CN108300438A - A kind of inorganic aluminum Gelling Water shutoff Agent - Google Patents
A kind of inorganic aluminum Gelling Water shutoff Agent Download PDFInfo
- Publication number
- CN108300438A CN108300438A CN201810112923.4A CN201810112923A CN108300438A CN 108300438 A CN108300438 A CN 108300438A CN 201810112923 A CN201810112923 A CN 201810112923A CN 108300438 A CN108300438 A CN 108300438A
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- CN
- China
- Prior art keywords
- water shutoff
- shutoff agent
- water
- agent
- salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
- C09K8/516—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls characterised by their form or by the form of their components, e.g. encapsulated material
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices, or the like
- E21B33/138—Plastering the borehole wall; Injecting into the formation
Abstract
The present invention relates to one kind being suitable for inorganic aluminum Gelling Water shutoff Agent, and it includes following components as raw material：Methenamine, aluminum soluble salt and complexing agent.The water shutoff agent can under cryogenic conditions (30~50 DEG C) plastic, the stifled requirement of low-temperature reservoir tune can be met；System gelation time is controllable；It is applicable to high salinity stratum；Better heat stability；With preferable salt resistant character；With preferable sealing characteristics and flushing resistance.
Description
Technical field
The present invention relates to one kind being suitable for inorganic aluminum Gelling Water shutoff Agent.Particularly, the present invention relates to one kind being suitable for low temperature
The inorganic aluminum Gelling Water shutoff Agent on stratum.
Background technology
China is land, which to have 80% or more oil field, is developed in a manner of waterflooding extraction.But due to stratum and stream
The reasons such as the anisotropism of body cause oil well water breakthrough.Profile control and water plugging technology is to improve waterflood recovery efficiency factor most efficient method.Each
In kind of profile control and water plugging technology, polymer weak gel is widely used, but it is higher with gelling temperature, not resistant to shearing and in glue
The larger disadvantage of loss of strength after body aging dehydration；Phenolic resin system gelation time under cryogenic conditions (20-40 DEG C) is longer,
Gelling strength is low；To the oil reservoir less than 40 DEG C, most common profile-controlling and plugging agent is chromium gel, but the chromium ion in chromium gel can be right
Environment causes damages.
Prior art discloses some blocking agents, wherein being used as host agent using partially hydrolyzed polyacrylamide (PHPA) (HPAM), use
Chromium acetate or chromium propionate and methenamine are (big see, for example, Tianjin science and technology to obtain polymer weak gel as crosslinking agent
Learn Master dissertation in 2012, " research of polyacrylamide gel water plugging profile control agent ", author Zhang Peng；Daqing Petroleum Institute
Master degree candidate's academic dissertation in 2010, " research of deep profile controlling cross-linking system ", author Luan Hongbo).Its gelation mechanism is：Three
The chromium ion of valence, which crosslinks after hydration, hydrolysis, ol bridge effect with HPAM molecules, to react, and it is (i.e. poly- to obtain three-dimensional net structure
Close object Weak Gels).The shortcomings that above-mentioned prior art system, is：(1) salt tolerance is low, in " polyacrylamide gel water plugging and profile controlling
In the research of agent " (Zhang Peng) text, obtained polyacrylamide gel ties up to 1.5%CaCl2In the case of, dehydration is serious；
In " research of deep profile controlling cross-linking system " (Luan Hongbo) text, obtained Organic Chromium deep profile controlling cross-linking system is applicable in mine
Change degree is only 4000-7000mg/L, this is because the electric double layer for the cation meeting comperession polymer being added, makes polymer charge base
Repulsion between group reduces, and to make polymer molecule draw closer together, promotes crosslinking；(2) heat resistance is low, because as host agent
Polyacrylamide may will produce chain rupture, to influence the performance of gel, reduce the service life of gel, part formulation is 45
10 days i.e. serious dehydration at DEG C, the stabilization time of optimization formula is also only above 10 days；(3) resistant to shearing poor performance, above-mentioned each body
System has used the great polyacrylamide of molecular weight to make host agent, therefore when system pumped in the earth formation, borehole, formation pore etc.
When shear action, viscosity necessarily has certain loss.
