CN106317321A - Composition used for preparing downhole cross-linked complex gel and cross-linked complex gel prepared thereby - Google Patents
Composition used for preparing downhole cross-linked complex gel and cross-linked complex gel prepared thereby Download PDFInfo
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Abstract
The invention relates to a composition used for preparing a downhole cross-linked complex gel leakage-preventing material. The composition comprises a cationic alkenyl monomer, calcium carbonate and an organic acid. The invention also relates to a method for preparing the complex gel leakage-preventing material, and application thereof in the field of oil well leakage prevention.
Description
Technical field
The present invention relates to technical field of oilfield chemistry, be specifically related to a kind of down-hole crosslinking pluralgel loss circulation material and
Its preparation method.
Background technology
Leakage always perplexs the major engineering problems of domestic and international petroleum exploration and development, the most pernicious leakage
Losing, serious threat, to drilling safety, greatly hinders wellbore construction to proceed.Generally for severe well leakage, relatively
It is to use cement class chemical consolidation slurry to carry out leak stopping for ripe method.But, cement mortar is originally in leakage channel
Middle anelasticity is poor, often flows into drop ply depths and causes leak stopping failure.And, if drop ply is aqueous or and subsoil water
Layer connection, cement mortar mixes with stratum aqueous phase, is more difficult to be detained, and is difficult to condensation cure, or setting strength fall
Low, cause leak stopping failure.Therefore, process severe mud losses it is critical only that guarantee sealing agent can be trapped in leakage
In passage, and to avoid being rushed by formation water dilute.Common bridge joint loss circulation material, high dehydration loss circulation material, nothing
Machine gelling sealing agent, soft or hard plug loss circulation material etc. are not enough to successfully manage.
Under above-mentioned background, gel is subject to people's attention as a kind of novel loss circulation material.Gel is one
Class semisolid viscoelastic body, is cross-linked to form three-dimensional net structure by water soluble polymer and absorbs a certain amount of water, tool
Having stable boundary, water phase and an oil phase is the most difficult mixed, and anti-dilution capacity is strong；There is deformability, can be wide
The pore throat of general adaptation different sizes and shapes or gap, be filled in formation pore, play formation fluid preferably
Packing effect；Having preferable adhesiveness with surface of stratum, flow resistance is big, and retention effect is good.Based on the most excellent
Point, gel application in terms of leak stopping has vast potential for future development.The gel of synthetic is most commonly that
The polyacrylamide gel of chemical crosslinking.Plain polypropylene acrylamide gel mechanical property is the most weak, anti-pressure ability difference and
Frangible, it is difficult to meet leak stopping demand.Improve gel bulk strength, contribute to strengthening the anti-pressure differential energy of gel
Power, it is possible to the strengthening gel obstruct to formation fluid and the closure to drop ply.
Document [Nature, 489,133-136] is prepared for a kind of calcium alginate-polyacrylamide and synchronizes IPN net
Network high intensity hydrogel.In composite network structure, polyacrylamide network passes through acrylamide monomer, cross-linking agent
N, N '-dimethylene bisacrylamide copolymerization formation；Calcium alginate network by sodium alginate aqueous solution with
CaSO4·2H2The calcium ion crosslinking of O release is formed.But, if this gel rubber system is applied at blocking construction
In, there are some problems: gelation time is short, it is difficult to enter purpose stratum and form gel；Formation gel time is difficult
With regulation.Patent CN103396562A describes one and prepares sodium alginate-polyacrylamide by two-step method
The method of hydrogel, the gel strength obtained is high, but, primary gel is first made due to two-step method, then will be solidifying
Glue is immersed in solution and continues to react into end product, thus it does not possess operability (just in drilling leakage blockage
Level gel cannot pump into stratum), it is not suitable for blocking construction.
