CN106433587A - Combined plugging agent - Google Patents
Combined plugging agent Download PDFInfo
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- CN106433587A CN106433587A CN201610828367.1A CN201610828367A CN106433587A CN 106433587 A CN106433587 A CN 106433587A CN 201610828367 A CN201610828367 A CN 201610828367A CN 106433587 A CN106433587 A CN 106433587A
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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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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Abstract
The invention provides a combined plugging agent. The combined plugging agent is prepared from, by mass, 0.2%-0.4% of partially hydrolyzed polyacrylamide, 0.1%-0.3% of a novel hydrophobic associated polymer, 0.1%-0.4% of a phosphate crosslinking agent, 0.05%-0.08% of a phenol crosslinking agent, 0.05%-0.08% of an aldehyde crosslinking agent, 0.03%-0.06% of a phenolic resin crosslinking agent, 0.2%-0.4% of a stabilizer, 0.05%-0.15% of a dehydration inhibitor, and the sum of the components is 100%, wherein the phosphate crosslinking agent is one of sodium hexametaphosphate and sodium pyrophosphate or the combination of sodium hexametaphosphate and sodium pyrophosphate; the phenol crosslinking agent is one of phenol and resorcinol or the combination of phenol and resorcinol; the aldehyde crosslinking agent is polyformaldehyde; the stabilizer is one of thiourea and sodium sulfite or the combination of thiourea and sodium sulfite; the dehydration inhibitor is sodium succinate. The combined plugging agent can form gel within the temperature of 45-120 DEG C, the gelling time is adjusted within 16-48 h, no dehydration or shrinkage phenomenon exists after aging is performed for 120 days under the temperature of 250 DEG C, the temperature resistance is excellent, the problem of steam channeling in the thick oil thermal recovery process can be solved, the combined plugging agent can be used for high-temperature oil deposit water plugging, and can also be adopted as a profile control and water shutoff agent of a near wellbore area and an oil well deep area.
Description
Technical field：
The present invention relates to a kind of resistance to envelope of low temperature plastic high-temperature stable alters composite plugging agent, more particularly, to partial hydrolysiss polyacrylamide
Amine/new hydrophobic association polymer is combined frozen glue, belongs to technical field of oilfield chemistry.
Background technology：
Gradually step into the middle and late stage stage with conventional oil gas field development, the nontraditional reservoir such as viscous crude, super-viscous oil becomes China
The emphasis of following petrol resources exploitation.The major way of heavy crude producing is steam soak and steam drives at present.But in steam injection
During exploitation, on the one hand there is steam overlap；On the other hand interlayer after excessive round operation, is being led to permeate
Rate difference increases, and oil-producing formation gas entry profile is uneven, and the high-temperature steam of injection is advanced by leaps and bounds along preferential path, channeling, fingering phenomenon
Seriously.Therefore, carry out the research of steam hot-producing high-temp blocking agent profile control technique, become the key improving recovery factor of heavy oil reservoir.Mesh
Before, domestic and international heavy crude heat extraction High Temperature Plugging Agent mainly has grain-type water shutoff agent, organic high temperature frozen glue, high temperature foam blocking agent, hot thixotroping
Polymeric system etc..Grain-type water shutoff agent, mainly in the form of suspended substance, the inorganic particles such as cement, flyash, bentonite is injected
The effect of closure is played on stratum.Although having the advantages that plugging strength height, temperature tolerance are good, the defect of grain-type water shutoff agent is it
Closure to stratum does not have selectivity, easily whole reservoir is damaged, and is only limitted near wellbore zone closure.Organic high temperature freezes
Glue mainly has tannic extract, lignin frozen glue and modified polyacrylamide frozen glue.Tannic extract class blocking agent price is more cheap, but uses process
Middle tannic extract and cross-linking agent concentration are higher, substantially increase development cost it is impossible to enough use in a large number.Modified polyacrylamide
The frozen glue being formed is limited in higher temperature (180 DEG C) stability inferior.High temperature foam blocking agent can suppress the onlap of steam, simultaneously system
In surfactant can also effectively reduce oil water interfacial tension, emulsified crude oil, improve displacement efficiency.Can be used in 250 DEG C at present
High-temp foaming agent mainly have alkylbenzenesulfonate, alpha-alkene sulfonate, but domestic by long-chain alpha-olefin raw material and sulfonation technology
Limitation, there is no the alkylbenzenesulfonate that straight chained alkyl is more than 20 and alpha-alkene sulfonate Surfactant Industryization to produce at present
Product, surely the technology of steeping there is also defect to high temperature simultaneously.Hot thixotroping system has hot thixotroping temperature and hot thixotroping gel strength is adjustable, note
The advantages of entering property and sealing ratiod are high, but heat-resisting quantity is still poor, even if after adding clay, just has started to be dehydrated after 4h at 200 DEG C.
