CN106317321B - It is used to prepare the composition of underground crosslinking plural gel and crosslinking plural gel prepared therefrom - Google Patents
It is used to prepare the composition of underground crosslinking plural gel and crosslinking plural gel prepared therefrom Download PDFInfo
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Abstract
The present invention relates to a kind of compositions for being used to prepare underground and being crosslinked plural gel plugging material, and the composition includes cationic alkenyl monomer, calcium carbonate and organic acid.The invention further relates to the preparation methods of the plural gel plugging material, and its application in oil well leak stopping field.
Description
Technical field
The present invention relates to technical field of oilfield chemistry, and in particular to a kind of underground crosslinking plural gel plugging material and its system
Preparation Method.
Background technology
Leakage is always to perplex the major engineering problems of domestic and international petroleum exploration and development, especially severe mud losses, sternly
Drilling safety is threatened again, greatly wellbore construction is hindered to continue.Generally for severe well leakage, more mature method is to make
Leak stopping is carried out with cement class chemical consolidation slurry.But cement mortar anelasticity in leakage channel itself is poor, and it is deep often to flow into drop ply
Place causes leak stopping to fail.Moreover, if drop ply is aqueous or be connected to water table, cement mortar is mixed with stratum water phase, is more difficult to
It is detained, and be difficult to condensation cure or setting strength to reduce, leak stopping is caused to fail.Therefore, the key for handling severe mud losses is to protect
Card sealing agent can be trapped in leakage channel, and avoid being rushed by water flooding dilute.Common bridge joint plugging material, high dehydration
The deficiencies of plugging material, inorganic gel sealing agent, soft or hard plug plugging material, is to successfully manage.
In the above context, gel is valued by people as a kind of novel plugging material.Gel is a kind of half solid
State viscoelastic body is cross-linked to form three-dimensional net structure by water soluble polymer and absorbs a certain amount of water, has stable boundary,
Water phase and an oil phase is difficult mixed, and anti-dilution capacity is strong；With deformability, the pore throat of different sizes and shapes can be adapted to extensively
Or gap, it is filled in formation pore, plays the role of preferable packing to formation fluid；There is preferable adhesiveness with surface of stratum,
Flow resistance is big, and retention effect is good.Based on the above advantage, application of the gel in terms of leak stopping has vast potential for future development.People
The polyacrylamide gel being most commonly chemically crosslinked in the gel of work synthesis.Plain polypropylene acrylamide gel mechanical property is very
Weak, anti-pressure ability is poor and frangible, it is difficult to meet leak stopping demand.Gel body intensity is improved, contributes to the resistance to compression for enhancing gel poor
Driving capability can strengthen barrier of the gel to formation fluid and the closure to drop ply.
Document【Nature, 489,133-136】It is high-strength to be prepared for a kind of calcium alginate-polyacrylamide synchronous making
Spend hydrogel.In composite network structure, polyacrylamide network is double by acrylamide monomer, crosslinking agent N, N '-dimethylene
Acrylamide is copolymerized to be formed；Calcium alginate network passes through sodium alginate aqueous solution and CaSO4·2H2The calcium ion crosslinking shape of O releases
At.But if applying the gel rubber system in blocking construction, there are problems that：Gelation time is short, it is difficult to enter purpose
Stratum forms gel；Gel time is formed to be difficult to adjust.Patent CN103396562A describes one kind and is prepared by two-step method
The method of sodium alginate-polyacrylamide hydrogel, obtained gel strength is high, still, since primary coagulate first is made in two-step method
Glue, then the reaction was continued in the solution into final product by soak, thus it does not have operability (just in drilling leakage blockage
Grade gel can not be pumped into stratum), it is not suitable for blocking construction.
Invention content
The object of the present invention is to provide a kind of compositions preparing underground crosslinking plural gel plugging material and application should
The method that composition prepares plural gel is improved gel body intensity, is enhanced gel using the composition and method of the present invention
Resistance to compression difference driving capability strengthens barrier of the gel to formation fluid and the closure to drop ply.In drilling leakage blockage field, leak stopping work
It is by being conveyed to drop ply inside drilling tool as liquid, too fast formation gel be easy to cause the obstruction of drilling tool.The present invention prepares multiple
The composition for closing gel is reacted with it as calcium ion source, and by using organic acid to control releasing for calcium ion using calcium carbonate
It puts, plays the role of " being sustained ", the time of plastic can be controlled, be particularly suitable for drilling leakage blockage field.