Therefore, there is an urgent need in the art to a kind of water shutoff agents suitable for low temperature formation that can overcome the above problem.
Invention content
In an aspect, the present invention provides a kind of inorganic aluminum Gelling Water shutoff Agent, it includes following components as raw material：
Methenamine, aluminum soluble salt and complexing agent.
In the water shutoff agent of the present invention, the aluminum soluble salt is preferably aluminium chloride, aluminum sulfate or aluminum nitrate etc..It is described can
Dissolubility aluminium salt can be in anhydrous form, for example, anhydrous Aluminum chloride or anhydrous slufuric acid aluminium；Or can be in hydrated form, for example, six water
Close aluminium chloride, Patent alum.Preferably, the aluminum soluble salt is aluminium chloride, more preferably anhydrous Aluminum chloride.
In the water shutoff agent of the present invention, the complexing agent be citric acid or and its salt, ethylene diamine tetra methylene phosphonic acid and its salt,
Hydroxy ethylene diphosphonic acid and its salt, hydrolysis of polymaleic anhydride, 2- phosphonic acid butane -1,2,4- tricarboxylic acids and its salt.The salt
Preferably soluble-salt, such as sylvite, sodium salt or ammonium salt.Preferably, the complexing agent be citric acid or and its salt, preferably lemon
Lemon acid trisodium, citric acid tri potassium or Triammonium citrate.The complexing agent can be in hydrate form, for example, two citric acid monohydrates three
Sodium or monohydrate potassium tripotassium.The number-average molecular weight of hydrolysis of polymaleic anhydride can be 100-10000, preferably 200-5000,
More preferably 300-3000, most preferably 400-1000, degree of hydrolysis can be 10-90%, preferably 20-80%, more preferably 30-
70%, most preferably 30-40%.
In the water shutoff agent of the present invention, the dosage of methenamine is 5-15%, preferably 6-15%, more preferably 8-
11%, the total weight based on the water shutoff agent.
In the water shutoff agent of the present invention, the dosage of aluminum soluble salt is 1-10%, preferably 2-8%, more preferably 3-
6%, the total weight based on the water shutoff agent.
In the water shutoff agent of the present invention, the dosage of complexing agent is 1-8%, and preferably 1-5%, more preferably 2-4% are based on
The total weight of the water shutoff agent.
The water shutoff agent of the present invention is inorganic water shutoff agent, is free of polymer such as polyacrylamide gel.
Water shutoff agent of the present invention is prepared with water, and the water can be fresh water, tap water or water flooding, preferably water flooding.This hair
Bright system salt tolerance is preferable, therefore applicable formation water salinity range is wider.Even if when Na ion concentration reaches
When 192550mg/L or calcium ion concentration reach 41000mg/L, system of the invention still has preferable gelation time and plastic
Intensity.
The pH value of water shutoff agent of the present invention can be about 5.5- about 8, preferably from about 6.5- about 7.5.
In another aspect, the present invention relates to a kind of method preparing water shutoff agent of the present invention, include the following steps：In water
Complexing agent and aluminum soluble salt is added, so that the two is reacted, methenamine is then added.
Preferably, make the complexing agent and soluble aluminum reactant salt 1-30 minutes, preferably 5-20 minutes, more preferable 10-15
Minute, methenamine is then added.The reaction temperature of complexing agent and methenamine is not particularly limited, usually at about 5-40 DEG C
At a temperature of carry out, such as carry out at room temperature.
In another aspect, the present invention relates to a kind of water plugging and profile controlling methods comprising injects ground by the water shutoff agent of the present invention
Under, so that it is reacted under reservoir temperature, to form gel.
Online injection can be used in the system of the present invention, this is also system of the present invention relative to other polymerization species water shutoff agents
Advantage.In contrast, traditional polymer water plugging agent to stratum when injecting, it is necessary to ground by proportioning, dispersion, curing,
Filtering, storage and etc., wherein maturation stage refers to polymer dry powder particle being changed into solution by dispersion in water
Process.The step for only curing just needs at least 4 hours, will also be subjected to the processes such as storage, mixing after curing.And the present invention
The water shutoff agent of online injection may be implemented in injects water shutoff agent while water shutoff agent system is prepared on ground to stratum, and whole process is time saving
Input that is laborsaving, using manpower and material resources sparingly.