Under currently low oil price situation, exploitation one kind can under Conventional cryogenic heavy crude reservoir temperature conditionss plastic it is adaptable to remote well ground
With profile control, low cost and the good blocking agent of resistance to elevated temperatures is significant to the exploitation of heavy crude reservoir.
Content of the invention：
For the deficiencies in the prior art, the invention aims to provide a kind of composite plugging agent, can low temperature (45 DEG C～
120 DEG C) under the conditions of stable under plastic and hot conditionss, be mainly used in heavy crude reservoir closure channeling.
Technical scheme is as follows：
A kind of composite plugging agent, is made up of host, cross-linking agent, stabilizer, dehydration inhibitor and water, and described host is low in hydrolysis
Degree partially hydrolyzed polyacrylamide (PHPA) and the mixture of new hydrophobic association polymer, described cross-linking agent is phosphate cross-linking agent, phenol
The mixture of class cross-linking agent, aldehyde crosslinking agent and phenolic resin crosslinking agent, described stabilizer is reducing substanceses, described dehydration suppression
Preparation is strong base-weak acid salt, and the mass percent composition of each component is as follows：
Lower degrees of hydrolysis partially hydrolyzed polyacrylamide (PHPA) 0.2%～0.4%；
New hydrophobic association polymer 0.1%～0.3%；
Phosphate cross-linking agent 0.1%～0.4% is sodium hexameta phosphate and one of sodium pyrophosphate or combine；
Phenolic crosslinkers 0.05%～0.08% are phenol and one of resorcinol or combine；
Aldehyde crosslinking agent 0.05%～0.08%, is paraformaldehyde；
Phenolic resin crosslinking agent 0.03%～0.06%, is phenol-formaldehyde resin modified HSX；
Stabilizer 0.2%～0.4% is thiourea and one of sodium sulfite or combine；
Dehydration inhibitor 0.05%～0.15%, is sodium succinate；
Water, surplus；
The mass percent sum of above-mentioned each component is 100%.
The relative molecular mass of the preferably described new hydrophobic association polymer of the present invention is 500 × 104～700 × 104；Excellent
The relative molecular mass selecting Lower degrees of hydrolysis partially hydrolyzed polyacrylamide (PHPA) is 800 × 104～1000 × 104, degree of hydrolysis be 10%～
15%.
The preparation method of above-mentioned composite plugging agent is as follows：
1st, partially hydrolyzed polyacrylamide (PHPA) and new hydrophobic association polymer are pressed aforementioned proportioning fully molten in tap water
Solution, standby；
2nd, press proportioning by phosphate cross-linking agent, Phenolic crosslinkers, aldehyde crosslinking agent, phenolic resin crosslinking agent, stabilizer, mistake
Water inhibitor and excess water mixing and stirring；Above two solution mixing and stirring is obtained plastic liquid.
3rd, glue will be become to be placed in ampoule bottle, sinter sealing with alcohol blast burner, be placed in aging 16 in 45～120 DEG C of baking oven
～48h obtains final product composite plugging agent of the present invention.