One aspect of the present invention is related to a kind of composition being used to prepare underground crosslinking plural gel plugging material, described
Composition includes cationic alkenyl monomer, calcium carbonate and organic acid.
In a preferred embodiment of the present invention, the composition includes by weight：
In a preferred embodiment of the present invention, the component includes the acrylamide 15-20 by weight
Part, preferably 16-18 parts；2-8 parts of the cationic alkenyl monomer, it is 3-5 parts more preferable；The N, N '-methylene-bisacrylamide
0.01-0.1 parts；Described alginate 4-5 parts；Described calcium carbonate 0.25-1 parts, preferably 0.5-1 parts；The initiator 0.5-1
Part；Described organic acid 1-2 parts.
In a preferred embodiment of the present invention, the cationic alkenyl monomer is selected from acrylyl oxy-ethyl-trimethyl
It is one or more in ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl ammonium chloride, preferably
Acrylyl oxy-ethyl-trimethyl salmiac；The one kind of the alginate in sodium alginate, potassium alginate and ammonium alginate
Or a variety of, preferred sodium alginate；The initiator is one or more in ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, excellent
Select ammonium persulfate；The calcium carbonate is calcium carbonate superfine powder, and average grain diameter is 300-800 mesh.
In a preferred embodiment of the present invention, the one kind of the organic acid in acetic acid, propionic acid and n-butyric acie
Or it is a variety of.
Another aspect of the present invention is related to a kind of method preparing underground crosslinking plural gel, and the method includes following
Step：
By acrylamide, cationic alkenyl monomer, N, N '-methylene-bisacrylamides are added to the water, stirring；Seaweed is added
Hydrochlorate, stirring；Calcium carbonate, stirring is added；Initiator and organic acid, stirring is added；Finally, mixed system reaction is heated to be formed
Gel；Wherein, the stirring in step described above stirs to mixed system and fully dissolves, disperses；And, wherein each component
It is calculated as by weight：
In a preferred embodiment of the present invention, the cationic alkenyl monomer is selected from acrylyl oxy-ethyl-trimethyl
It is one or more in ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl ammonium chloride, preferably
Acrylyl oxy-ethyl-trimethyl salmiac；The one kind of the alginate in sodium alginate, potassium alginate and ammonium alginate
Or a variety of, preferred sodium alginate；The initiator is one or more in ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, excellent
Select ammonium persulfate；The organic acid is one or more in acetic acid, propionic acid and n-butyric acie；The calcium carbonate is ultra-fine carbonic acid
Calcium, average grain diameter are 300-800 mesh.
In a preferred embodiment of the present invention, the one kind of the organic acid in acetic acid, propionic acid and n-butyric acie
Or it is a variety of.
In a preferred embodiment of the present invention, heat reaction reaction temperature be 50 DEG C -90 DEG C, preferably 50 DEG C -
60℃。
In a preferred embodiment of the present invention, the reaction time of heating reaction is 1-5 hours, and preferably 2-3 is small
When.The present invention gel need be used for drilling leakage blockage, therefore, be heated to plastic overlong time or it is too short to practical application not
Profit, for majority of case, the time control that will warm up plastic was preferred within 2-3 hours.
Another aspect of the present invention is related to being crosslinked plural gel by underground prepared by the method.
Another aspect of the present invention is related to application of the plural gel plugging material in oil well leak stopping field.
Beneficial effects of the present invention：
The present invention obtains high-strength gel by building cation acrylamide copolymer-alginate composite network；
In the gel of the present invention, the introducing of cationic alkenyl monomer can generate strong electrostatic adsorption with electronegative surface of stratum, increase
The adhesion strength of strong gel and stratum, improves gel plugging strength；The preparation method of the present invention ensure that system has delayed cross-linking
Feature, can react to form gel slug into leakage channel, formed gel time can adjust, help to improve leak stopping success
Rate.
Specific implementation mode
The present invention is further detailed with reference to embodiments, it should be noted that following embodiment is not anticipated
In the limitation present invention.