The water shutoff agent of the present invention has the following advantages that：
1) can under cryogenic conditions (30~50 DEG C) plastic, the stifled requirement of low-temperature reservoir tune can be met；System gelation time
Controllably, generally 10-40 hours, preferably 15-35 hours, more preferably 20-35 hours；And current Common Polymers Weak Gels
System gelling temperature is higher, it is difficult to meet the closure requirement of low-temperature reservoir, such as Organic Chromium/aldehyde/HPAM Weak Gels systems at
Glue temperature is 90 DEG C；
2) system of the invention is applicable to high salinity stratum, even if making mould when sodium chloride is added into simulated formation water
When quasi- formation water salinity reaches 99047.60mg/L, system gelation time changes also very little；
3) water shutoff agent of the invention can keep higher-strength, i.e. better heat stability under 60 DEG C of environment in 60 days；
4) product of water shutoff agent of the present invention will not dissolve in inorganic salts, therefore have preferable salt resistant character；
5) system of the invention can carry out control system gelling time by using complexing agent, by changing complexing agent and remaining
The relative amount of two components realizes different gelling times；
6) system of the present invention is inorganic system, low at gelatin viscosity, has preferable injection efficiency；And it is stifled to polymerize species
Aqua system viscosity is high, it is more difficult to be injected into stratum；
7) system of the invention has preferable sealing characteristics and flushing resistance；
8) system of the present invention has preferable de-plugging performance.Hydrochloric acid de-plugging can be used in the gel of formation, and plugging removal effect is good
It is good, thus system is low to the potential injury on stratum.
Description of the drawings
Fig. 1 is the single tube experimental model figure for measuring sealing ratiod.The meaning of wherein each reference numeral is as follows：1- tapers
Bottle, 2- twin-tub constant speed and constant pressures pump, 3- six-way valves, 4- intermediate receptacles, 5- triple valves, 6- pressure gauges, 7- fill out sand tube, 8- graduated cylinders.
Below by embodiment, the present invention is further explained.
Embodiment
1. test method
The assay method of 1.1 gelling times
Experiment is using 10ml colorimetric cylinders as reaction vessel.It includes water blockoff of the embodiment of the present invention that 5ml is prepared in colorimetric cylinder
The solution of agent is put into after sealing in baking oven, and the form of water shutoff agent in a colorimetric cylinder is observed every 5min.Colorimetric cylinder is tilted
After 45 °, if liquid level remains unchanged, then it is assumed that water shutoff agent system plastic.Will since colorimetric cylinder is put into baking oven to system at
This time interval of glue is considered as the gelation time of system.
The judgment method of 1.2 gel strengths
Experiment measures gel strength using range estimation code method, and by the way that colorimetric cylinder to be inverted, the plastic state for observing gel is come
Determine that gelling strength, the intensity criteria for classifying use Wang Jian, Luoping is sub-, the development [J] of New Associative Polymer In Profile Control, oil
Drilling technique, 2000,22 (3):The standard determined in 054-56, referring specifically to the following table 1：
Table 1
Water used in embodiment is to utilize sodium chloride, anhydrous chlorination according to the formation water salinity of Bohai Bay Oil indoors
The mineralized water that calcium, Magnesium dichloride hexahydrate, sodium bicarbonate, anhydrous sodium sulfate are prepared, ion composition are as shown in table 2；Used in experiment
Quartz sand mesh number is 40-80 mesh.
2 Bohai Bay Oil SZ36-1 types stratum water ion composition of table
The evaluation method of 1.3 sealing characteristics
The sealing characteristics of water shutoff agent is characterized using sealing ratiod.Experiment is surveyed using single tube experimental model (as shown in Figure 1)
Fixed, fill out sand tube will be injected at glue, and (outer diameter 3.5cm, internal diameter 3.0cm, effective length 29cm, overall length 33cm screw on total after end cap
A length of 38.5cm), it is put into the insulating box of set temperature and reaches gelling time, measure the water after blocking and survey permeability.Sealing ratiod
Calculation formula be：
In formula：E is sealing ratiod, %；Kw0Permeability is surveyed for initial water, μm2；Kw1Permeability is surveyed for water after gelling, μm2。
1.4 flushing resistance
Judge system flushing resistance by the variation of injection pressure.It is measured using single tube experimental model, experiment is surveyed
Determining step is：(1) gravel, making artificial back-up sand rock core are filled into fill out sand tube, and measure core permeability；(2) 0.3 times is injected
The alumina gel of pore volume is put into the insulating box of set temperature at glue and reaches gelling time；(3) simulated formation water pair is used
Fill out sand tube carries out displacement, observes variation tendency of the injection pressure with water drive pore volume injected.
