CN102849907B - Separation method and device of polymer-containing oil sludge - Google Patents
Separation method and device of polymer-containing oil sludge Download PDFInfo
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- CN102849907B CN102849907B CN201210335234.2A CN201210335234A CN102849907B CN 102849907 B CN102849907 B CN 102849907B CN 201210335234 A CN201210335234 A CN 201210335234A CN 102849907 B CN102849907 B CN 102849907B
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- 238000000926 separation method Methods 0.000 title claims abstract description 32
- 239000010802 sludge Substances 0.000 title abstract description 15
- 229920000642 polymer Polymers 0.000 title abstract description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 23
- 239000007790 solid phase Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 34
- 239000002994 raw material Substances 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 33
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 29
- -1 polyoxyethylene Polymers 0.000 claims description 29
- 239000003292 glue Substances 0.000 claims description 22
- 238000004062 sedimentation Methods 0.000 claims description 22
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 239000010779 crude oil Substances 0.000 claims description 14
- 238000002604 ultrasonography Methods 0.000 claims description 12
- 125000000217 alkyl group Chemical group 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 11
- 239000003995 emulsifying agent Substances 0.000 claims description 9
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 5
- 239000012028 Fenton's reagent Substances 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims description 5
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000004159 Potassium persulphate Substances 0.000 claims description 3
- 235000019394 potassium persulphate Nutrition 0.000 claims description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract 1
- 238000012994 industrial processing Methods 0.000 abstract 1
- 238000012667 polymer degradation Methods 0.000 abstract 1
- 230000005855 radiation Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 33
- 239000003921 oil Substances 0.000 description 26
- 230000000694 effects Effects 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 239000012071 phase Substances 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000002525 ultrasonication Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910003480 inorganic solid Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- OKIIEJOIXGHUKX-UHFFFAOYSA-L Cadmium iodide Inorganic materials [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 229940075417 cadmium iodide Drugs 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 230000002925 chemical effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000011278 co-treatment Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010734 process oil Substances 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002569 water oil cream Substances 0.000 description 1
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Abstract
The invention discloses a separation method and a separation device of polymer-containing oil sludge. The separation method comprises the steps of: (1) ultrasonic gel breaking of the polymer-containing oil sludge; (2) ultrasonic cleaning; and (3) standing separation. An ultrasonic device comprises a cylinder, an ultrasonic generation device, an ultrasonic controller arranged in the ultrasonic generation device, and ultrasonic transducers matching the ultrasonic generation device. The ultrasonic transducers are arrayed and are uniformly distributed on the two ends of the cylinder. A feeding port and a discharging port are respectively arranged on the top and the bottom of the cylinder. A feeding direction is perpendicular to an ultrasonic emission direction. According to the invention, polymer degradation is enhanced by using ultrasonic, stabilization of the polymer upon the oil-water-solid phase is reduced, and separation efficiency is improved. The feeding direction is perpendicular to the ultrasonic emission direction, and the ultrasonic device runs on line. Ultrasonic field radiation energy is concentrated, and an irradiation time is short, such that polymer-containing oil sludge can be subjected to large-scale industrial processing.
Description
Technical field
The present invention relates to, containing poly-greasy filth purifying treatment method, specifically refer to a kind of separation method and equipment containing poly-greasy filth.
Background technology
Along with the use of polymer flooding is in recent years more and more extensive, in the Produced Liquid process of oil, produced the very stable greasy filth of a class character,, containing poly-greasy filth, it belongs to tank bottom oil sludge.Containing poly-greasy filth, under polymer flooding oil condition, produce, it is that the component interactions such as polyacrylamide (HPAM) residual in the water conditioner that adds in paraffin in oil, Produced Liquid treating processes, Produced Liquid and bituminous matter form highly stable netted property structure, oil droplet in Produced Liquid, earth, heavy metal salt, mechanical impurity, the grains of sand etc. are wrapped, form the thickness milk sap of stable in properties.Due to difference in specific gravity, containing poly-greasy filth natural subsidence, be accumulated in tank bottom, and the interfacial film that naturally occurring emulsifying agent forms makes the character containing poly-greasy filth of water-oil emulsion highly stable.