The frozen glue gelation time of the present invention is 16～48h.
The invention has the beneficial effects as follows：
1st, new hydrophobic association polymer used in the present invention has auto polymerization property, can gradually form cause at high temperature
Close 3 D stereo network-like structure, by solution be wrapped in lose flowability.Host partially hydrolyzed polyacrylamide (PHPA) and crosslinking
The space net structure that agent carries out cross-linking reaction formation is mutual with the network structure that new hydrophobic association polymer auto polymerization is formed
It is wound around, further increase the density of frozen glue network.New hydrophobic association polymer carries amide group, Ke Yiyu simultaneously
Phosphate, phenolic aldehyde cross-linking system produce crosslinked action further, drastically increase the cancellated moisture holding capacity of frozen glue so that
The intensity of frozen glue, heat stability greatly improve.
2nd, the host that the present invention uses is partially hydrolyzed polyacrylamide (PHPA), adds a small amount of new hydrophobic association polymer, becomes
Originally substantially reduce, in new hydrophobic association polymer used, contain hydrophobic group, configuration is simple, become gelatin viscosity relatively low, injection
Functional.Phenol, aldehyde cross-linking agent and phenolic resin crosslinking agent are used in conjunction with, and compensate for single cross-linking system on high salinity stratum
Under the conditions of cross-link intensity is weak, the problem of easy dehydration.
3rd, this formula equal energy plastic in 45～120 DEG C of temperature ranges, the new hydrophobic association polymer of interpolation can not only
Enough improve gel strength, and be not dehydrated after 120 days through 250 DEG C of high-temperature heat treatment after low temperature plastic, heat stability greatly improves.
Therefore, this formula disclosure satisfy that the requirement of plastic under different heavy crude reservoir formation temperatures.Gelation time 16-48h is adjustable simultaneously, energy
Enough meet nearly well, the needs of remote well area profile control simultaneously.
Specific embodiment：
In order to be more clearly understood from the present invention, now specific embodiments of the present invention are explained in detail, but this
Invention institute protection domain is not limited only to this.
Embodiment 1：
In beaker add 0.1g sodium hexameta phosphate, 0.03g paraformaldehyde, 0.03g resorcinol, 0.3g sodium sulfite,
0.05g sodium succinate, plus tap water is to 50g, stirs so as to abundant dissolve, then the quality that 50g is prepared with tap water is dense
Spend the mixed solution of the partially hydrolyzed polyacrylamide (PHPA) for 0.5% and new hydrophobic association polymer that mass concentration is 0.1%
Mix with above-mentioned solution, stir, that is, the frozen glue obtaining the present invention becomes glue.Sinter sealing with alcohol blast burner, be placed in temperature
In 55 DEG C of baking oven, aging 28h obtains final product composite plugging agent of the present invention.
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
Fill out sand tube filling quartz sand grain for 30cm is obtained simulation core, is denoted as 1#, obtains original permeability after water drive to pressure stability
k1, then by above-mentioned one-tenth glue inverse injection fill out sand tube, injected slurry volume is 0.6PV (rock pore volume), is then injected into
0.3PV water is replaced, and after the sealing of two ends, fill out sand tube is placed in aging 28h plastic in 55 DEG C of constant temperature ovens, fill out sand tube is placed in
Aging 30 days and 90 days respectively in 250 DEG C of baking ovens, finally water drive, to pressure stability, records the stifled rear permeability of simulation core respectively
k2, and press formula E=(k1-k2)/k1* 100%, calculate reservoir core plugging rate E, experimental result is as shown in table 1 below.
Table 1
Embodiment 2：
In beaker add 0.15g sodium hexameta phosphate, 0.05g paraformaldehyde, 0.05g resorcinol, 0.3g sodium sulfite,
0.1g sodium succinate, plus 3%NaCl aqueous solution is to 50g, stirs so as to abundant dissolve, then 50g is prepared with tap water
Mass concentration be 0.5% partially hydrolyzed polyacrylamide (PHPA) and new hydrophobic association polymer that mass concentration is 0.2% mixed
Close solution to mix with above-mentioned solution, stir, that is, the frozen glue obtaining the present invention becomes glue.Sinter sealing with alcohol blast burner, put
In the baking oven of 65 DEG C of temperature, aging 32h obtains final product composite plugging agent of the present invention.