Summary of the invention
It is an object of the invention to provide a kind of compositions preparing down-hole crosslinking pluralgel loss circulation material and answer
The method preparing pluralgel by said composition, uses compositions and the method for the present invention, improves gel body strong
Degree, strengthens the resistance to compression difference driving force of gel, the strengthening gel obstruct to formation fluid and the closure to drop ply.
In drilling leakage blockage field, plugging operation liquid is by carrying to drop ply inside drilling tool, and too fast formation gel holds
Easily cause the obstruction of drilling tool.The present invention prepare pluralgel compositions use calcium carbonate as calcium ion source, and
Control the release of calcium ion by using organic acid to react, serve the effect of " slow release ", it is possible to right
The time of plastic is controlled, and is particularly suited for drilling leakage blockage field.
One aspect of the present invention relates to a kind of compositions for preparing down-hole crosslinking pluralgel loss circulation material,
Described compositions includes cationic alkenyl monomer, calcium carbonate and organic acid.
In a preferred embodiment of the present invention, described compositions includes by weight:
In a preferred embodiment of the present invention, described component includes by weight, described acrylamide
15-20 part, preferably 16-18 part；Described cationic alkenyl monomer 2-8 part, more preferably 3-5 part；Described N, N '
-methylene-bisacrylamide 0.01-0.1 part；Described alginate 4-5 part；Described calcium carbonate 0.25-1 part is excellent
Select 0.5-1 part；Described initiator 0.5-1 part；Described organic acid 1-2 part.
In a preferred embodiment of the present invention, described cationic alkenyl monomer is selected from acrylyl oxy-ethyl three
One in ammonio methacrylate, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl ammonium chloride
Or multiple, preferably acrylyl oxy-ethyl-trimethyl salmiac；Described alginate is selected from sodium alginate, alginic acid
One or more in potassium and ammonium alginate, preferably sodium alginate；Described initiator is selected from Ammonium persulfate., over cure
One or more in acid potassium, sodium peroxydisulfate, initiator system of ammonium persulfate；Described calcium carbonate is calcium carbonate superfine powder, its
Mean diameter is 300-800 mesh.
In a preferred embodiment of the present invention, described organic acid is in acetic acid, propanoic acid and n-butyric acie
One or more.
Another aspect of the present invention relates to a kind of method preparing down-hole crosslinking pluralgel, and described method includes
Following steps:
Acrylamide, cationic alkenyl monomer, N, N '-methylene-bisacrylamide are added to the water, stirring；
Add alginate, stirring；Add calcium carbonate, stirring；Add initiator and organic acid, stirring；Finally,
Mixed system reacting by heating is formed gel；Wherein, the stirring in the above step, all stir to mixture
System fully dissolves, dispersion；Further, wherein, each component is calculated as by weight:
In a preferred embodiment of the present invention, described cationic alkenyl monomer is selected from acrylyl oxy-ethyl three
One in ammonio methacrylate, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl ammonium chloride
Or multiple, preferably acrylyl oxy-ethyl-trimethyl salmiac；Described alginate is selected from sodium alginate, alginic acid
One or more in potassium and ammonium alginate, preferably sodium alginate；Described initiator is selected from Ammonium persulfate., over cure
One or more in acid potassium, sodium peroxydisulfate, initiator system of ammonium persulfate；Described organic acid selected from acetic acid, propanoic acid and
One or more in n-butyric acie；Described calcium carbonate is calcium carbonate superfine powder, and its mean diameter is 300-800 mesh.
In a preferred embodiment of the present invention, described organic acid is in acetic acid, propanoic acid and n-butyric acie
One or more.
In a preferred embodiment of the present invention, the reaction temperature of reacting by heating is 50 DEG C-90 DEG C, preferably
50℃-60℃。
In a preferred embodiment of the present invention, response time of reacting by heating be 1-5 hour, preferably
2-3 hour.The gel of the present invention needs for drilling leakage blockage, therefore, is heated to overlong time or the mistake of plastic
Short all unfavorable to reality application, for majority of case, the time that will warm up plastic controls at 2-3 little
It is preferred time within.