Due to very complicated containing the composition of poly-greasy filth, in the face of its treatment process also has many kinds both at home and abroad, wherein mainly comprise pyroprocessing technology, solvent extraction technology, biologic treating technique, freezing disposal technology, ultrasonication technology, chemical cleaning technique etc.
Chemical cleaning method refers to chemical joined in pending greasy filth, fully stirs afterwards, joins in separating centrifuge centrifugally, reaches the effect that oil, water, mud three-phase separate.At present, be mainly that ground sludge is being used this method.The chemical cleaning method that EPA takes is mainly, by alkali lye, greasy filth is carried out to repetitive scrubbing, then makes greasy filth carry out separation with air-floating apparatus.Conventionally, washing time 20min, wash conditions is generally at temperature 70 C, and liquid-solid ratio is about 3:1, can be that to be washed till residual oil content be below 1% to 30% greasy filth by oleaginousness.Alkali lye can be comprised of cheap mineral alkali and inorganic salt, also can select cheap tensio-active agent, as washing powder etc.The outstanding feature of the method is that energy expenditure is lower.This method is comparatively ripe in states such as the U.S., and application is at present comparatively extensive, can reach the level of large-scale industrial continuous production.
Yet, oily sludge forms extremely complicated, the a large amount of chemical agents that add in Oil extraction process make oily sludge in the bridge crosslinking structure of sump oil and inoganic solids firm, mineralization degree is high, oil, emulsifying water fully cannot be removed the sump oil in oily sludge effectively with existing chemical cleaning method.
Ultrasonication meeting produce high frequency mechanical vibration effect, cavatition, heat effect, with the multiple effect such as chemical effect, can make profit breakdown of emulsion efficient rapidly, oil particles make with the mutual desorb of inorganic solid particles sump oil particle mutually assemble floating separated with inorganic solid particles.At present, utilize ultrasonication mainly to process containing sand greasy filth or common ground sludge or tank bottom oil sludge, but treatment capacity is limited, treatment time length, complex treatment process, effect are poor.
For example, Chinese patent 200320126412.7 reports are oil sludge and sand treatment unit, and its ultrasonic transducer, in a reactor, mainly plays cleanup action, and ultrasonic field distributes also uneven.Chinese patent 200610046818.2 has been reported treatment process and the equipment of oil-containing mud sand, its ultrasonic transducer is evenly distributed on reactor inwall, but what transverter was not described specifically arranges distance, apart from too far away, be that reactor diameter is greater than 1m, the ultrasonic region intermediate that acts on is kept to zero substantially, and irradiation time is very long, and treatment capacity is limited.The ultrasonic Oil Containing Sludge Treatment of Chinese patent 200710021086.6 reports, its ultrasound wave irradiation direction is from bottom up, similar ultrasonic emulsification or washing unit, the ultrasound wave irradiation time is longer.Chinese patent 201010147313.1 report adopts low frequency ultrasounds and high frequency ultrasound to process oil-containing mud sand, ultrasound wave irradiation time 20-60min, but do not provide the direction of ultrasound wave irradiation, its ultrasonic effect is unable to estimate.
And, from current patent documentation and periodical literature, have no and adopt ultrasonic online equipment collaboration chemicals treatment containing poly-greasy filth, to reclaim the report of crude oil.
Summary of the invention
Object of the present invention is for the not enough of supersound process oily sludge in prior art and without supersound process, contain the method for gathering greasy filth, and a kind of separation method containing poly-greasy filth is provided.
Another object of the present invention is to provide the equipment of realizing this separation method.
