CN104745162A - Emulsified and cross-linked oil-containing sludge profile control agent - Google Patents
Emulsified and cross-linked oil-containing sludge profile control agent Download PDFInfo
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- CN104745162A CN104745162A CN201510088462.8A CN201510088462A CN104745162A CN 104745162 A CN104745162 A CN 104745162A CN 201510088462 A CN201510088462 A CN 201510088462A CN 104745162 A CN104745162 A CN 104745162A
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- oily sludge
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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Abstract
The invention discloses an emulsified and cross-linked oil-containing sludge profile control agent. The profile control agent is prepared from the following raw materials in percentage by weight: 5-15% of oil-containing slurry, 0.1-0.5% of an emulsifier, 0.6-0.8% of a suspending agent, 1-3% of a cross-linker and the balance of water. The slurry content of the profile control agent is 3-5%, sludge with particle size distribution less than 100 microns accounts for more than 90%, and most oil-containing slurry is less than 50 microns in particle size. The profile control agent is excellent stability, oil-water layering time is more than 70h and water bleeding amount within 24h is less than 10mL; the cementing time of the profile control agent is more than 12h, jelly strength is more than 50000mPa.s, and the blocking rate for cores differing in permeability is more than 90%; and the profile control agent can meet the requirements of profile control construction in the field.
Description
Technical field
The present invention relates to oil field amendment technical field, particularly relate to a kind of emulsification and cross linked oily sludge base profile modificator.
Background technology
Oil field mining liquid defines self-cleaning oil and oilfield sewage after processed.And oilfield sewage is in regeneration process, bottom buffering slurry tank and water tank, form one deck dark thick liquid gradually, i.e. oily sludge.Due to the additive such as oilfield stimulation auxiliary agent, crude oil chemical demulsifier, produced water disposal agent containing remnants, this oily sludge has larger activity, after measured, water content 20% ~ 40% in oily sludge, silt content 30% ~ 60%, oleaginousness 10% ~ 30%, size distribution is less than 100 μm and accounts for more than 90%.Oil field produces a large amount of oily sludges every year, and because disposal of oily sludge amount is large, the method process such as expropriation of land can only be adopted to deposit, bury, is unfavorable for environment protection.Therefore, the process of oily sludge or regeneration, become the difficult problem that domestic and international each oil field is researched and solved.
Water content higher in oily sludge is that the pumping of amendment lays the foundation, and integrated distribution and higher silt content, the oleaginousness of particle diameter have possessed the condition entering stratum and shutoff High Permeability Interval.Utilize oily sludge to originate in stratum, have the favorable factor of good compatibleness with oil reservoir, chemical treatment is implemented to oily sludge, becomes oily sludge base profile modificator, for Thief zone Profile Control in Injection Well, to oil field environment-protection and oil-field development all tool have very important significance.
Summary of the invention
The invention provides a kind of emulsification and cross linked oily sludge base profile modificator.
The present invention adopts following technical scheme:
Emulsification and cross linked oily sludge base profile modificator of the present invention is made up of the raw material of following weight percent: oily sludge 5-15%, emulsifying agent 0.1-0.5%, suspension agent 0.6-0.8%, linking agent 1-3%, all the other are water.Preferably be made up of the raw material of following weight percent: oily sludge 10%, emulsifying agent 0.3%, suspension agent 0.8%, linking agent 2%, all the other are for water.
Described oily sludge is buffering slurry tank and water tank bottom precipitation, and silt content is between 30-50wt%, and size distribution is less than 100 μm and accounts for more than 90%, and most of oily sludge particle diameter is less than 50 μm.
Described emulsifying agent is emulsifying agent DQX-1, and emulsifying agent DQX-1 is obtained by epoxy chloropropane and reacting ethylenediamine, is a kind of emulsifying agent with cationic property.
Described suspension agent is suspension agent CPAM, and suspension agent CPAM is compound ion polyacrylamide, and molecular weight is greater than 5,000,000, and cationic degree is greater than 10%.CPAM not only plays the effect of solid particulate in suspension oily sludge, and can participate in plastic under the effect of linking agent, improves the gel-strength of oily sludge base profile modificator and the plugging rate to profile control stratum.
Described linking agent is organic chromium solution linking agent, phenol resin solution linking agent or urea solids phenol-formaldehyde resin linking agent.Preferably urea solids phenol-formaldehyde resin linking agent.Urea solids phenol-formaldehyde resin linking agent increases the quantity of resol crosslinked group, introduces the methylol crosslinked group on urea-formaldehyde resin, and crosslinking ability improves; Be a kind of powdery product, improve the stability of linking agent, transport performance and shelf-time.