2. general experimental procedure
By in embodiment complexing agent and aluminum soluble salt be added to the water, and both make to react 10-15 minutes at room temperature,
Then methenamine is added and methenamine is made fully to dissolve, obtained sample is stored at different temperatures, according to institute above
The method stated measures its gelling time and gel strength.The formula and test result of each embodiment are referring to the following table 3.
Table 3 is formulated and test result
* hydrolysis of polymaleic anhydride is obtained from Shandong You Suo Chemical Industry Science Co., Ltd, and trade mark GB/T10535-2014, number is
Molecular weight 400~800.
As can be seen from the above table, low-temperature inorganic alumina gel system of the invention has good gel-forming property at low temperature,
The tune for meeting low-temperature reservoir blocks up demand；And the present invention has good sealing characteristics, sealing ratiod has relatively strong 97% or more
Resistance to erosion ability.
In addition, the gelling also to the aluminium chloride system of 9% methenamine in embodiment 3/4% under different amount of complex
Time is tested, wherein different amounts of complexing agent is added, experimental temperature is 40 DEG C, tests gelation time, as a result such as the following table 4
It is shown.
Table 4
| Complexing agent mass fraction | 2.0% | 2.1% | 2.2% | 2.6% |
| Gelling time | 22 | 24 | 26 | 29 |
As can be seen from Table 4, as complexing agent dosage increases, system gelling time constantly increases.
In addition, be also determined to the salt tolerance of 1 system of embodiment, used in water be table 2 water, salinity
For 9047.60mg/L.As a result as shown in table 5 below.
Table 5
| Sodium chloride dosage, g/L | 0 | 5 | 10 | 20 | 40 | 90 |
| Salinity, mg/L | 9047.60 | 14047.60 | 19047.60 | 29047.60 | 49047.60 | 99047.60 |
| Gelation time, h | 23.3 | 22.2 | 21.3 | 21.0 | 24 | 24 |
As can be seen from Table 5, when the salinity significant changes of simulated formation water, the gelation time of system of the present invention changes
It is smaller.Therefore, system of the invention has good salt tolerance.
In addition, being also tested to the temperature tolerance of 1 system of the embodiment of the present invention.By the system after plastic in embodiment 1
It is put into 60 DEG C of baking ovens, the gel strength of system is observed at any time, as a result referring to the following table 6.
Table 6
| Time/d | 0 | 2 | 6 | 20 | 40 | 60 |
| Gel grade | D | F | H | H | I | I |
As can be seen from Table 6, it when by the system of the present invention, constant temperature places 60d under 60 DEG C of plastic environment, remains to
Keep higher strength grade.This fully proves that the system of the present invention has preferable stability.
It can be seen from foregoing embodiments the present invention water shutoff agent can under cryogenic conditions (30~50 DEG C) plastic, can expire
The stifled requirement of sufficient low-temperature reservoir tune；System gelation time is controllable；It is applicable to high salinity stratum；Better heat stability；Have
Preferable salt resistant character；With preferable sealing characteristics and flushing resistance.
Claims (9)
1. a kind of inorganic aluminum Gelling Water shutoff Agent, it includes following components as raw material：Methenamine, aluminum soluble salt and complexing
Agent.
2. inorganic aluminum Gelling Water shutoff Agent as described in claim 1, wherein the aluminum soluble salt is aluminium chloride, aluminum sulfate or nitre
Sour aluminium.