Embodiment 1
By 16g acrylamides, 4g acrylyl oxy-ethyl-trimethyl salmiacs, 0.01g N, N '-methylene-bisacrylamides
It is added in 100g water, stirs fully dissolving, 2g sodium alginates are added, stir fully dissolving, 0.25g calcium carbonate superfine powders are added, stir
Fully dispersed, addition 0.2g ammonium persulfates and 0.4g acetic acid are mixed, fully dissolving is stirred, finally, mixed system is placed at 70 DEG C
Reaction, gel is formed after 2 hours.Obtained gel compressive strength (70% strain) is 1.2Mpa.
Embodiment 2
By 10g acrylamides, 10g acrylyl oxy-ethyl-trimethyl salmiacs, 0.05g N, N '-methylene-bisacrylamides
It is added in 100g water, stirs fully dissolving, 1g sodium alginates are added, stir fully dissolving, 1g calcium carbonate superfine powders are added, stirring is filled
1g ammonium persulfates and 1.5g acetic acid is added in dispersion, stirs and fully dissolves, finally, mixed system is placed at 90 DEG C and is reacted, and 1
Gel is formed after hour.Obtained gel compressive strength (70% strain) is 0.8Mpa.
Embodiment 3
15g acrylamides, 5g acrylyl oxy-ethyl-trimethyl salmiacs, 0.1g N, N '-methylene-bisacrylamides are added
Enter in water, stir fully dissolving, 3g sodium alginates are added, 0.5g calcium carbonate superfine powders, abundant point of stirring is added in stirring fully dissolving
It dissipates, 0.5g ammonium persulfates and 1g propionic acid is added, stir fully dissolving, finally, mixed system is placed at 60 DEG C and is reacted, 3 hours
After form gel.Obtained gel compressive strength (70% strain) is 1.5Mpa.
Embodiment 4
By 10g acrylamides, 5g acrylyl oxy-ethyl-trimethyl salmiacs, 0.005g N, N '-methylene-bisacrylamides
It is added to the water, stirs fully dissolving, 0.5g sodium alginates are added, stirs fully dissolving, 0.1g calcium carbonate superfine powders are added, stirring is filled
0.05g ammonium persulfates and 0.2g propionic acid is added in dispersion, stirs and fully dissolves, finally, mixed system is placed at 70 DEG C instead
It answers, gel is formed after 5 hours.Obtained gel compressive strength (70% strain) is 0.9Mpa.
Embodiment 5
By 18g acrylamides, 2g acrylyl oxy-ethyl-trimethyl salmiacs, 0.05g N, N '-methylene-bisacrylamides
It is added to the water, stirs fully dissolving, 4g sodium alginates are added, stir fully dissolving, 0.5g calcium carbonate superfine powders are added, stirring is abundant
0.5g ammonium persulfates and 1g n-butyric acies is added in dispersion, stirs fully dissolving, finally, mixed system is placed at 50 DEG C and is reacted, and 3
Gel is formed after hour.Obtained gel compressive strength (70% strain) is 1.6Mpa.
Embodiment 6
By 10g acrylamides, 2g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 0.005g N, N '-methylene bisacrylamides
Amide is added in 100g water, stirs fully dissolving, 0.5g potassium alginates are added, and stirs fully dissolving, the ultra-fine carbonic acid of 0.05g is added
Calcium, stirring is fully dispersed, and 0.05g potassium peroxydisulfates and 0.1g acetic acid is added, and stirs fully dissolving, finally, mixed system is placed in
It is reacted at 90 DEG C, gel is formed after 5 hours.Obtained gel compressive strength (70% strain) is 1.1Mpa.
Embodiment 7
20g acrylamides, 10g dimethyl diallyl ammonium chlorides, 0.1g N, N '-methylene-bisacrylamides are added
In 100g water, fully dissolving is stirred, 5g ammonium alginates are added, 1g calcium carbonate superfine powders, abundant point of stirring is added in stirring fully dissolving
It dissipates, 1g sodium peroxydisulfates and 2g acetic acid is added, stir fully dissolving, finally, mixed system is placed at 50 DEG C and is reacted, after 1 hour
Form gel.Obtained gel compressive strength (70% strain) is 1.2Mpa.
Embodiment 8
17g acrylamides, 4g acrylyl oxy-ethyl-trimethyl salmiacs, 0.2g N, N '-methylene-bisacrylamides are added
Enter in 100g water, stir fully dissolving, 4g ammonium alginates are added, stirs fully dissolving, 0.5g calcium carbonate superfine powders are added, stirring is filled
1g ammonium persulfates and 1g acetic acid is added in dispersion, stirs and fully dissolves, finally, mixed system is placed at 55 DEG C and is reacted, 2 is small
When after form gel.Obtained gel compressive strength (70% strain) is 1.8Mpa.