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
Fill out sand tube filling quartz sand grain for 30cm is obtained simulation core, is denoted as 2#, obtains original permeability after water drive to pressure stability
k1, then by above-mentioned one-tenth glue inverse injection fill out sand tube, injected slurry volume is 0.6PV (rock pore volume), is then injected into
0.3PV water is replaced, and after the sealing of two ends, fill out sand tube is placed in aging 32h plastic in 65 DEG C of constant temperature ovens, fill out sand tube is placed in
Aging 30 days and 90 days respectively in 250 DEG C of baking ovens, finally water drive, to pressure stability, records the stifled rear permeability of simulation core respectively
k2, and press formula E=(k1-k2)/k1* 100%, calculate reservoir core plugging rate E, experimental result is as shown in table 2 below.
Table 2
Embodiment 3：
0.15g sodium hexameta phosphate, 0.05g paraformaldehyde, 0.05g resorcinol, 0.3g thiourea, 0.1g is added in beaker
Sodium succinate, stirs, plus 7%NaCl aqueous solution is to 50g so as to abundant dissolve, then the quality that 50g is prepared with tap water
Concentration be 0.5% partially hydrolyzed polyacrylamide (PHPA) and new hydrophobic association polymer that mass concentration is 0.4% mixing molten
Liquid is mixed with above-mentioned solution, stirs, that is, the frozen glue obtaining the present invention becomes glue.Sinter sealing with alcohol blast burner, be placed in temperature
In the baking oven of 75 DEG C of degree, aging 35h obtains final product composite plugging agent of the present invention.
For investigating the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
Spend the fill out sand tube filling quartz sand grain for 30cm and simulation core is obtained, be denoted as 3#, after water drive to pressure stability, obtain original infiltration
Rate k1, then by above-mentioned one-tenth glue inverse injection fill out sand tube, injected slurry volume is 0.6PV (rock pore volume), is then injected into
0.3PV water is replaced, and after the sealing of two ends, fill out sand tube is placed in aging 35h plastic in 75 DEG C of constant temperature ovens, fill out sand tube is placed in
Aging 30 days and 90 days respectively in 250 DEG C of baking ovens, finally water drive, to pressure stability, records the stifled rear permeability of simulation core respectively
k2, and press formula E=(k1-k2)/k1* 100%, calculate reservoir core plugging rate E, experimental result is as shown in table 3 below.
Table 3
Embodiment 4：
0.2g sodium hexameta phosphate, 0.06g paraformaldehyde, 0.06g resorcinol, 0.03g modified phenolic is added in beaker
Resin HSX, 0.3g thiourea, 0.15g sodium succinate, plus 10%NaCl aqueous solution is to 50g, stirs so as to abundant dissolve, then
By 50g tap water prepare mass concentration be 0.5% partially hydrolyzed polyacrylamide (PHPA) and mass concentration be 0.4% new dredge
The mixed solution of water association polymer is mixed with above-mentioned solution, stirs, that is, the frozen glue obtaining the present invention becomes glue.Use ethanol
Blowtorch sintering sealing, is placed in aging 38h in the baking oven of 85 DEG C of temperature and obtains final product composite plugging agent of the present invention.
For investigating the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
Spend the fill out sand tube filling quartz sand grain for 30cm and simulation core is obtained, be denoted as 4#, after water drive to pressure stability, obtain original infiltration
Rate k1, then by above-mentioned one-tenth glue inverse injection fill out sand tube, injected slurry volume is 0.6PV (rock pore volume), is then injected into
0.3PV water is replaced, and after the sealing of two ends, fill out sand tube is placed in aging 38h plastic in 85 DEG C of constant temperature ovens, fill out sand tube is placed in
Aging 30 days and 90 days respectively in 250 DEG C of baking ovens, finally water drive, to pressure stability, records the stifled rear permeability of simulation core respectively
k2, and press formula E=(k1-k2)/k1* 100%, calculate reservoir core plugging rate E, experimental result is as shown in table 4 below.
