CN105062444A - High temperature swellable granule plugging agent and preparation method thereof - Google Patents
High temperature swellable granule plugging agent and preparation method thereof Download PDFInfo
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- CN105062444A CN105062444A CN201510477938.7A CN201510477938A CN105062444A CN 105062444 A CN105062444 A CN 105062444A CN 201510477938 A CN201510477938 A CN 201510477938A CN 105062444 A CN105062444 A CN 105062444A
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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Abstract
The invention relates to a high temperature swellable granule plugging agent and a preparation method thereof. The raw materials include, by mass, 20-50% of acrylamide, 20-50% of acrylic acid, 1-15% of sodium hydroxide, 2-10% of inner rigid particles, 0.1-0.5% of ammonium persulfate, 0.05%-0.25% of sodium bisulfite, 0.1-0.5% of N, N-methylene-bisacrylamide, 1-5% of dodeyl methacrylate and the balance water. The high temperature swellable granule plugging agent provided by the invention has the plugging mechanism of ordinary profile control agents used as profile control and water plugging agents, has a flexible outer layer, and can deform and advance in stratum, when the flexible outer layer is destroyed and lose efficacy, the internal rigid inner core still can form effective plugging to the stratum so as to realize stratum successive deep profile control and flooding, thus reaching the purposes of twice plugging and increase of plugging time. The high temperature swellable granule plugging agent is applicable to a stratum temperature below 200DEG C, has a water-absorbent expanding multiple of 20-40 times and a rock core plugging rate of greater than 98%, and after 10PV (pore volume) injected water scouring, the plugging rate still remains above 96%. The high temperature swellable granule plugging agent is suitable for profile control and water plugging of ordinary oil-water wells, and also can be applied to profile control and channel plugging of heavy oil thermal recovery wells.
Description
Technical field
The present invention relates to oil-field thick-oil producing oil layer High Temperature Plugging Agent and preparation method thereof, belong to technical field of oilfield chemistry, specifically a kind of high temperature volume expansion grain blocking agent and preparation method thereof.
Background technology
At present in heavy crude heat extraction, the high-temperature steam of injection trends towards rising to oil reservoir top, forms steam and alter in macropore most permeable zone, reduces steam utilization and volumetric conformance efficiency, causes steam entry profile uneven, reduces exploitation effect.In addition, heavy crude heat extraction district enters many rounds and handles up after the stage, due to the nonuniformity on stratum, the impact of the factor such as mobility ratio difference and steam overlap, cause vapour, water breakthrough situation is on the rise, part well steam injection pressure is low, and steam injection efficiency is poor, cause idlely adopting liquid, invalidly to handle up, even cause water logging.Therefore, the profile control and water plugging operation carrying out thick oil thermal extraction seems particularly important.For steam macropore problem in heavy crude heat extraction, it is inorganic particle class blocking agent because cost is lower that the blocking agent profile control and water plugging technology of development mainly contains following three kinds: one, temperature tolerance is good, obtain in thick oil thermal extraction profile control envelope is altered and apply comparatively widely, but there is injection difference, inject radius shorter, the defects such as plugging strength is lower, add that inorganic particle belongs to rigid particles, not yielding, size was difficult to hold with zone permeability and mating of duct size, easily cause difficult injection and form filter cake at the borehole wall, or the problem that shutoff does not live, thus cause can not effectively macropore plugging and validity period shorter, also easy certain injury is caused to Middle-Low Permeability Reservoirs.Two is that organic polymer class blocking agent comprises polymer gel, polymer microballoon etc., heat resistance is poor, salt resistant character is limited, plugging strength is lower, and resistance to erosion ability is lower, and cost is higher, prepare and inject more loaded down with trivial details, alter water plugging effect as thick oil thermal extraction envelope poor, validity period is shorter, particularly oozes the shutoff of macropore for height not ideal.Three is that hydroexpanding body type blocking agent has the unrivaled advantage of other water blockoff adjusting driving agnet, and achieves the effect increasing oil, precipitation preferably.But the water suction of the part hydroexpanding body blocking agent existence of onsite application is too fast at present, and expansion multiple is excessive, and intensity is less, and temperature tolerance is poor, and scour resistance is poor, the problem that sealing characteristics is not good enough.