Comparative example 1
17g acrylamides, 0.2g N, N '-methylene-bisacrylamides are added in 100g water, fully dissolving is stirred, adds
Enter 4g ammonium alginates, stir fully dissolving, 0.5g calcium carbonate superfine powders are added, stirring is fully dispersed, be added 1g ammonium persulfates and
1.5g acetic acid stirs fully dissolving, finally, mixed system is placed at 55 DEG C and is reacted, gel is formed after 1 hour.What is obtained is solidifying
Glue compressive strength (70% strain) is 1.0Mpa.
Comparative example 2
17g acrylamides, 4g acrylyl oxy-ethyl-trimethyl salmiacs, 0.2g N, N '-methylene-bisacrylamides are added
Enter in 100g water, stir fully dissolving, 4g ammonium alginates are added, 0.5g calcium sulfate, abundant point of stirring is added in stirring fully dissolving
It dissipates, 1g ammonium persulfates is added, stir fully dissolving, finally, mixed system is placed at 55 DEG C and is reacted, formed after 30 minutes solidifying
Glue.Obtained gel compressive strength (70% strain) is 0.5Mpa.
Plugging strength is tested
After the gel prepared by the method for above example is fully absorbed water, it is placed in the logical appearance of the crannied round metal in lower part
In device.Using nitrogen to the piston pressurization of container to push gel downlink, until when it is extruded from crack, record is made at this time
Nitrogen pressure, and it is defined as crush resistance strength.Test result is as shown in table 1：
| Embodiment/comparative example | Crush resistance strength (MPa) |
| Embodiment 1 | 0.66 |
| Embodiment 2 | 0.65 |
| Embodiment 3 | 0.69 |
| Embodiment 4 | 0.69 |
| Embodiment 5 | 0.62 |
| Embodiment 6 | 0.53 |
| Embodiment 7 | 0.54 |
| Embodiment 8 | 0.72 |
| Comparative example 1 | 0.45 |
| Comparative example 2 | 0.66 |
Table 1
By the table as it can be seen that the comparative example 1 of cationic alkenyl monomer is not added, obtained gel crush resistance strength is opposite
Relatively low, addition cationic alkenyl monomer has the sealing characteristics of gel important influence in component.
Claims (13)
1. a kind of composition being used to prepare underground crosslinking plural gel plugging material, the composition includes cationic alkenyl list
Body, calcium carbonate, alginate, N, N '-methylene-bisacrylamides and organic acid, the organic acid are selected from acetic acid, propionic acid and just
It is one or more in butyric acid；The composition includes following components by weight：
100 parts of water；
10-20 parts of acrylamide；
2-10 parts of cationic alkenyl monomer；
N, N ' 0.005-0.1 parts of-methylene-bisacrylamide；
0.5-5 parts of alginate；
0.05-1 parts of calcium carbonate；And
0.1-2 parts of organic acid.
2. composition according to claim 1, which is characterized in that the composition includes following components by weight：
100 parts of water；
15-20 parts of acrylamide；
3-5 parts of cationic alkenyl monomer；
N, N ' 0.01-0.1 parts of-methylene-bisacrylamide；
4-5 parts of alginate；
0.25-1 parts of calcium carbonate；And
1-2 parts of organic acid.
3. composition according to claim 2, which is characterized in that the cationic alkenyl monomer is selected from acrylyl oxy-ethyl
One kind or more in trimethyl ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl ammonium chloride
Kind；The alginate is one or more in sodium alginate, potassium alginate and ammonium alginate；The calcium carbonate is ultra-fine
Calcium carbonate, average grain diameter are 300-800 mesh.
4. composition according to claim 2, which is characterized in that the cationic alkenyl monomer is acrylyl oxy-ethyl three
Ammonio methacrylate；The alginate is sodium alginate.
5. a kind of method preparing underground crosslinking plural gel, the described method comprises the following steps：
By acrylamide, cationic alkenyl monomer, N, N '-methylene-bisacrylamides are added to the water, stirring；Alginic acid is added
Salt, stirring；Calcium carbonate, stirring is added；Initiator and organic acid, stirring is added；Finally, mixed system is heated reaction and is formed and coagulated
Glue；Wherein, each component is calculated as by weight：
100 parts of water；
10-20 parts of acrylamide；
2-10 parts of cationic alkenyl monomer；
N, N ' 0.005-0.1 parts of-methylene-bisacrylamide；
0.5-5 parts of alginate；
0.05-1 parts of calcium carbonate；
0.05-1 parts of initiator；And
0.1-2 parts of organic acid.