For achieving the above object, the present invention, containing the separation method of poly-greasy filth, comprises the following steps:
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 60～90 ℃ of mixing, water is 1:1～5:1 with the mass ratio containing poly-greasy filth, then in mixture, add gel breaker, gel breaker dosage is for containing 0.1%～2% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.2min～5min; Described gel breaker is selected from a kind of in Fenton reagent, Fenton-like reagent, hydrogen peroxide, Potassium Persulphate, Sodium Persulfate, potassium ferrate, Na2Fe04, clorox, Losantin, potassium permanganate;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding clean-out system and non-emulsifying agent in poly-greasy filth mixture, wherein, clean-out system dosage is for containing 0.01%～0.03% of poly-greasy filth raw materials quality, non-emulsifying agent dosage is for containing 0.005%～0.03% of poly-greasy filth raw materials quality, after mixing, at 60～90 ℃, carry out supersound process 0.2～3min;
3) standing separation: at 60～90 ℃ of standing sedimentation 10～60min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 2 of the present invention) in, described clean-out system is alkylphenol polyoxyethylene, and wherein, alkyl chain is C
8～C
12alkyl, ethoxymer distribution is 5～10, described non-emulsifying agent is selected from SP169, PFA-8311, BP-2040, AE-1910 or TA1031.
Described step 1) and 2), in, supersound process is carried out in same ultrasonic device.
The form that in the present invention, gel breaker, clean-out system and emulsion resistance add is solution, and its add-on all refers to active substance in solution and accounts for the per-cent containing poly-greasy filth raw materials quality.
The reagent of Fenton described in the present invention is hydrogen peroxide and catalyst Fe
2+the solution forming.
The reagent of Fenton-like described in the present invention is hydrogen peroxide and catalyst Fe
3+the solution forming.
The equipment of realizing above-mentioned separation method that the present invention is designed, the ultrasonic transducer that comprises cylindrical shell, ultra-sonic generator, is arranged on the ultrasonic controller in ultra-sonic generator and matches with ultra-sonic generator, described ultrasonic transducer is array, be evenly distributed on the two ends of cylindrical shell, the top of described cylindrical shell and bottom are respectively arranged with opening for feed and discharge port, and feedstock direction is vertical with ultrasound emission direction.
In such scheme, described ultrasonic transducer is 10～60KHz to the ultrasonic frequency of launching in cylindrical shell, and sound field intensity is 1000～12000W/m
2.
In such scheme, in described ultrasonic controller, be provided with frequency sweep control module, time control module, power control module and temperature control modules.
In such scheme, the length d of described cylindrical shell is 20cm～80cm.
Beneficial effect of the present invention: the present invention adopts ultrasonication and medicament co-treatment containing poly-greasy filth, has following advantage:
1, utilize the degraded of ultrasound-enhanced polymkeric substance, Gu greatly reduce the stabilization of polymkeric substance to oil-water-three-phase, be convenient to the separation of three-phase;
2, ultrasonic cavitation can destroy the colloid-stabilised structure of oily sludge, reduce the adhesive attraction of sump oil and inoganic solids, utilize the naturally occurring emulsifying agents such as the bituminous matter of the solid absorption in ultrasound-enhanced medicament cleaning mud oil and colloid, destroy the emulsifying effect of mud phase, reduce the oil length of mud phase, rapidly and efficiently separate sump oil and inorganic solid particles, separation efficiency is improved greatly;
3, feedstock direction is vertical with ultrasound emission direction, Vltrasonic device on-line operation, and ultrasonic field irradiation energy is concentrated, and irradiation time is short, is convenient to large-scale industrialization and processes containing poly-greasy filth;
4, more than the rate of recovery of greasy filth Crude Oil reaches 98%wt, isolated solid phase oil length is low, and water COD value can drop in 700.
Accompanying drawing explanation
Fig. 1 is the left TV structure schematic diagram of ultrasonic device of the present invention.