Summary of the invention
Object of the present invention is exactly for above-mentioned the deficiencies in the prior art part, provides swollen blocking agent of a kind of high-temperature body and preparation method thereof.
Above-mentioned purpose is achieved through the following technical solutions:
Raw material composition mass ratio in high temperature volume expansion grain blocking agent and preparation method thereof is: acrylamide is 20 ~ 50%, vinylformic acid is 20 ~ 50%, sodium hydroxide 1 ~ 15%, interior just particle is 2 ~ 10%, and Ammonium Persulfate 98.5 is 0.1 ~ 0.5%, and sodium bisulfite is 0.05% ~ 0.25%, N, N-methylene-bisacrylamide is 0.1 ~ 0.5%, and lauryl fat is 1 ~ 5%, and all the other are water.
Water in above-mentioned high temperature volume expansion grain blocking agent and preparation method thereof is the clear water of salinity lower than 500mg/L.
Each component in above-mentioned high temperature volume expansion grain blocking agent and preparation method thereof is commercially available prod, described sodium hydroxide, vinylformic acid, acrylamide, sodium soil, sodium bisulfite, persulfuric acid, N,N methylene bis acrylamide, lauryl fat are chemical pure.
Interior firm particle in above-mentioned high temperature volume expansion grain blocking agent and preparation method thereof is any one in carclazyte, sodium soil, gac, zeolite powder, rubber powder.
Preparation method in above-mentioned high temperature volume expansion grain blocking agent and preparation method thereof is: first in reaction vessel, add water, then sodium hydroxide is added, vinylformic acid is added after stirring and dissolving is even, be stirred well to and mix, then under whipped state, lauryl fat is added, acrylamide and interior firm particle, stirring is warming up to 40 DEG C, when inflated with nitrogen is protected, add N, N-methylene-bisacrylamide, then 80 DEG C are warming up to, add sodium bisulfite and ammonium persulphate, stirring reaction two hours, take out finished product, shred oven dry, then powder is ground into, obtained high temperature volume expansion grain blocking agent.
Beneficial effect of the present invention is: have the shutoff mechanism that common amendment is used as profile-controlling and plugging agent, there is flexible outer layer, propelling can be out of shape in the earth formation, after flexible outer layer damage inactivation, inner rigid inner core still formation can cause effective shutoff, realize stratum successively deep profile correction, reach secondary plugging, increase the object of shutoff timeliness, adapting to formation temperature is less than 200 DEG C, water-absorbent expanding multiple 20 ~ 40 times, reservoir core plugging rate is greater than 98%, through 10PV(volume of voids) inject water and wash away, sealing ratiod still keeps more than 96%, adapt to the profile control and water plugging with conventional oil well, also the profile control envelope that can be applicable to thick oil thermal extraction is altered.
Accompanying drawing explanation
Fig. 1-rock core displacement device schematic diagram.
Injection pressure and the relation curve injecting hole system of Fig. 2-embodiment 7 blocking agent.
In figure, 1. constant-flux pump, 2. intermediate receptacle, 3. six-way valve, 4. precision pressure gauge, 5. core holding unit, 6. graduated cylinder; PV-X-coordinate, injects hole system, Mpa-ordinate zou, injection pressure.
Embodiment
For further illustrating the present invention, below enumerate specific embodiment, but institute of the present invention protection domain is not limited only to this.
embodiment 1
High temperature volume expansion grain blocking agent, raw material forms:
Acrylamide 20.9%, vinylformic acid 20.9%, sodium hydroxide 4.6%, sodium soil 2.9%, ammonium persulphate 0.25%, sodium bisulfite 0.5%, N,N methylene bis acrylamide 0.1%, lauryl fat 1.5%, all the other are water.
Preparation method:
First in 500ml there-necked flask, 180ml water is added, add 20g sodium hydroxide, 90ml vinylformic acid is added after stirring and dissolving is even, be stirred well to and mix, then under whipped state, add 6.5g lauryl fat, 90g acrylamide and 12.6g sodium soil, stirring is warming up to 40 DEG C, add 0.4gN, N-methylene-bisacrylamide, is then warming up to 80 DEG C, adds the sodium bisulfite of 10ml1% and the ammonium persulphate of 20ml1%, stirring reaction 2h, take out finished product, shred oven dry, be ground into powder.