Table 4
Embodiment 5：
In beaker add 0.3g sodium hexameta phosphate, 0.08g paraformaldehyde, 0.08g resorcinol, 0.04g phenol,
0.04g phenol-formaldehyde resin modified HSX, 0.3g thiourea, 0.15g sodium succinate, plus 10%NaCl+0.3%CaCl2Aqueous solution to 50g,
Stir so as to abundant dissolve, then the partial hydrolysiss polyacrylamide that the mass concentration that 50g tap water is prepared is 0.8%
Amine and the mixed solution that mass concentration is 0.4% new hydrophobic association polymer are mixed with above-mentioned solution, stir, that is, obtain
The frozen glue of the present invention becomes glue.Sinter sealing with alcohol blast burner, be placed in aging 43h in the baking oven of 95 DEG C of temperature and obtain final product institute of the present invention
State composite plugging agent.
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
Fill out sand tube filling quartz sand grain for 30cm is obtained simulation core, is denoted as 5#, obtains original permeability after water drive to pressure stability
k1, then by above-mentioned one-tenth glue inverse injection fill out sand tube, injected slurry volume is 0.6PV (rock pore volume), is then injected into
0.3PV water is replaced, and after the sealing of two ends, fill out sand tube is placed in aging 43h plastic in 95 DEG C of constant temperature ovens, fill out sand tube is placed in
Aging 30 days and 90 days respectively in 250 DEG C of baking ovens, finally water drive, to pressure stability, records the stifled rear permeability of simulation core respectively
k2, and press formula E=(k1-k2)/k1* 100%, calculate reservoir core plugging rate E, experimental result is as shown in table 5 below.
Table 5
Embodiment 6：
In beaker add 0.3g sodium hexameta phosphate, 0.1g sodium pyrophosphate, 0.08g paraformaldehyde, 0.08g resorcinol,
0.06g phenol, 0.05g phenol-formaldehyde resin modified HSX, 0.3g thiourea, 0.15g sodium succinate, plus 10%NaCl+
0.3%CaCl2+ 0.3%MgCl2Aqueous solution, to 50g, stirs so as to abundant dissolve, then the matter that 50g is prepared with tap water
Amount concentration be 0.8% partially hydrolyzed polyacrylamide (PHPA) and mixing that mass concentration is 0.6% new hydrophobic association polymer molten
Liquid is mixed with above-mentioned solution, stirs, that is, the frozen glue obtaining the present invention becomes glue.Sinter sealing with alcohol blast burner, be placed in temperature
In the baking oven of 120 DEG C of degree, aging 48h obtains final product composite plugging agent of the present invention.
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
Fill out sand tube filling quartz sand grain for 30cm is obtained simulation core, is denoted as 6#, obtains original permeability after water drive to pressure stability
k1, then by above-mentioned one-tenth glue inverse injection fill out sand tube, injected slurry volume is 0.6PV (rock pore volume), is then injected into
0.3PV water is replaced, and after the sealing of two ends, fill out sand tube is placed in aging 48h plastic in 120 DEG C of constant temperature ovens, fill out sand tube is placed in
Aging 30 days and 90 days respectively in 250 DEG C of baking ovens, finally water drive, to pressure stability, records the stifled rear permeability of simulation core respectively
k2, and press formula E=(k1-k2)/k1* 100%, calculate reservoir core plugging rate E, experimental result is as shown in table 6 below.
Table 6
From table 1 to table 6 test result indicate that, frozen glue formula provided by the present invention, in larger temperature, salinity scope
Interior gel-forming property is good, and after 250 DEG C of high temperature is aging, sealing characteristics is good, and sealing ratiod, more than 90%, is favorably improved crude oil and adopts
Yield.