Positively effect of the present invention is as follows:
In oily sludge base profile modificator of the present invention between silt content 3%-5%, size distribution is less than 100 μm and accounts for more than 90%, and most of oily sludge particle diameter is less than 50 μm.Amendment has good stability, and profit separation time is greater than 70h, and 24h condensate rate is less than 10mL; Amendment gelation time is greater than 12h, and gel-strength is greater than 50000mPas, is greater than 90% to the plugging rate of different rate of permeation rock core, can meet the requirement of field profile control construction.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1
Emulsification and cross linked oily sludge base profile modificator of the present invention is made up of the raw material of following weight percent: oily sludge 5%, emulsifying agent 0.5%, suspension agent 0.6%, linking agent 3%, all the other are water.
Described oily sludge is buffering slurry tank and water tank bottom precipitation, and silt content is between 30-50wt%, and size distribution is less than 100 μm and accounts for more than 90%, and most of oily sludge particle diameter is less than 50 μm.
Described emulsifying agent is emulsifying agent DQX-1, and emulsifying agent DQX-1 is obtained by epoxy chloropropane and reacting ethylenediamine, is a kind of emulsifying agent with cationic property.
Described suspension agent is suspension agent CPAM, and suspension agent CPAM is compound ion polyacrylamide, and molecular weight is greater than 5,000,000, and cationic degree is greater than 10%.
Described linking agent is organic chromium solution linking agent.
Embodiment 2
Emulsification and cross linked oily sludge base profile modificator of the present invention is made up of the raw material of following weight percent: oily sludge 15%, emulsifying agent 0.1%, suspension agent 0.8%, linking agent 1%, all the other are water.
Described oily sludge is buffering slurry tank and water tank bottom precipitation, and silt content is between 30-50wt%, and size distribution is less than 100 μm and accounts for more than 90%, and most of oily sludge particle diameter is less than 50 μm.
Described emulsifying agent is emulsifying agent DQX-1, and emulsifying agent DQX-1 is obtained by epoxy chloropropane and reacting ethylenediamine, is a kind of emulsifying agent with cationic property.
Described suspension agent is suspension agent CPAM, and suspension agent CPAM is compound ion polyacrylamide, and molecular weight is greater than 5,000,000, and cationic degree is greater than 10%.
Described linking agent is phenol resin solution linking agent.
Embodiment 3
Emulsification and cross linked oily sludge base profile modificator of the present invention is made up of the raw material of following weight percent: oily sludge 10%, emulsifying agent 0.3%, suspension agent 0.8%, linking agent 2%, all the other are water.
Described oily sludge is buffering slurry tank and water tank bottom precipitation, and silt content is between 30-50wt%, and size distribution is less than 100 μm and accounts for more than 90%, and most of oily sludge particle diameter is less than 50 μm.
Described emulsifying agent is emulsifying agent DQX-1, and emulsifying agent DQX-1 is obtained by epoxy chloropropane and reacting ethylenediamine, is a kind of emulsifying agent with cationic property.
Described suspension agent is suspension agent CPAM, and suspension agent CPAM is compound ion polyacrylamide, and molecular weight is greater than 5,000,000, and cationic degree is greater than 10%.
Described linking agent is urea solids phenol-formaldehyde resin linking agent.
(1) oily sludge composition analysis
Get a certain amount of oily sludge, its water content is measured by distillation method, then distillation residue are filtered with sand core funnel while hot, and with mixed solvent (sherwood oil and acetone) repetitive scrubbing, till resistates not oil-containing, finally the sand core funnel filling resistates is weighed, in table 1 after constant temperature 12h in 85 DEG C of baking ovens.
Table 1 oily sludge compositional analysis
| Sampling spot | Water content (%) | Silt content (%) | Oleaginousness (%) |
| Buffering slurry tank | 16.9 | 35.3 | 47.8 |
| Bottom water tank | 41.5 | 47.9 | 10.6 |
From table 1, the oily sludge composition of different sites is identical, and just content to some extent
Difference, but silt content is generally between 30%-50%.
(2) oily sludge particle size analysis
By the above-mentioned shale component separated, adopt the sieve of different meshes, survey its size-grade distribution, in table 2.
Table 2 shale component size distribution
From table 2, oily sludge size distribution is less than 100 μm and accounts for more than 90%, and most of oily sludge particle diameter is less than 50 μm.Water content higher in oily sludge is that the pumping of amendment lays the foundation, and the silt content that particle diameter is less and higher has possessed the condition entering stratum and shutoff High Permeability Interval.
