CN101898860B - 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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- CN101898860B CN101898860B CN2010102454299A CN201010245429A CN101898860B CN 101898860 B CN101898860 B CN 101898860B CN 2010102454299 A CN2010102454299 A CN 2010102454299A CN 201010245429 A CN201010245429 A CN 201010245429A CN 101898860 B CN101898860 B CN 101898860B
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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 staple is water, silt particle, gum asphalt and wax.The As China's oil exploitation progressively gets into ultra-high water cut stage, is accompanied by the use that number of chemical auxiliary agent combination flooding replaces, and the output of oily sludge can constantly increase.Oily sludge has characteristics such as generation is big, oleaginousness is high, BO 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, exist radiating dangerous but increasing data shows 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; All only for the crude oil in the oily sludge is being reclaimed, remaining solid is deposited in the well site or the landfill of digging pit to the method for most of oilfield treatments oily sludge.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 basically.
On the other hand; WIW needs a large amount of amendments that use in the oilfield water extraction process, and present amendment kind is a lot, exists a lot of problems also a lot; Flexibility is bad; On the high side, a large amount of chemical assistants forms secondary pollution along with amendment gets into 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, and the profile control working fluid of gained has good suspension property, and 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 high infiltration of macropore WIW and be the displacement of reservoir oil environment that secondary, three water flood recoveries provide.
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, and it is characterized in that including oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent and form through mixed preparing, described tensio-active agent is an X 2073; 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 is characterized in that taking by weighing oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent, and described tensio-active agent is an X 2073; 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 ratio is no more than 20%; Must be able to not flow behind the working fluid 5h of the amendment of gained, through 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 combines the industry standard of construction condition and existing mineral-type amendment, has introduced this intractability great achievement of oily sludge and has divided extremely complicated raw material.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, adds oily sludge separately, and 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, and solidified dominant mechanism is that hydrated cementitious is fixed; Organic type of 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
Below in conjunction with embodiment the present invention is described further, but can not be as to qualification of the present invention.
The reagent chemicals specification and the place of production involved among the present invention are following: 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 CP chemistry reagent, and tensio-active agent is an X 2073, 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 staple 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 X 2073,3 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 height.Tipping supernatant 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, and the surface no longer includes water after having dried by the fire, 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 accounts for TV 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 height.Tipping supernatant 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, and the surface no longer includes water after having dried by the fire, 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 accounts for TV 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 height.Tipping supernatant 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, and the surface no longer includes water after having dried by the fire, 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 accounts for TV 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 height.Tipping supernatant 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, and the surface no longer includes water after having dried by the fire, 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 accounts for TV 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 to annotate in ground transport and pump; Yet need the time to let colloid have certain fluidity early stage after getting into the stratum, lets amendment fully flow into the profile control face, and site operation requires to be no more than 20% for 0.5-1h left and right sides amendment working fluid supernatant 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 TV of supernatant volume; Stirring is difficult for too fast; Because system is the organic-inorganic mixed system, has also added a spot of tensio-active agent sometimes, the bubble in the too fast meeting increase system; And these bubbles stable existence in system is difficult for discharging; After working fluid got into 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 basically, 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 not bathed experiment after gained sample 5h did not basically flow, and let system become adhesive curing, and 3d takes out induration later on and measures the solid ultimate compression strength after solidifying.Ultimate compression strength was about 0.5MPa after one was used for the curing of solidifiability amendment of WIW, 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 cut is measured according to two kinds of methods of measurement of water ratio method in " GB26-77 " crude oil products and direct oven drying method in the oily sludge.
Organic content is used after oily sludge is washed soluble salt off among following method: the embodiment 3 in the oily sludge; Filter cake washes with the methylene dichloride that heavily steams repeatedly; All solvents are accepted with beaker; Up to the liquid clarification of funnel lower end, gained dark-brown liquid revolves dried solvent, weighing gained quality of organic matter.Obtain the organic content of oily sludge.Organic matter is done IR spectroscopy.(see figure 1)
The sandy sandy staple 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 is characterized in that including oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent and forms through mixed preparing, and described tensio-active agent is an X 2073; 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 0.2; Described cement is magnificent new brand of A# normal silicate, Huangshi, Hubei Province, the place of production.
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 is characterized in that taking by weighing oily sludge, cement, flyash, retardant, solidifying agent, tensio-active agent, and described tensio-active agent is an X 2073; 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 0.2; 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 ratio is no more than 20%; Must be able to not flow behind the working fluid 5h of the amendment of gained, through 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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| CN102091712A (en) * | 2010-12-17 | 2011-06-15 | 大庆大丰油田科技有限公司 | Comprehensive utilization method for sludge generated in ASP flooding sewage treatment process |
| CN103965848B (en) * | 2014-04-29 | 2017-02-08 | 中国石油大学(华东) | Composite profile control agent and preparation method thereof |
| CN105295877B (en) * | 2015-10-10 | 2018-03-13 | 中国石油天然气股份有限公司 | Water plugging agent prepared from oil residue or oily sludge and preparation method thereof |
| CN107841300B (en) * | 2016-12-20 | 2020-06-12 | 西安思瑞迪能源环保塔器技术工程有限公司 | Oil-containing sludge type profile control and water shutoff complexing agent |
| CN106833573B (en) * | 2016-12-28 | 2019-05-07 | 中国石油天然气股份有限公司 | Plugging modifier and preparation method and application thereof |
| CN106967400A (en) * | 2017-03-08 | 2017-07-21 | 中国石油天然气股份有限公司 | Slug type oily sludge profile control agent, profile control method and application |
| CN106968654B (en) * | 2017-04-10 | 2019-04-05 | 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 |
| 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 |
| CN110080702B (en) * | 2019-05-21 | 2021-04-09 | 成都西南石大石油工程技术有限公司 | Compound solvent for vibrating screen slurry leakage while-drilling treatment and treatment device |
| CN111635744A (en) * | 2020-04-14 | 2020-09-08 | 中国石油化工股份有限公司 | Composition for profile control and water shutoff, profile control and water shutoff agent and preparation method thereof, and method for resource utilization of white clay residue |
| CN113818869A (en) * | 2021-11-22 | 2021-12-21 | 捷贝通石油技术集团股份有限公司 | Tracing identification and capacity expansion yield increase method for water flooding dominant channel of water-drive reservoir |
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| CN1237145C (en) * | 2003-06-26 | 2006-01-18 | 大庆油田有限责任公司 | Cement fly ash profile control agent for plugging of oil and water well |
| CN101451061B (en) * | 2008-12-30 | 2011-03-16 | 山东大学 | Sand consolidation and water plugging profile control agent made by oil sand |
| CN101475295B (en) * | 2008-12-30 | 2010-09-29 | 中国石化股份胜利油田分公司孤东采油厂 | Recycling method for oilfield oil sand |
| RU2387688C1 (en) * | 2009-01-15 | 2010-04-27 | Владимир Иванович Матыцын | Modified curing composition for hardening mineralised drilling sludge ("мос"-1) |
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