Fig. 2 is the main TV structure schematic diagram of ultrasonic device of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
As shown in Figure 1, 2, separation method of the present invention ultrasonic device used, the ultrasonic transducer 1 that comprises cylindrical shell 4, ultra-sonic generator 5, is arranged on the ultrasonic controller 6 in ultra-sonic generator 5 and matches with ultra-sonic generator 5.Ultrasonic transducer 1 is array, is evenly distributed on the two ends of cylindrical shell 4, and the top of cylindrical shell 4 and bottom are respectively arranged with opening for feed 2 and discharge port 3, and feedstock direction is vertical with ultrasound emission direction.In ultrasonic controller 6, be provided with frequency sweep control module 6.1, time control module 6.2, power control module 6.3 and temperature control modules 6.4.
Non-emulsifying agent SP169, PFA-8311 in following examples, BP-2040, AE-1910, TA1031 all buy in Shandong limited liability company of Bin Hua group.
Following examples are used takes from SZ 36-1 Field containing poly-greasy filth, and its character is as shown in table 1:
Table 1 is containing the character of poly-greasy filth
The dry mud volatile content of@heats and records for 3 hours at 750 ℃
* adopt the concentration of starch-cadmium iodide colorimetric method for determining HPAM
Embodiment 1
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 90 ℃ of mixing, water is 1:1 with the mass ratio containing poly-greasy filth, then in mixture, add potassium persulfate solution, in potassium persulfate solution, Potassium Persulphate is for containing 0.1% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.2min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and SP169 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.01% of poly-greasy filth raw materials quality, SP169 is for containing 0.03% of poly-greasy filth raw materials quality, after mixing, at 90 ℃, carry out supersound process 0.2min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
8alkyl, ethoxymer distribution is 5;
3) standing separation: at 90 ℃ of standing sedimentation 10min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 20cm of this ultrasonic device, and ultrasonic transducer 1 is 10KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 1000W/m
2.
Embodiment 2
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 80 ℃ of mixing, water is 2:1 with the mass ratio containing gathering greasy filth, then adds hydrogen peroxide in mixture, H in hydrogen peroxide
2o
2for containing 2% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.2min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and PFA-8311 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene solution is for containing 0.03% of poly-greasy filth raw materials quality, PFA-8311 is for containing 0.005% of poly-greasy filth raw materials quality, after mixing, at 80 ℃, carry out supersound process 3min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
12alkyl, ethoxymer distribution is 10;
3) standing separation: at 60 ℃ of standing sedimentation 60min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 80cm of this ultrasonic device, and ultrasonic transducer 1 is 10KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 2000W/m
2.
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 60 ℃ of mixing, water is 5:1 with the mass ratio containing poly-greasy filth, then in mixture, add Sodium Persulfate solution, in Sodium Persulfate solution, Sodium Persulfate is for containing 0.4% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 5min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and BP-2040 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.02% of poly-greasy filth raw materials quality, BP-2040 amount is for containing 0.02% of poly-greasy filth raw materials quality, after mixing, at 60 ℃, carry out supersound process 0.5min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
9alkyl, ethoxymer distribution is 6;
3) standing separation: at 60 ℃ of standing sedimentation 40min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 80cm of this ultrasonic device, and ultrasonic transducer 1 is 60KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 6000W/m
2.
Embodiment 4
1) containing the ultrasonic broken glue of poly-greasy filth: by water and containing poly-greasy filth 70 ℃ of mixing, water is 3:1 with the mass ratio containing poly-greasy filth, then in mixture, adds Fenton reagent, Fenton reagent consist of the aqueous solution being formed by ferrous sulfate and 30%wt hydrogen peroxide, H
2o
2/ Fe=5mol, pH=4.0, H in Fenton reagent
2o
2for containing 1% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 1min; ;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and AE-1910 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.01% of poly-greasy filth raw materials quality, AE-1910 is for containing 0.01% of poly-greasy filth raw materials quality, after mixing, at 70 ℃, carry out supersound process 0.5min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
9alkyl, ethoxymer distribution is 6;
3) standing separation: at 70 ℃ of standing sedimentation 30min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 70cm of this ultrasonic device, and ultrasonic transducer 1 is 28KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 5000W/m
2.