(3) determination of emulsifying agent DQX-1 consumption
In order to reduce the interfacial tension of oily sludge, preventing from forming oil, mud, water aggregate, making oily sludge form the dispersion liquid of stable homogeneous, emulsifying agent DQX-1 must be added.In 100mL water, add 10g oily sludge, then add the DQX-1 of different amount, under 1000rev/min, stir 10min, leave standstill, there is the time of profit layering in record, in table 3.
The emulsifying property evaluation of table 3 oily sludge
| Emulsifying agent DQX-1 dosage (%) | Profit separation time (h) |
| 0 | 0.5 |
| 0.1 | 12 |
| 0.2 | 48 |
| 0.3 | 70 |
| 0.4 | 120 |
From table 3, the dosage of DQX-1 adds the stability of oily sludge system, with the increase of DQX-1 dosage, occurs the time lengthening of profit layering.According to the requirement of field profile control construction, the consumption of DQX-1 is advisable 0.3% ~ 0.4%.
(4) determination of suspension agent CPAM consumption
Owing to containing a large amount of shale components in oily sludge, there is different size distribution, for preventing the sedimentation of shale component in oily sludge, suspension agent CPAM must be added.In 100mL water, add 10g oily sludge, then add the CPAM of different amount, stir 10min, leave standstill under 1000rev/min, record 24h condensate rate, in table 4.
The condensate rate of table 4 oily sludge
| Suspension agent CPAM dosage (%) | Condensate rate (mL) |
| 0 | 90.7 |
| 0.1 | 50.1 |
| 0.2 | 22.5 |
| 0.4 | 11.7 |
| 0.6 | 8.1 |
| 0.8 | 5.2 |
From table 4, with the increase of CPAM dosage, the condensate rate of oily sludge reduces, and the stability of system improves, and CPAM has good suspension effect to oily sludge, slow down the settling velocity of solid particulate in oily sludge.According to the requirement of field profile control construction, the consumption of CPAM is advisable 0.6% ~ 0.8%.
(5) determination of urea phenolic resin crosslinking agent consumption
In order to strengthen the intensity of oily sludge base profile modificator, add the gel-strength that urea phenolic resin crosslinking agent improves oily sludge, after adding the urea phenolic resin crosslinking agent of different amount, maintenance at 50 DEG C, the time that record oily sludge base profile modificator loses flowability is gelation time, measure the gel-strength of maintenance 48d, in table 5.
The gelation time of table 5 oily sludge base profile modificator and gel-strength
| Urea phenolic resin crosslinking agent dosage (%) | Gelation time (h) | Gel-strength (mPas) |
| 0 | Do not coagulate | 3200 |
| 0.5 | 36 | 28900 |
| 1.0 | 24 | 48500 |
| 1.5 | 18 | 68900 |
| 2.0 | 12 | 85600 |
From table 5, after urea phenolic resin crosslinking agent dosage is greater than 1.0%, oily sludge base profile modificator can form certain intensity, and with the increase of urea phenolic resin crosslinking agent dosage, oily sludge base profile modificator gelation time shortens, and gel-strength increases.According to the requirement of field profile control construction, the consumption of urea phenolic resin crosslinking agent is advisable 1.0% ~ 2.0%.
(6) oily sludge base profile modificator is to the plugging rate of different rate of permeation rock core
Select the synthetic core of different rate of permeation, inject the oily sludge base profile modificator of 1PV, maintenance 48h at 50 DEG C, measure before blocking up, block up the rate of permeation of rear rock core, calculate plugging rate, in table 6.
Table 6 oily sludge base profile modificator is to the plugging rate of different rate of permeation rock core
| Rate of permeation before rock core is stifled, 10 -3μm 2 | 93.5 | 120 | 235 | 369 |
| Rate of permeation after rock core is stifled, 10 -3μm 2 | 2.6 | 5.3 | 17.8 | 32.8 |
| Plugging rate, % | 97.2 | 95.6 | 92.4 | 91.1 |
From table 6, along with the increase of core permeability, the plugging rate of rock core reduces gradually, but its plugging rate is more than 90%, can meet the requirement of field profile control construction.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (7)
1. an emulsification and cross linked oily sludge base profile modificator, is characterized in that: described amendment is made up of the raw material of following weight percent: oily sludge 5-15%, emulsifying agent 0.1-0.5%, suspension agent 0.6-0.8%, linking agent 1-3%, all the other are water.
2. emulsification and cross linked oily sludge base profile modificator as claimed in claim 1, is characterized in that: described amendment is made up of the raw material of following weight percent: oily sludge 10%, emulsifying agent 0.3%, suspension agent 0.8%, linking agent 2%, all the other are water.