3. inorganic aluminum Gelling Water shutoff Agent as claimed in claim 1 or 2, wherein the complexing agent be citric acid or and its salt, second
Four methylenephosphonic acid of diamines and its salt, hydroxy ethylene diphosphonic acid and its salt, hydrolysis of polymaleic anhydride, phosphonic acid butane -1,2 2-,
4- tricarboxylic acids and its salt, preferably citric acid and its salt, more preferably trisodium citrate, citric acid tri potassium or Triammonium citrate.
4. inorganic aluminum Gelling Water shutoff Agent as claimed in any one of claims 1-3, the wherein dosage of methenamine are 5-15%,
Preferably 6-15%, more preferably 8-11%, the total weight based on the water shutoff agent.
5. the inorganic aluminum Gelling Water shutoff Agent as described in any one of claim 1-4, wherein the dosage of the aluminum soluble salt is
1-10%, preferably 2-8%, more preferably 3-6%, the total weight based on the water shutoff agent.
6. the inorganic aluminum Gelling Water shutoff Agent as described in any one of claim 1-5, wherein the dosage of the complexing agent is 1-
8%, preferably 1-5%, more preferably 2-4%, the total weight based on the water shutoff agent.
7. the inorganic aluminum Gelling Water shutoff Agent as described in any one of claim 1-6, wherein the water shutoff agent is used selected from fresh water, certainly
The water of water or water flooding is prepared.
8. a kind of method preparing the inorganic aluminum Gelling Water shutoff Agent as described in any one of claim 1-7, includes the following steps：
Complexing agent and aluminum soluble salt are added in water, so that the two is reacted, methenamine is then added.
9. a kind of water plugging and profile controlling method comprising will be the inorganic aluminum Gelling Water shutoff Agent as described in any one of claim 1-7
Water shutoff agent injects underground, so that it is reacted under reservoir temperature, to form gel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810112923.4A CN108300438A (en) | 2018-02-05 | 2018-02-05 | A kind of inorganic aluminum Gelling Water shutoff Agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810112923.4A CN108300438A (en) | 2018-02-05 | 2018-02-05 | A kind of inorganic aluminum Gelling Water shutoff Agent |
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| CN108300438A true CN108300438A (en) | 2018-07-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111534293A (en) * | 2020-04-29 | 2020-08-14 | 扬州大学 | Temperature-responsive self-lubricating hydrogel profile control agent and preparation method thereof |
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| US20040102331A1 (en) * | 2002-11-22 | 2004-05-27 | Chan Keng Seng | Selective stimulation with selective water reduction |
| CN101787268A (en) * | 2009-12-31 | 2010-07-28 | 新疆新易通石油科技有限公司 | Gel profile control agent for delaying generation of precipitation granules and preparation method thereof |
| CN104140801A (en) * | 2013-10-29 | 2014-11-12 | 中国石油化工股份有限公司 | Aluminum gel oil displacement profile control agent and preparation method thereof |
-
2018
- 2018-02-05 CN CN201810112923.4A patent/CN108300438A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040102331A1 (en) * | 2002-11-22 | 2004-05-27 | Chan Keng Seng | Selective stimulation with selective water reduction |
| CN101787268A (en) * | 2009-12-31 | 2010-07-28 | 新疆新易通石油科技有限公司 | Gel profile control agent for delaying generation of precipitation granules and preparation method thereof |
| CN104140801A (en) * | 2013-10-29 | 2014-11-12 | 中国石油化工股份有限公司 | Aluminum gel oil displacement profile control agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111534293A (en) * | 2020-04-29 | 2020-08-14 | 扬州大学 | Temperature-responsive self-lubricating hydrogel profile control agent and preparation method thereof |
| CN111534293B (en) * | 2020-04-29 | 2022-07-05 | 扬州大学 | Temperature-responsive self-lubricating hydrogel profile control agent and preparation method thereof |
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Inventor after: Wang Zenglin Inventor after: Chen Haolin Inventor after: Fan Haiming Inventor after: Zheng Tong Inventor after: Zhao Jingbing Inventor after: An Huitong Inventor after: Qi Xiang Inventor after: Kang Wanli Inventor after: Dai Caili Inventor before: Fan Haiming Inventor before: Chen Haolin Inventor before: Zheng Tong Inventor before: Zhao Jingbing Inventor before: An Huitong Inventor before: Qi Xiang Inventor before: Kang Wanli Inventor before: Dai Caili |
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