Gained high temperature volume expansion grain blocking agent water-swelling test case: under normal temperature condition, the water-swelling quality multiple in tap water is 32 times; Be water-absorbent expanding multiple in 40% ethanol in mass concentration it is 5 times; Water-absorbent expanding multiple in 10g/L sodium chloride solution is 29 times.
embodiment 2
As described in Example 1, gained high temperature volume expansion grain blocking agent sealing characteristics test case is as follows: under 60 DEG C of conditions, and (rate of permeation is 1.12 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 24.6MPa/m; Reservoir core plugging rate is 99.6%; Inject water through 10PV to wash away, blocking agent is 98.6% to the sealing ratiod of rock core.
embodiment 3
As described in Example 1, gained high temperature volume expansion grain blocking agent sealing characteristics test case is as follows: burin-in process high temperature volume expansion grain blocking agent 7 days at 150 DEG C of temperature, (rate of permeation is 1.20 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 20.9MPa/m; Burin-in process high temperature volume expansion grain blocking agent 7 days at 200 DEG C of temperature, (rate of permeation is 1.23 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 14.2MPa/m.
embodiment 4
As described in Example 1, gained high temperature volume expansion grain blocking agent sealing characteristics secondary plugging test case is as follows: under 60 DEG C of conditions, record same concentrations, under identical injection rate, the shutoff scouring effect of different blocking agent system is shown in Fig. 2.
The injection pressure of Fig. 2 high temperature volume expansion grain blocking agent occurs two " steps ", and first pressure " step " is that after the blocking agent particulate water absorbent injected expands, formation causes shutoff; Along with washing away of follow-up injection water, the flexible outer layer of high temperature volume expansion grain blocking agent is destroyed, pressure drop, but owing to having rigid inner core, still formation can cause effective shutoff, pressure-stabilisation is at second " step ", and the shutoff in the earth formation of high temperature volume expansion grain blocking agent embodies the feature of secondary plugging.And other class particle blocking agent systems do not embody the feature of secondary plugging.
reference examples 1
Commercially available water-swelling type hydroexpanding body, water-swelling test case:
Under normal temperature condition, the water-swelling quality multiple in tap water is 79 times; Be water-absorbent expanding multiple in 40% ethanol in mass concentration it is 4 times; Water-absorbent expanding multiple in 10g/L sodium chloride solution is 19 times.
reference examples 2
Commercially available water-swelling type hydroexpanding body, sealing characteristics test case:
Under 60 DEG C of conditions, (rate of permeation is 0.98 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 18.7MPa/m; Reservoir core plugging rate is 96.6%; Inject water through 10PV to wash away, blocking agent is 86.8% to the sealing ratiod of rock core.
reference examples 3
Commercially available water-swelling type hydroexpanding body, heatproof sealing characteristics test case:
Burin-in process high temperature volume expansion grain blocking agent 7 days at 150 DEG C of temperature, (rate of permeation is 1.32 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 2.9MPa/m; Burin-in process high temperature volume expansion grain blocking agent 7 days at 200 DEG C of temperature, (rate of permeation is 1.03 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 1.1MPa/m.
Claims (3)
1. high temperature volume expansion grain blocking agent and preparation method thereof, it is characterized in that: raw material composition mass ratio is: acrylamide is 20 ~ 50%, vinylformic acid is 20 ~ 50%, sodium hydroxide 1 ~ 15%, and interior firm particle is 2 ~ 10%, Ammonium Persulfate 98.5 is 0.1 ~ 0.5%, sodium bisulfite is 0.05% ~ 0.25%, and N,N methylene bis acrylamide is 0.1 ~ 0.5%, lauryl fat is 1 ~ 5%, and all the other are water.
2. high temperature volume expansion grain blocking agent according to claim 1 and preparation method thereof, is characterized in that: described interior firm particle is any one in carclazyte, sodium soil, gac, zeolite powder, rubber powder.
3. high temperature volume expansion grain blocking agent according to claim 1 and preparation method thereof, its preparation method is: first in reaction vessel, add water, then sodium hydroxide is added, vinylformic acid is added after stirring and dissolving is even, be stirred well to and mix, then under whipped state, lauryl fat is added, acrylamide and interior firm particle, stirring is warming up to 40 DEG C, when inflated with nitrogen is protected, add N, N-methylene-bisacrylamide, then 80 DEG C are warming up to, add sodium bisulfite and ammonium persulphate, stirring reaction two hours, take out finished product, shred oven dry, then powder is ground into, obtained high temperature volume expansion grain blocking agent.