6. according to the method described in claim 5, it is characterized in that, the described method comprises the following steps：
By acrylamide, cationic alkenyl monomer, N, N '-methylene-bisacrylamides are added to the water, stirring；Alginic acid is added
Salt, stirring；Calcium carbonate, stirring is added；Initiator and organic acid, stirring is added；Finally, mixed system is heated reaction and is formed and coagulated
Glue；Wherein, each component is calculated as by weight：
100 parts of water；
15-20 parts of acrylamide；
3-5 parts of cationic alkenyl monomer；
N, N ' 0.01-0.1 parts of-methylene-bisacrylamide；
4-5 parts of alginate；
0.25-1 parts of calcium carbonate；
0.5-1 parts of initiator；And
1-2 parts of organic acid.
7. according to the method described in claim 5, it is characterized in that, the cationic alkenyl monomer is selected from acrylyl oxy-ethyl three
It is one or more in ammonio methacrylate, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl ammonium chloride；
The alginate is one or more in sodium alginate, potassium alginate and ammonium alginate；The initiator is selected from over cure
It is one or more in sour ammonium, potassium peroxydisulfate, sodium peroxydisulfate；The calcium carbonate is calcium carbonate superfine powder, average grain diameter 300-
800 mesh.
8. according to the method described in claim 5, it is characterized in that, the cationic alkenyl monomer is acrylyl oxy-ethyl front three
Ammonium chloride；The alginate is sodium alginate；The initiator is ammonium persulfate；The calcium carbonate is calcium carbonate superfine powder,
Its average grain diameter is 300-800 mesh.
9. according to the method described in claim 5, it is characterized in that, the organic acid is in acetic acid, propionic acid and n-butyric acie
It is one or more.
10. according to the method described in any one of claim 5-9, which is characterized in that the temperature of the heating reaction is 50 °
C-90 °C, and the reaction time for heating reaction is 1-5 hours.
11. according to the method described in claim 10, it is characterized in that, it is described heating reaction temperature be 50 °C -60 °C, and add
The reaction time of thermal response is 2-3 hours.
12. underground prepared by the method according to any one of claim 5-11 is crosslinked plural gel.
13. application of the crosslinking plural gel in underground according to claim 12 as plugging material in drilling leakage blockage field.
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| US10144859B1 (en) | 2017-07-20 | 2018-12-04 | Saudi Arabian Oil Company | Loss circulation compositions (LCM) having Portland cement clinker |
| CN110358513B (en) * | 2018-03-26 | 2021-07-30 | 中国石油化工股份有限公司 | Bridging leak stoppage slurry and preparation method thereof |
| US10619090B1 (en) | 2019-04-15 | 2020-04-14 | Saudi Arabian Oil Company | Fracturing fluid compositions having Portland cement clinker and methods of use |
| CN110229266B (en) * | 2019-04-19 | 2021-12-14 | 中国石油化工股份有限公司 | Preparation method of crosslinked polymer, modified calcium carbonate particles and plugging agent |
| CN110105933B (en) * | 2019-05-15 | 2020-05-05 | 中国石油大学(华东) | High-temperature-resistant core/shell structure gel particle plugging agent and preparation method and application thereof |
| CN111732941B (en) * | 2020-07-15 | 2023-04-07 | 北京石大博诚科技有限公司 | Supermolecular gel leakage-stopping slurry and preparation method thereof |
| CN112920327B (en) * | 2021-01-28 | 2022-05-17 | 中国石油大学(北京) | Temporary plugging agent, preparation method thereof and application thereof in oilfield exploitation |
| CN115926073B (en) * | 2022-12-02 | 2024-07-02 | 西南石油大学 | Nanometer calcium carbonate modified acrylamide amphoteric copolymer and preparation method thereof |
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| CN103374854A (en) * | 2012-04-23 | 2013-10-30 | 李汝基 | Specific papermaking filling and paper containing same |
| CN103396562A (en) * | 2013-07-09 | 2013-11-20 | 西安交通大学 | Preparation method for sodium alginate-acrylamide-based hydrogel |
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