CN101898860A - Inorganic profile control agent with oil sludge and application method thereof - Google Patents
Inorganic profile control agent with oil sludge and application method thereof Download PDFInfo
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Abstract
The invention relates to an inorganic profile control agent with oil sludge and an application method thereof. The inorganic profile control agent with oil sludge is prepared by mixing the following components in parts by weight: 10-15 parts of oil sludge, 5-25 parts of cement, 0-5 parts of flyash, 0-10 parts of retarder, 0-10 parts of firming agent and 0-0.2 part of surfactant, wherein the surfactant is sodium dodecyl benzene sulfonate. The invention has the advantages as follows: 1) a certain amount of water is added in the formula, so that the obtained working solution has small viscosity, thereby facilitating stirring and pouring; 2) the working solution is uniform and stable, has good suspension property and can meet the stability requirement of the work solution for on-site construction; and 3) the injected inorganic profile control agent with oil sludge has moderate curing strength in a bottom layer environment, and can perform water shutoff and profile control.
Description
Technical field
The present invention relates to a kind of inorganic profile control agent with oil sludge and application method thereof, be mainly used in high permeability macropore profile control face.
Background technology
Oily sludge is meant by idle oil-containing solids and gunk.Oil field mining liquid can form one deck black thick liquid gradually at the bottom of jar after art breading such as oil removing, sedimentation, i.e. oily sludge, and its main component is water, silt particle, gum asphalt and wax.Along with the China's oil exploitation progressively enters ultra-high water cut stage, be accompanied by the use that number of chemical auxiliary agent combination flooding replaces, the output of oily sludge can constantly increase.Oily sludge has characteristics such as generation is big, oleaginousness is high, mink cell focus component height, wherein also contains cacodorous toxic substances such as benzene series thing, phenols, anthracene, pyrene except that containing a large amount of residual alkane oils; Also contain radioelement in some stratum also along with the extraction of extraction liquid, and be deposited in the mud; Also contain heavy metals such as a large amount of pathogenic bacterias, parasite, copper, zinc, chromium, mercury in the oily sludge.A large amount of oily sludges is bulky, if effectively do not handle, not only takies a large amount of arable lands, and all will pollute surrounding soil, water body, air, and have rubble flow hidden danger.At present, oily sandy sludge is classified as Hazardous wastes by country.The processing of oily sludge also is a great problem of puzzlement petroleum and petrochemical industry always.
One method of handling oily sludge at present both at home and abroad has: burning method, biological treatment, hot washing method, solvent extration, chemical demulsification method, solid-liquid isolation method etc.The specific aim that great majority are handled the oily sludge technology is not strong, cost is higher.Recently a lot of oil fields is solidified oil field sludge or is made building brick on ground, but increasing data shows that there is radiating danger in the building brick made from oily sludge, thereby can not get promoting.Researching and proposing about oily sludge Central Plains oil recovery of a lot of scholars also arranged, utilize physics and chemical process that crude oil in the oily sludge and other organic matters are extracted as far as possible, but imperfection is gone back in the research about remaining solid purifying treatment aspect at present, the method of most of oilfield treatments oily sludge is all only for reclaiming the crude oil in the oily sludge, and remaining solid is deposited in the well site or the landfill of digging pit.But these ways obviously do not have fundamentally to solve the pollution problem of oil field sludge, and processing cost is higher.Therefore present domestic most oily sludges are deposited in You Qu ground, do not have utility value substantially.
On the other hand, water injection well needs a large amount of amendments that use in the oilfield water extraction process, present amendment kind is a lot, exist a lot of problems also a lot, adaptability is bad, on the high side, a large amount of chemical assistants forms secondary pollution along with amendment enters the stratum, and might bring problems such as expendable injury to ground environment and structure.So it is wide, cheap to search out adaptation, be amendment research of present oil field and application direction to the eco-friendly good amendment in stratum.
