particle (b), MGO (c), LDH (d), MGO/LDH 3 (e) and MGO/LDH 4 (f) exist The microstructure and pattern of 15000 times of observations of amplification factor under transmission electron microscope.
The Zeta electric potential of MGO/LDH 3 and MGO/LDH 4 is given in Fig. 2 as a result, showing that two kinds of MGO/LDH are nano combined Object carries positive charge in the range of pH 5-10.
Embodiment 1
Crude oil-in-water, white oil-in-water and the decane-in- for taking surfactant to stablize Each 5 parts of water lotions, totally 15 parts, every part of 1000mL, the initial concentration 2000mg/L of oil emulsion, 20 DEG C of temperature, pH 6-8.
It is separately added into MGO/LDH in the oil-in-water emulsion stablized to 15 parts of surfactants by the dosage of 0.1-0.4g/L 1, MGO/LDH 2, MGO/LDH 3, MGO/LDH 4 and MGO/LDH 5 maintain 100-130 revs/min of mixing speed, stir 10- 15 minutes, then Magneto separate 2-4 minutes in the case where adding magnetic fields outside, collected supernatant liquor, carry out the survey of residual emulsification oil concentration It is fixed.
Result of implementation shows:For the crude oil-in-water lotions that surfactant is stablized, MGO/LDH 3 has Maximum oil removal efficiency, and for white oil-in-water and the decane-in-water breasts of surfactant stabilization Liquid, MGO/LDH 4 have maximum oily removal efficiency.Meanwhile as magnetic adsorbent from 0.1g/L increases to 0.4g/L, oil is gone Except efficiency obviously increases, crude oil-in-water emulsion systems, oily removal rate increases to 99.51% from 98.09%, Whiteoil-in-water emulsion systems, oily removal rate increases to 99.61% from 99.48%, and decane-in-water is newborn Liquid system, oily removal rate increase to 99.91% from 99.46%, as shown in Figure 3.
Embodiment 2
Crude oil-in-water, white oil-in-water and the decane-in- for taking surfactant to stablize Each 4 parts of water lotions, totally 12 parts, every part of 1000mL, initial concentration 2000mg/L, the pH 6-8 of oil emulsion.Three kinds different O/W lotions, each O/W lotion take 4 parts, are controlled respectively at 10 DEG C, 20 DEG C, 30 DEG C and 40 DEG C per a temperature.To crude 3 magnetic adsorbent of 0.3g/L MGO/LDH is added in oil-in-water lotions, to white oil-in-water and 4 magnetic adsorbents of 0.3g/L MGO/LDH are added in decane-in-water lotions, maintain 100-130 revs/min of stir speed (S.S.) Clock, time of contact controlled at 10-15 minutes, and then Magneto separate 2-4 minutes in the case where adding magnetic fields outside, collect supernatant liquor, into The measurement of the remaining emulsification oil concentration of row.
Result of implementation shows:The removal efficiency of oil emulsion declines with the raising of temperature, as shown in figure 4, determination MGO/ It is an exothermic process that LDH magnetic adsorbents remove oil emulsion from the O/W lotions that surfactant is stablized.This is because emulsification The solubility of oil in the liquid phase is increased with the raising of temperature, and oil emulsion removal difficulty is caused to increase.Therefore, temperature increases not Conducive to the generation of adsorption process.
Embodiment 3
Take crude oil-in-water, white oil-in-water that three kinds of different surfactants are stablized and Each 5 parts of decane-in-water lotions, totally 15 parts, every part of 1000mL, the initial concentration 2000mg/L of oil emulsion, using ion The ionic strength that intensity adjustment agent adjusts three kinds of oil-in-water emulsions is respectively 0.001,0.01,0.02,0.05 and 0.1mol/L, from Sub- intensity adjustment agent is NaCl and Na2CO3In one kind.
It is added MGO/LDH 3 into crude oil-in-water lotions by the dosage of 0.3g/L, and to white MGO/LDH 4 is added in oil-in-water and decane-in-water lotions, maintains 100-130 revs/min of mixing speed, Stirring 10-15 minutes, then Magneto separate 2-4 minutes in the case where adding magnetic fields outside, collect supernatant liquor, carry out residual oil emulsion It measures.
Result of implementation shows:The removal efficiency of oil emulsion increases with the increase of ionic strength, as shown in Figure 5.This is Because with electrolyte (inorganic salts, such as NaCl or Na2CO3) addition, the negative electrical charge on electrolyte meeting " shielding " emulsion droplets surface, The electrostatic repulsion between emulsion droplets is caused to reduce, small emulsion droplets are easy coalescence into big drop, and the stability of oil-in-water emulsion subtracts It is weak.In this case, under the action of magnetic adsorbent, oil emulsion is easy to remove from oil-in-water emulsion.
Embodiment 4
The initial concentration that oil emulsion is added at 10-40 DEG C, pH 7, adsorbent MGO/LDH 3 for temperature control is 2000mg/L Crude oil-in-water lotions in carry out adsorption experiment, mixing speed is controlled at 100-130 revs/min, stirs 10-15 Minute, then Magneto separate 2-3 minutes in the case where adding magnetic fields outside, collect supernatant liquor, carry out the measurement of remaining oil emulsion.Absorption MGO/LDH 3 after saturation is cleaned with 150mL petroleum ethers, and the MGO/LDH 3 after Magneto separate is added directly into oil emulsion Initial concentration is in the crude oil-in-water lotions of 2000mg/L, and the above operation is known as a cycle.It grasps repeatedly Make 5 times, MGO/LDH 3 is using after 5 times, and the removal rate of oil emulsion still reaches in crude oil-in-water lotions 95.14%.
At 10-40 DEG C, pH 7, the initial concentration that adsorbent MGO/LDH 4 is added to oil emulsion is for temperature control Adsorption experiment, mixing speed are carried out in the white oil-in-water lotions and decane-in-water lotions of 2000mg/L It 100-130 revs/min, stirs 10-15 minutes, then Magneto separate 2-3 minutes in the case where adding magnetic fields outside, collect supernatant liquor, Carry out the measurement of residual oil emulsion.MGO/LDH 4 after adsorption saturation is cleaned with 150mL ethyl alcohol, the MGO/ after Magneto separate LDH 4 is directly added into white oil-in-water lotions and decane-in-water lotions carry out adsorption experiment, above behaviour It is known as one cycle as process.After operating 5 cycles repeatedly, going for white oil is emulsified in white oil-in-water lotions Except rate is 96.26%, and the removal rate that decane oil is emulsified in decane-in-water lotions is still up to 97.88%.Fig. 6 gives The case where removal efficiency of oil emulsion changes with the change of sorbent circulation number is gone out.
MGO/LDH magnetic adsorbents have outstanding recycling ability, can be substantially reduced oiliness sewage treatment process Totle drilling cost.
The oil-in-water emulsion that Fig. 7 gives surfactant stabilization is added before and after magnetic adsorbent and in externally-applied magnetic field Effect issues the state of raw Oil-water separation.