Embodiment 5
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 65 ℃ of mixing, water is 4:1 with the mass ratio containing poly-greasy filth, then in mixture, add potassium ferrate solution, in potassium ferrate solution, potassium ferrate is for containing 0.1% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.8min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and TA1031 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.02% of poly-greasy filth raw materials quality, TA1031 is for containing 0.005% of poly-greasy filth raw materials quality, after mixing, at 65 ℃, carry out supersound process 1min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
8alkyl, ethoxymer distribution is 6;
3) standing separation: at 75 ℃ of standing sedimentation 20min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 60cm of this ultrasonic device, and ultrasonic transducer 1 is 40KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 6000W/m
2.
Embodiment 6
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 65 ℃ of mixing, water is 3:1 with the mass ratio containing poly-greasy filth, then in mixture, add Na2Fe04 solution, in Na2Fe04 solution, Na2Fe04 is for containing 0.5% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.8min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and PFA-8311 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.03% of poly-greasy filth raw materials quality, PFA-8311 is for containing 0.01% of poly-greasy filth raw materials quality, after mixing, at 65 ℃, carry out supersound process 0.5min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
12alkyl, ethoxymer distribution is 6;
3) standing separation: at 75 ℃ of standing sedimentation 20min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 80cm of this ultrasonic device, and ultrasonic transducer 1 is 50KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 6000W/m
2.
Embodiment 7
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 85 ℃ of mixing, water is 4:1 with the mass ratio containing poly-greasy filth, then in mixture, add chlorine bleach liquor, in chlorine bleach liquor, clorox is for containing 1% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.8min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and PFA-8311 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.02% of poly-greasy filth raw materials quality, PFA-8311 is for containing 0.03% of poly-greasy filth raw materials quality, after mixing, at 65 ℃, carry out supersound process 2min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
9alkyl, ethoxymer distribution is 6;
3) standing separation: at 75 ℃ of standing sedimentation 60min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 50cm of this ultrasonic device, and ultrasonic transducer 1 is 20KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 12000W/m
2.
Embodiment 8
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 85 ℃ of mixing, water is 3:1 with the mass ratio containing poly-greasy filth, then in mixture, adds calcium hypochlorite solution, and in calcium hypochlorite solution, Losantin is for containing 1% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 5min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene solution and SP169 solution in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.03% of poly-greasy filth raw materials quality, SP169 is for containing 0.03% of poly-greasy filth raw materials quality, after mixing, at 65 ℃, carry out supersound process 3min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
9alkyl, ethoxymer distribution is 6;
3) standing separation: at 75 ℃ of standing sedimentation 20min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 40cm of this ultrasonic device, and ultrasonic transducer 1 is 20KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 10000W/m
2.
Embodiment 9
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 65 ℃ of mixing, water is 4:1 with the mass ratio containing poly-greasy filth, then in mixture, add potassium permanganate solution, in potassium permanganate solution, potassium permanganate is for containing 0.4% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.8min;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding alkylphenol polyoxyethylene and PFA-8311 in poly-greasy filth mixture, alkylphenol polyoxyethylene is for containing 0.02% of poly-greasy filth raw materials quality, PFA-8311 is for containing 0.03% of poly-greasy filth raw materials quality, after mixing, at 65 ℃, carry out supersound process 0.2min; Wherein, the alkyl chain that adds alkylphenol polyoxyethylene is C
9alkyl, ethoxymer distribution is 6;
3) standing separation: at 75 ℃ of standing sedimentation 30min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
Step 1) and 2), in, supersound process is carried out in same ultrasonic device, the cylindrical shell 4 length 60cm of this ultrasonic device, and ultrasonic transducer 1 is 20KHz to the ultrasonic frequency of cylindrical shell 4 interior transmittings, sound field intensity is 7000W/m
2.
Embodiment 1～9 is as shown in table 2 containing the treatment effect of poly-greasy filth.After reclaiming in table 2, oil phase water ratio adopts GB GB 260-77, water by distillation; Reclaiming oil phase mud containing rate=1-adopts toluene extraction process to measure oil length-water ratio; The measurement of COD value adopts chromium Fa-Re to clear up.