Summary of the invention
The problem that the present invention is directed to above-mentioned prior art existence proposes a kind of inorganic profile control agent with oil sludge, it can utilize a large amount of discarded oily sludge that produces in the Oil extraction, the profile control working fluid of gained has good suspension property, viscosity is little, potential of hydrogen is moderate, anti-salt and high infiltration with characteristics such as formation rock cement, can be satisfied middle-temperature section high permeability profile control face profile control; Experimental result shows, has certain intensity after fixed can adapt to waterflood flush, can effectively oily sludge be backfilling into disused well, also can be backfilling into the displacement of reservoir oil environment that the high infiltration of macropore water injection well provides for secondary, three water flood recoveries.
The present invention is adopted solution to be by the problem of the above-mentioned proposition of solution: inorganic profile control agent with oil sludge, it is characterized in that including oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent forms through mixed preparing, described tensio-active agent is a Sodium dodecylbenzene sulfonate, each raw materials by weight portion is counted: oily sludge 10-15, cement 5-25, flyash 0-5, solidifying agent 0-10, retardant 0-10, tensio-active agent 0-0.2.
Press such scheme, described retardant is that gac is or/and the phosphorus ore slag.
Press such scheme, described solidifying agent is that sodium sulfate is or/and ammonium chloride.
The application method of inorganic profile control agent with oil sludge, it is characterized in that taking by weighing oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent, described tensio-active agent is a Sodium dodecylbenzene sulfonate, each raw materials by weight portion is counted: oily sludge 10-15, cement 5-25, flyash 0-5, solidifying agent 0-10, retardant 0-10, tensio-active agent 0-0.1, add water and stir the colloidal working fluid that mixes that is made into solid content 30%-45%, behind natural subsidence 0.5-1h, obtain the working fluid of amendment, guarantee that the supernatant liquor ratio is no more than 20%, must be able to not flow behind the working fluid 5h of the amendment of gained, by profile control equipment amendment is filled into the stratum at last, be completion of cure behind the experience 72-150h.
Press such scheme, described whipping step is meant under the 500-800r/min condition and stirs 10-20min.
The present invention has introduced this intractability great achievement of oily sludge and has divided extremely complicated raw material in conjunction with the industry standard of construction condition and existing mineral-type amendment.Given full play to the chemical property of other compositions in oily sludge and the prescription, the amendment of final gained is compared with existing amendment and is mainly contained following advantage:
The first, the working fluid viscosity that prescription adds a certain amount of water stirring gained is little, is convenient to stir and perfusion; Owing to contain a large amount of colloids in the organic matter in the oily sludge, viscosity is big, add oily sludge separately, viscosity became bigger after solid content was added to 40% in the prescription, it is big that the interpolation of cement can reduce viscosity, certainly the solid content conference increases the viscosity of working fluid, thus after the amendment among the present invention prepares amount of water one be not less than 55%, the working fluid stable homogeneous;
The second, the working fluid stable homogeneous, suspension property is good, satisfies site operation to the working fluid stability requirement; Porosity is big, absorptivity is strong, chemical property is stable because flyash in the prescription and gac have, and excellent surface property can be provided, increase-volume, and improve sticking power.The adding of tensio-active agent also can change the surface property of organism and inorganics in the working fluid, improves suspension.
The 3rd, it is moderate to inject back solidification intensity under BOTTOM LAYER ENVIRONMENT, can water plugging and profile controlling, solidified dominant mechanism is that hydrated cementitious is fixed, organic class material is bigger to the cement solidification intensity effect, the flyash here and the macropore of gac can adsorb the organic matter in the oily sludge, thereby reduce organic influence to hydrated cementitious, improve solidification intensity.The phosphorus ore slag, sodium sulfate, ammonium chloride can be accelerated hydrated cementitious, and in the later stage, injects bottom and accelerate the suspension system solid particles sediment later on, reduces being suspended in bubble in the working fluid, also can play enhancement to solidification intensity.