3. emulsification and cross linked oily sludge base profile modificator as claimed in claim 1 or 2, is characterized in that: described oily sludge is buffering slurry tank and water tank bottom precipitation, and silt content is between 30-50wt%, and size distribution is less than 100 μm and accounts for more than 90%.
4. emulsification and cross linked oily sludge base profile modificator as claimed in claim 1 or 2, it is characterized in that: described emulsifying agent is emulsifying agent DQX-1, emulsifying agent DQX-1 is obtained by epoxy chloropropane and reacting ethylenediamine, is a kind of emulsifying agent with cationic property.
5. emulsification and cross linked oily sludge base profile modificator as claimed in claim 1 or 2, is characterized in that: described suspension agent is suspension agent CPAM, and suspension agent CPAM is compound ion polyacrylamide, and molecular weight is greater than 5,000,000, and cationic degree is greater than 10%.
6. emulsification and cross linked oily sludge base profile modificator as claimed in claim 1 or 2, is characterized in that: described linking agent is organic chromium solution linking agent, phenol resin solution linking agent or urea solids phenol-formaldehyde resin linking agent.
7. emulsification and cross linked oily sludge base profile modificator as claimed in claim 1 or 2, is characterized in that: described linking agent is urea solids phenol-formaldehyde resin linking agent.
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| CN105112033A (en) * | 2015-08-21 | 2015-12-02 | 中国石油天然气股份有限公司 | Plugging agent prepared from oil residue or oily sludge and preparation method thereof |
| CN105368421A (en) * | 2015-11-19 | 2016-03-02 | 里群 | Non-resin type profile control agent and application thereof in petroleum exploitation process |
| CN106007296A (en) * | 2016-07-22 | 2016-10-12 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | Oily sludge treatment method |
| CN106433591A (en) * | 2016-08-30 | 2017-02-22 | 陕西海山能源发展有限公司 | Binary-gel-reconstruction-oily-sludge combined with microorganisms profile control and displacement technology |
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| CN107841300A (en) * | 2016-12-20 | 2018-03-27 | 西安思瑞迪能源环保塔器技术工程有限公司 | A kind of oily sludge type profile control and water plugging complexing agent |
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- 2015-02-26 CN CN201510088462.8A patent/CN104745162A/en active Pending
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| CN105112033B (en) * | 2015-08-21 | 2017-12-01 | 中国石油天然气股份有限公司 | Plugging agent prepared from oil residue or oily sludge and preparation method thereof |
| CN105368421A (en) * | 2015-11-19 | 2016-03-02 | 里群 | Non-resin type profile control agent and application thereof in petroleum exploitation process |
| CN105368421B (en) * | 2015-11-19 | 2018-12-21 | 里群 | Non-resinous profile control agent and its application during oil exploitation |
| CN106007296A (en) * | 2016-07-22 | 2016-10-12 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | Oily sludge treatment method |
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| CN107841300A (en) * | 2016-12-20 | 2018-03-27 | 西安思瑞迪能源环保塔器技术工程有限公司 | A kind of oily sludge type profile control and water plugging complexing agent |
| 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 |
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| CN107815300B (en) * | 2017-11-08 | 2020-06-12 | 中国石油化工股份有限公司 | Oil-containing sludge profile control plugging agent and preparation method thereof |
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| CN109609109B (en) * | 2019-01-17 | 2020-11-03 | 长江大学 | Profile control system and preparation method thereof |
| CN110129016A (en) * | 2019-06-21 | 2019-08-16 | 克拉玛依市建业油田技术服务有限责任公司 | Oily sludge resource utilization tune blocks up preparation |
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| CN110964490A (en) * | 2019-10-30 | 2020-04-07 | 中国石油化工股份有限公司 | Plugging adjusting system containing waste drilling fluid and preparation method thereof |
| CN110964490B (en) * | 2019-10-30 | 2022-01-21 | 中国石油化工股份有限公司 | Plugging adjusting system containing waste drilling fluid and preparation method thereof |
| CN111944504A (en) * | 2020-09-23 | 2020-11-17 | 盘锦天诚源科技有限公司 | Preparation method of organic resin coupling agent phenolic resin for oil extraction |
| CN113897185A (en) * | 2021-08-25 | 2022-01-07 | 安徽中科日升科技有限公司 | Oil-based mud waste oil sludge emulsification and reutilization method |
| CN117285213A (en) * | 2023-10-08 | 2023-12-26 | 北京航天中伟科技工程自动化有限公司 | Universal oil field oil-containing dirty sludge recycling reduction treatment process |
| CN117285213B (en) * | 2023-10-08 | 2024-05-10 | 北京航天中伟科技工程自动化有限公司 | Universal oil field oil-containing dirty sludge recycling reduction treatment process |
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Application publication date: 20150701 |