Another aspect of the present invention relates to the down-hole crosslinking pluralgel prepared by described method.
Another aspect of the present invention relates to the application in oil well leak stopping field of the described pluralgel loss circulation material.
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, strong electrostatic can be produced with electronegative surface of stratum
Adsorption, strengthens the adhesion of gel and stratum, improves gel plugging strength；The preparation method of the present invention is protected
Demonstrate,prove system and there is the feature of delayed cross-linking, leakage channel reaction can have been entered and form gel slug, when forming gel
Between can regulate, be favorably improved leak stopping success rate.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further detailed, it should be noted that following example
It is not intended to limit the present invention.
Embodiment 1
By 16g acrylamide, 4g acrylyl oxy-ethyl-trimethyl salmiac, 0.01g N, N '-di-2-ethylhexylphosphine oxide third
Acrylamide adds in 100g water, and stirring is fully dissolved, and adds 2g sodium alginate, and stirring is fully dissolved, and adds
0.25g calcium carbonate superfine powder, stirs fully dispersed, adds 0.2g Ammonium persulfate. and 0.4g acetic acid, stirs the most molten
Solve, finally, mixed system is placed at 70 DEG C reaction, after 2 hours, form gel.The gel compression obtained is strong
Degree (70% strain) is 1.2Mpa.
Embodiment 2
By 10g acrylamide, 10g acrylyl oxy-ethyl-trimethyl salmiac, 0.05g N, N '-di-2-ethylhexylphosphine oxide third
Acrylamide adds in 100g water, and stirring is fully dissolved, and adds 1g sodium alginate, and stirring is fully dissolved, and adds
1g calcium carbonate superfine powder, stirs fully dispersed, adds 1g Ammonium persulfate. and 1.5g acetic acid, and stirring is fully dissolved,
Finally, mixed system is placed at 90 DEG C reaction, after 1 hour, forms gel.The gel compressive strength (70% obtained
Strain) it is 0.8Mpa.
Embodiment 3
By 15g acrylamide, 5g acrylyl oxy-ethyl-trimethyl salmiac, 0.1g N, N '-methylene bisacrylamide
Amide is added to the water, and stirring is fully dissolved, and adds 3g sodium alginate, and stirring is fully dissolved, and adds 0.5g and surpasses
Thin calcium carbonate, stirs fully dispersed, adds 0.5g Ammonium persulfate. and 1g propanoic acid, and stirring is fully dissolved, finally,
Mixed system is placed at 60 DEG C reaction, after 3 hours, forms gel.(70% should for the gel compressive strength obtained
Become) into 1.5Mpa.
Embodiment 4
By 10g acrylamide, 5g acrylyl oxy-ethyl-trimethyl salmiac, 0.005g N, N '-di-2-ethylhexylphosphine oxide third
Acrylamide is added to the water, and stirring is fully dissolved, and adds 0.5g sodium alginate, and stirring is fully dissolved, and adds 0.1g
Calcium carbonate superfine powder, stirs fully dispersed, adds 0.05g Ammonium persulfate. and 0.2g propanoic acid, and stirring is fully dissolved,
Finally, mixed system is placed at 70 DEG C reaction, after 5 hours, forms gel.The gel compressive strength (70% obtained
Strain) it is 0.9Mpa.
Embodiment 5
By 18g acrylamide, 2g acrylyl oxy-ethyl-trimethyl salmiac, 0.05g N, N '-di-2-ethylhexylphosphine oxide third
Acrylamide is added to the water, and stirring is fully dissolved, and adds 4g sodium alginate, and stirring is fully dissolved, and adds 0.5g
Calcium carbonate superfine powder, stirs fully dispersed, adds 0.5g Ammonium persulfate. and 1g n-butyric acie, and stirring is fully dissolved,
Finally, mixed system is placed at 50 DEG C reaction, after 3 hours, forms gel.The gel compressive strength (70% obtained
Strain) it is 1.6Mpa.