Description of drawings
Fig. 1 is the infared spectrum of used oily sludge wash-out oil (methylene dichloride eluent) among the embodiment 3
Fig. 2 is the EDS collection of illustrative plates of sand sample after the embodiment 3 used oily sludge de-oilings
Embodiment
The invention will be further described below in conjunction with embodiment, but can not be as limitation of the invention.
The reagent chemicals specification and the place of production involved among the present invention are as follows: cement is magnificent new brand of A# normal silicate, Huangshi, Hubei Province, the place of production; Flyash is that granularity is 300 order thermal power plant flyash, Wuhan City, place of production green hill flyash company; Retardant phosphorus ore slag, Yichang City, Hubei Province, the place of production; The retardant gac, Wuhan City, Hubei Province, the place of production; Solidifying agent sodium sulfate and ammonium chloride are chemical pure chemistry reagent, and tensio-active agent is a Sodium dodecylbenzene sulfonate, is chemically pure reagent.
Oily sludge source used among the present invention is the triumph Gudao oilfield, and oily sludge is apparent to be dark-brown, and black colloidal bitumen shape fritter is arranged.Sample sampling analysis composition, oily sludge main component are shale, a small amount of crude oil and colloid, wash away organic matter after, sandy granularity is less.Sandy and the organic effective constituent that all can be used as amendment among the present invention in the oily sludge.
Embodiment 1:
Get 15 parts of oily sludges, 5 parts of cement, 5 parts of flyash, 5 parts of phosphorus ore slags (retardant), 0.2 part of Sodium dodecylbenzene sulfonate, 3 parts of sodium sulfate, 3 parts of ammonium chlorides, 64 parts of high salinity well water.Place beaker, under 500r/min, stir 10min, make it become the colloidal working fluid that mixes.Unload whipping appts, will stir resulting working fluid and pour in the glass test tube of 300mm * 22mm (internal diameter), Glass tubing leaves standstill natural subsidence 1h measures the supernatant liquor height.Tipping supernatant liquor behind the 5h after observing solid and not flowing mutually, places 60 ℃ of water-baths with Glass tubing, after three days Glass tubing is taken out, and the Glass tubing unstopper places 60 ℃ in baking oven baking 20h down, has dried by the fire with the rear surface to no longer include water, and solid is rendered as Dark grey or dark-brown.Break Glass tubing after the cooling gently into pieces, take out column form object.Measure its ultimate compression strength.
Experimental result: the working fluid pH8.0 of configuration gained, supernatant liquor accounts for cumulative volume 4.7% behind the 1h.No longer mobile behind the static 5h of working fluid in the Glass tubing.Column form object ultimate compression strength is 0.3MPa after 3 days.
Embodiment 2:
Get 10 parts of oily sludges, 25 parts of cement, 5 parts of phosphorus ore slags (retardant), 5 parts of gacs (retardant), 55 parts of high salinity well water.Place beaker, under 500r/min, stir 10min, make it mix homogeneous.Unload whipping appts, will stir resulting working fluid and pour in the Glass tubing of 300mm * 22mm (internal diameter), Glass tubing leaves standstill natural subsidence 1h measures the supernatant liquor height.Tipping supernatant liquor behind the 5h after observing solid and not flowing mutually, places 60 ℃ of water-baths with Glass tubing, after three days Glass tubing is taken out, and the Glass tubing unstopper places 60 ℃ of bakings of baking oven 20h, has dried by the fire with the rear surface to no longer include water, and solid is rendered as Dark grey or dark-brown.Break Glass tubing after the cooling gently into pieces, take out column form object.Measure its ultimate compression strength.
Experimental result: configuration gained working fluid pH7.5.The 1h supernatant liquor accounts for cumulative volume 8.7%.No longer mobile behind the static 5h of working fluid in the Glass tubing.Column form object ultimate compression strength is 0.4MPa after 3 days.