Claims (3)
1. a kind of composite plugging agent is it is characterised in that be made up of following components and its mass percent：Partially hydrolyzed polyacrylamide (PHPA)
0.2%～0.4%, new hydrophobic association polymer 0.1%～0.3%, phosphate cross-linking agent 0.1%～0.4%, phenols are crosslinked
Agent 0.05%～0.08%, aldehyde crosslinking agent 0.05%～0.08%, phenolic resin crosslinking agent 0.03%～0.06%, stabilizer
0.2%～0.4%, dehydration inhibitor 0.05%～0.15% and excess water, the mass percent sum of each component is 100%,
Wherein, phosphate cross-linking agent is one of sodium hexameta phosphate and sodium pyrophosphate or combines；Phenolic crosslinkers are phenol and resorcinol
One of or combination；Aldehyde crosslinking agent is paraformaldehyde；Phenolic resin crosslinking agent is phenol-formaldehyde resin modified HSX；Stabilizer is thiourea
With one of sodium sulfite or combine；Dehydration inhibitor is sodium succinate.
2. composite plugging agent according to claim 1 is it is characterised in that the average molecular of described partially hydrolyzed polyacrylamide (PHPA)
Quality is 800 × 104～1000 × 104, degree of hydrolysis is 10%～15%.
3. composite plugging agent according to claim 1 is it is characterised in that described new hydrophobic association polymer average molecular matter
Measure as 500 × 104～700 × 104.
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| CN108531159A (en) * | 2018-04-11 | 2018-09-14 | 东北石油大学 | A kind of High Temperature Plugging Agent system for heavy crude heat extraction oil reservoir |
| CN111087986A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Composite gel plugging agent and preparation method and application thereof |
| CN111286311A (en) * | 2020-03-03 | 2020-06-16 | 中国石油天然气股份有限公司 | Multiple cross-linking type polymer gel profile control agent and application thereof |
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| CN111087986A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Composite gel plugging agent and preparation method and application thereof |
| CN111826143B (en) * | 2019-04-22 | 2022-06-03 | 中国石油天然气股份有限公司 | Thermosetting foam plugging agent and application thereof |
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| CN112852393B (en) * | 2019-11-28 | 2022-10-04 | 中国石油天然气股份有限公司 | High-temperature-resistant plugging agent for thick oil horizontal well and water plugging method |
| CN112852393A (en) * | 2019-11-28 | 2021-05-28 | 中国石油天然气股份有限公司 | High-temperature-resistant plugging agent for thick oil horizontal well and water plugging method |
| CN111286311A (en) * | 2020-03-03 | 2020-06-16 | 中国石油天然气股份有限公司 | Multiple cross-linking type polymer gel profile control agent and application thereof |
| CN114106800A (en) * | 2020-08-26 | 2022-03-01 | 中国海洋石油集团有限公司 | Bisphenol S and formaldehyde cross-linked high-temperature-resistant gel blocking agent |
| CN113249103A (en) * | 2021-06-01 | 2021-08-13 | 中国石油大学(华东) | Seawater-based polyacrylamide high-temperature jelly profile control system |
| CN116218494A (en) * | 2021-12-06 | 2023-06-06 | 中国石油天然气股份有限公司 | Composite auxiliary agent, deep profile control crosslinking agent, preparation method and application thereof |
| CN116218494B (en) * | 2021-12-06 | 2024-04-12 | 中国石油天然气股份有限公司 | Composite auxiliary agent, deep profile control crosslinking agent, preparation method and application thereof |
| CN117247771A (en) * | 2023-11-10 | 2023-12-19 | 中国石油大学(华东) | Particle composite gel reinforced foam system and preparation method and application thereof |
| CN117247771B (en) * | 2023-11-10 | 2024-03-29 | 中国石油大学(华东) | Particle composite gel reinforced foam system and preparation method and application thereof |
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