Claims (7)

1. a kind of method of oil emulsion in oil-in-water emulsion that removal surfactant is stablized, characterized in that include the following steps:
(1) magnetic adsorbent is prepared:
1. graphene oxide, ferric trichloride and ferrous sulfate mixing salt solution and layered double hydroxide are taken, by 0.15g The ratio of graphene oxide and 200-220mL ferric trichlorides and ferrous sulfate mixing salt solution adds graphene oxide into mixed It closes in salting liquid, is heated to 80-90 DEG C and is passed through N2Protection;
2. concentration 1.5mol/L NaOH solutions are added, pH to the 10-11 of regulation system is stirred 30-40 minutes at 80-90 DEG C; Then, it is filtered, washed, is dried in vacuo 20-24 hours at 50-65 DEG C, obtain black MGO hybrids;
3. a concentration of 5mg/L of fixed MGO hybrids, according to MGO hybrids and layered double hydroxide mass ratio MGO: LDH is 5:1~1:5 ratio, the two is mixed, and is persistently stirred at 10-40 DEG C 1-2 hours, filtering precipitate, and It is magnetic adsorbent after cleaning-drying;
(2) oil-in-water emulsion that Surfactant is stablized carries out ionic strength adjusting, the oil-in-water for making surfactant stablize The ionic strength of lotion reaches 0.001-0.1mol/L;
(3) adsorption process:
According to 0.1g/L-0.4g/L dosage to pH be 6-8, ionic strength be 0.001-0.1mol/L surfactant it is steady It is added magnetic adsorbent in fixed oil-in-water emulsion, 10-40 DEG C is stirred 10-15 minutes, then magnetic under the action of externally-applied magnetic field Separation.
2. the method for oil emulsion, feature in the oil-in-water emulsion that removal surfactant according to claim 1 is stablized It is the ferric trichloride and Fe in ferrous sulfate mixing salt solution3+With Fe2+Mass ratio is 2:1.
3. the method for oil emulsion, feature in the oil-in-water emulsion that removal surfactant according to claim 1 is stablized Be, the step (1) 2. in mixing speed be 100-130 revs/min.
4. the method for oil emulsion, feature in the oil-in-water emulsion that removal surfactant according to claim 1 is stablized It is that 3. middle drying precipitate temperature is 50-65 DEG C to the step (1).
5. the method for oil emulsion, feature in the oil-in-water emulsion that removal surfactant according to claim 1 is stablized It is that the conditioning agent for adjusting ionic strength is sodium chloride or sodium carbonate.
6. the method for oil emulsion, feature in the oil-in-water emulsion that removal surfactant according to claim 1 is stablized It is 100-130 revs/min of mixing speed in the step (3).
7. the method for oil emulsion, feature in the oil-in-water emulsion that removal surfactant according to claim 1 is stablized It is that the Magneto separate time is 2-4 minutes in the step (3).
CN201810479415.XA 2018-05-18 2018-05-18 A method of oil emulsion in the oil-in-water emulsion that removal surfactant is stablized Pending CN108579679A (en)

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Application publication date: 20180928