Embodiment 3:
Get 10 parts of oily sludges, 15 parts of cement, 5 parts of sodium sulfate (solidifying agent), 70 parts of well water.Place beaker, under 500r/min, stir 15min, make it mix homogeneous.Unload whipping appts, will stir resulting working fluid and pour in the glass test tube of 300mm * 22mm (internal diameter), Glass tubing leaves standstill natural subsidence 1h measures the supernatant liquor height.Tipping supernatant liquor behind the 5h after observing solid and not flowing mutually, places 60 ℃ of water-baths experiments with test tube, after three days Glass tubing is taken out, and the Glass tubing unstopper places 60 ℃ of bakings of baking oven 20h, has dried by the fire with the rear surface to no longer include water, and solid is rendered as Dark grey or dark-brown.Break Glass tubing after the cooling gently into pieces, take out column form object.Measure column form object ultimate compression strength.
Experimental result: the working fluid pH9.5 of configuration gained.The 1h supernatant liquor accounts for cumulative volume 19.1%.No longer mobile behind the static 5h of working fluid in the Glass tubing.Induration ultimate compression strength is 0.65MPa after 3 days.
Embodiment 4:
Get 10 parts of oily sludges, 10 parts of cement, 5 parts of flyash, 5 parts of sodium sulfate (solidifying agent), 70 parts of tap water.Place beaker, under 500r/min, stir 15min, make its thorough mixing homogeneous.Unload whipping appts, will stir resulting working fluid and pour in the glass test tube of 300mm * 22mm (internal diameter), Glass tubing leaves standstill natural subsidence 1h measures the supernatant liquor height.Tipping supernatant liquor behind the 5h after observing solid and not flowing mutually, places 60 ℃ of water-baths experiments with test tube, after three days Glass tubing is taken out, and the Glass tubing unstopper places 60 ℃ of bakings of baking oven 20h, has dried by the fire with the rear surface to no longer include water, and solid is rendered as Dark grey or dark-brown.Break test tube after the cooling gently into pieces, take out column form object.Measure its ultimate compression strength.
Experimental result: the system pH9.5 of configuration gained.The 1h supernatant liquor accounts for cumulative volume 19.6%.No longer mobile behind the static 5h of working fluid in the Glass tubing.Column form object ultimate compression strength is 0.55MPa after 3 days.
Precaution of the present invention:
1) after oily sludge of the present invention adds prescription, adds high salinity well water and stir the colloidal working fluid that mixes that is made into solid content 30%-45%.For the ease of site operation, early stage, solid settlement can not be too fast, working fluid must have time enough in ground transport and infusion, yet need the time to allow colloid have certain fluidity early stage after entering the stratum, allow amendment fully flow into the profile control face, site operation requires to be no more than 20% for 0.5-1h left and right sides amendment working fluid supernatant liquor ratio.Specific practice is to pour in the Glass tubing of an end closure mixing the working fluid that stirs gained, leaves standstill the ratio that 1h measures the shared system cumulative volume of supernatant liquor volume; Stirring is difficult for too fast, because system is the organic-inorganic mixed system, sometimes also added a spot of tensio-active agent, bubble in the too fast meeting increase system, and these bubbles stable existence in system is difficult for discharging, after working fluid entered bottom, bubble more can't effectively be discharged, and this will reduce the curing system intensity in later stage;
2) must be able to not flow behind the working fluid 5h of gained.Amendment is filled into some specific duct that 3-5h behind the stratum should arrive the profile control face substantially, no longer circulation, and the curing in later stage also requires these colloids in relatively stable environment chemical reaction to take place.So also should in addition strict control to the colloid 5h flowability in the Glass tubing, specific practice is to be inverted test tube after room temperature leaves standstill 5h, observes its flowability, immobilising prescription could satisfy the requirement of amendment;
3) 60 ℃ of water (oil) were bathed experiment after gained sample 5h did not substantially flow, and allowed system become adhesive curing, and 3d takes out the solid ultimate compression strength after the induration measurement is solidified later on.Ultimate compression strength was about 0.5MPa after one was used for the curing of solidifiability amendment of water injection well, and one just can be used for the macropore profile control of well.