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| CN201510477938.7A CN105062444A (en) | 2015-08-07 | 2015-08-07 | High temperature swellable granule plugging agent and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106640000A (en) * | 2016-09-13 | 2017-05-10 | 中国石油大学(华东) | Expandable graphite plugging agent system for deep channel blocking of heavy oil reservoir steam flooding and injection method |
| CN108690584A (en) * | 2018-05-18 | 2018-10-23 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | A kind of compound profile control agent |
| CN109915115A (en) * | 2019-04-02 | 2019-06-21 | 中国石油大学(华东) | Determine the method and device of the closure matching relationship of elastic granule and formation pore throat |
| CN109957377A (en) * | 2019-04-28 | 2019-07-02 | 祝亚琴 | A kind of closure dispersing agent |
| CN111434748A (en) * | 2019-01-11 | 2020-07-21 | 中国石油化工股份有限公司 | Organic/inorganic hybrid high-temperature-resistant plugging gel for well drilling and preparation method thereof |
| CN112321777A (en) * | 2020-11-20 | 2021-02-05 | 西安博众科技发展有限责任公司 | Nano composite microsphere plugging agent for water shutoff and profile control of low-permeability oil field and preparation method thereof |
| US11612525B2 (en) | 2017-12-21 | 2023-03-28 | Essity Hygiene And Health Aktiebolag | Absorbent article and method for manufacturing an absorbent article |
| US11793683B2 (en) | 2017-12-21 | 2023-10-24 | Essity Hygiene And Health Aktiebolag | Absorbent article and method for manufacturing an absorbent article |
| US11833015B2 (en) | 2017-12-21 | 2023-12-05 | Essity Hygiene And Health Aktiebolag | Absorbent article and method for manufacturing an absorbent article |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106640000A (en) * | 2016-09-13 | 2017-05-10 | 中国石油大学(华东) | Expandable graphite plugging agent system for deep channel blocking of heavy oil reservoir steam flooding and injection method |
| CN106640000B (en) * | 2016-09-13 | 2018-06-08 | 中国石油大学(华东) | Viscous oil field operated by steam Deep channel blocking expansible graphite blocking agent system and method for implanting |
| US11612525B2 (en) | 2017-12-21 | 2023-03-28 | Essity Hygiene And Health Aktiebolag | Absorbent article and method for manufacturing an absorbent article |
| US11793683B2 (en) | 2017-12-21 | 2023-10-24 | Essity Hygiene And Health Aktiebolag | Absorbent article and method for manufacturing an absorbent article |
| US11833015B2 (en) | 2017-12-21 | 2023-12-05 | Essity Hygiene And Health Aktiebolag | Absorbent article and method for manufacturing an absorbent article |
| CN108690584A (en) * | 2018-05-18 | 2018-10-23 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | A kind of compound profile control agent |
| CN111434748A (en) * | 2019-01-11 | 2020-07-21 | 中国石油化工股份有限公司 | Organic/inorganic hybrid high-temperature-resistant plugging gel for well drilling and preparation method thereof |
| CN109915115A (en) * | 2019-04-02 | 2019-06-21 | 中国石油大学(华东) | Determine the method and device of the closure matching relationship of elastic granule and formation pore throat |
| CN109915115B (en) * | 2019-04-02 | 2022-06-14 | 中国石油大学(华东) | Method and device for determining plugging matching relationship between elastic particles and stratum pore throats |
| CN109957377A (en) * | 2019-04-28 | 2019-07-02 | 祝亚琴 | A kind of closure dispersing agent |
| CN112321777A (en) * | 2020-11-20 | 2021-02-05 | 西安博众科技发展有限责任公司 | Nano composite microsphere plugging agent for water shutoff and profile control of low-permeability oil field and preparation method thereof |
| CN112321777B (en) * | 2020-11-20 | 2023-02-14 | 西安博众科技发展有限责任公司 | Nano composite microsphere plugging agent for water plugging and profile control of low-permeability oil field and preparation method thereof |
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Application publication date: 20151118 |