Table 2 is containing the treatment effect of poly-greasy filth
More than the rate of recovery of greasy filth Crude Oil of the present invention can reach 98%wt as can be seen from Table 2, isolated solid phase oil length is low, and water COD value can drop in 700.Separating effect is very good.
Claims (5)
1. containing a separation method for poly-greasy filth, comprise the following steps:
1) containing the ultrasonic broken glue that gathers greasy filth: by water with containing gathering greasy filth 60～90 ℃ of mixing, water is 1:1～5:1 with the mass ratio containing poly-greasy filth, then in mixture, add gel breaker, gel breaker dosage is for containing 0.1%～2% of poly-greasy filth raw materials quality, after mixing, carry out supersound process 0.2min～5min; Described gel breaker is selected from a kind of in Fenton reagent, Fenton-like reagent, hydrogen peroxide, Potassium Persulphate, Sodium Persulfate, potassium ferrate, Na2Fe04, clorox, Losantin, potassium permanganate;
2) ultrasonic cleaning: to after above-mentioned ultrasonic broken glue containing adding clean-out system and non-emulsifying agent in poly-greasy filth mixture, wherein, described clean-out system is alkylphenol polyoxyethylene, wherein, alkyl chain is C
8～C
12alkyl, ethoxymer distribution is 5～10; Described non-emulsifying agent is selected from SP169, PFA-8311, BP-2040, AE-1910 or TA1031, clean-out system dosage is for containing 0.01%～0.03% of poly-greasy filth raw materials quality, non-emulsifying agent dosage is for containing 0.005%～0.03% of poly-greasy filth raw materials quality, after mixing, at 60～90 ℃, carry out supersound process 0.2～3min;
3) standing separation: at 60～90 ℃ of standing sedimentation 10～60min, upper strata is isolated crude oil by the above-mentioned mixture through ultrasonic cleaning, the solid phase that lower floor is sedimentation, centre is water.
2. according to claim 1 containing the separation method of poly-greasy filth, it is characterized in that: described step 1) and 2), supersound process is carried out in same ultrasonic device.
3. an equipment of realizing separation method described in claim 1, comprise ultrasonic device, it is characterized in that: described ultrasonic device comprises cylindrical shell (4), ultra-sonic generator (5), be arranged on the ultrasonic controller (6) in ultra-sonic generator (5) and the ultrasonic transducer (1) matching with ultra-sonic generator (5), described ultrasonic transducer (1) is array, be evenly distributed on the two ends of cylindrical shell (4), the top of described cylindrical shell (4) and bottom are respectively arranged with opening for feed (2) and discharge port (3), feedstock direction is vertical with ultrasound emission direction, the length d of described cylindrical shell (4) is 20cm～80cm.
4. the equipment of separation method according to claim 3, is characterized in that: described ultrasonic transducer (1) is 10～60KHz to the ultrasonic frequency of transmitting in cylindrical shell (4), and sound field intensity is 1000～12000W/m
2.
5. the equipment of separation method according to claim 3, is characterized in that: in described ultrasonic controller (6), be provided with frequency sweep control module (6.1), time control module (6.2), power control module (6.3) and temperature control modules (6.4).
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| CN109231355A (en) * | 2018-10-26 | 2019-01-18 | 知合环境（北京）有限责任公司 | A kind of polymer-containing oil sludge purifying treatment method and cleaning agent used |
| CN111253964B (en) * | 2020-02-12 | 2021-11-05 | 北京矿冶科技集团有限公司 | Method for treating polymer-containing oil sludge |
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| CN111849651A (en) * | 2020-07-15 | 2020-10-30 | 中国海洋大学 | Thermochemical cleaning agent containing polymer oil sludge in oil field and preparation method and application thereof |
| CN111841408A (en) * | 2020-07-20 | 2020-10-30 | 中国海洋石油集团有限公司 | Pulping method containing polymer-containing oil sludge |
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