Main ingredient mass content in the oily sludge in the oil field, Gudao area of Shengli Oilfield area among the embodiment 1-3.(seeing attached list 1)
Each component concentration such as following table in subordinate list 1 oily sludge
Water content is measured according to measurement of water ratio method in " GB26-77 " crude oil products and two kinds of methods of direct oven drying method in the oily sludge.
Organic content makes with the following method in the oily sludge: after oily sludge is washed soluble salt off among the embodiment 3, filter cake washes repeatedly with the methylene dichloride that heavily steams, all solvents are accepted with beaker, liquid clarification up to the funnel lower end, gained dark-brown liquid is spin-dried for solvent, weighing gained quality of organic matter.Obtain the organic content of oily sludge.Organic matter is done Infrared spectroscopy.(see figure 1)
The sandy sandy main component of the preliminary understanding of power spectrum of doing of the intact organic gained of used oily sludge wash-out among the embodiment 3.(see figure 2)
Claims (5)
1. inorganic profile control agent with oil sludge, it is characterized in that including oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent forms through mixed preparing, described tensio-active agent is a Sodium dodecylbenzene sulfonate, each raw materials by weight portion is counted: oily sludge 10-15, cement 5-25, flyash 0-5, solidifying agent 0-10, retardant 0-10, tensio-active agent 0-0.2.
2. by the described inorganic profile control agent with oil sludge of claim 1, it is characterized in that described retardant is that gac is or/and the phosphorus ore slag.
3. by claim 1 or 2 described inorganic profile control agent with oil sludge, it is characterized in that described solidifying agent is that sodium sulfate is or/and ammonium chloride.
4. the application method of inorganic profile control agent with oil sludge, it is characterized in that taking by weighing oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent, described tensio-active agent is a Sodium dodecylbenzene sulfonate, each raw materials by weight portion is counted: oily sludge 10-15, cement 5-25, flyash 0-5, solidifying agent 0-10, retardant 0-10, tensio-active agent 0-0.1, add water and stir the colloidal working fluid that mixes that is made into solid content 30%-45%, behind natural subsidence 0.5-1h, obtain the working fluid of amendment, guarantee that the supernatant liquor ratio is no more than 20%, must be able to not flow behind the working fluid 5h of the amendment of gained, by profile control equipment amendment is filled into the stratum at last, be completion of cure behind the experience 72-150h.
5. by the application method of the described inorganic profile control agent with oil sludge of claim 4, it is characterized in that described whipping step is meant under the 500-800r/min condition to stir 10-20min.
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CN101451061A (en) * | 2008-12-30 | 2009-06-10 | 山东大学 | Sand consolidation and water plugging profile control agent made by oil sand |
CN101475295A (en) * | 2008-12-30 | 2009-07-08 | 中国石化股份胜利油田分公司孤东采油厂 | Recycling method for oilfield oil sand |
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CN103965848B (en) * | 2014-04-29 | 2017-02-08 | 中国石油大学(华东) | Composite profile control agent and preparation method thereof |
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CN106968654A (en) * | 2017-04-10 | 2017-07-21 | 中国石油化工股份有限公司 | Method is altered in a kind of profile control suppression of heavy crude well |
CN109943307A (en) * | 2019-04-26 | 2019-06-28 | 中国石油大学(华东) | The method that foam solution blocked during heavy crude heat extraction for profile control and preparation method thereof and foam system and profile control block |
CN109943307B (en) * | 2019-04-26 | 2020-04-03 | 中国石油大学(华东) | Foam solution for profile control plugging in thick oil thermal recovery process, preparation method thereof, foam system and profile control plugging method |
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