Embodiment 6
By 10g acrylamide, 2g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 0.005g N, N '-methylene
Bisacrylamide adds in 100g water, and stirring is fully dissolved, and adds 0.5g potassium alginate, and stirring is fully dissolved,
Add 0.05g calcium carbonate superfine powder, stir fully dispersed, add 0.05g potassium peroxydisulfate and 0.1g acetic acid, stirring
Fully dissolve, finally, mixed system is placed at 90 DEG C reaction, after 5 hours, form gel.The gel obtained
Compressive strength (70% strain) is 1.1Mpa.
Embodiment 7
By 20g acrylamide, 10g dimethyl diallyl ammonium chloride, 0.1g N, N '-methylene bisacrylamide acyl
Amine adds in 100g water, and stirring is fully dissolved, and adds 5g ammonium alginate, and stirring is fully dissolved, and adds 1g
Calcium carbonate superfine powder, stirs fully dispersed, adds 1g sodium peroxydisulfate and 2g acetic acid, and stirring is fully dissolved, finally,
Mixed system is placed at 50 DEG C reaction, after 1 hour, forms gel.(70% should for the gel compressive strength obtained
Become) into 1.2Mpa.
Embodiment 8
By 17g acrylamide, 4g acrylyl oxy-ethyl-trimethyl salmiac, 0.2g N, N '-methylene bisacrylamide
Amide adds in 100g water, and stirring is fully dissolved, and adds 4g ammonium alginate, and stirring is fully dissolved, and adds 0.5g
Calcium carbonate superfine powder, stirs fully dispersed, adds 1g Ammonium persulfate. and 1g acetic acid, and stirring is fully dissolved, finally,
Mixed system is placed at 55 DEG C reaction, after 2 hours, forms gel.(70% should for the gel compressive strength obtained
Become) into 1.8Mpa.
Comparative example 1
By 17g acrylamide, 0.2g N, N '-methylene-bisacrylamide adds in 100g water, stirs the most molten
Solving, add 4g ammonium alginate, stirring is fully dissolved, and adds 0.5g calcium carbonate superfine powder, stirs fully dispersed,
Adding 1g Ammonium persulfate. and 1.5g acetic acid, stirring is fully dissolved, and finally, is placed in by mixed system at 55 DEG C anti-
Should, form gel after 1 hour.The gel compressive strength (70% strain) obtained is 1.0Mpa.
Comparative example 2
By 17g acrylamide, 4g acrylyl oxy-ethyl-trimethyl salmiac, 0.2g N, N '-methylene bisacrylamide
Amide adds in 100g water, and stirring is fully dissolved, and adds 4g ammonium alginate, and stirring is fully dissolved, and adds 0.5g
Calcium sulfate, stirs fully dispersed, adds 1g Ammonium persulfate., and stirring is fully dissolved, finally, by mixed system
It is placed at 55 DEG C reaction, after 30 minutes, forms gel.The gel compressive strength (70% strain) obtained is 0.5Mpa.
Plugging strength is tested
After fully being absorbed water by the gel prepared by the method for above example, it is placed in the crannied round metal in bottom
In logical container.Use nitrogen to the piston pressurization of container to promote gel descending, to its be extruded from crack time,
The nitrogen pressure that record is now used, and it is defined as crush resistance strength.Result of the test 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
From this table, not adding the comparative example 1 of cationic alkenyl monomer, its obtained gel is anti-extrusion by force
Spending relatively low, adding cationic alkenyl monomer in component has important impact to the sealing characteristics of gel.
Claims (10)
1. for prepare down-hole crosslinking pluralgel loss circulation material a compositions, described compositions include sun from
Sub-alkenyl monomer, calcium carbonate and organic acid.
Compositions the most according to claim 1, it is characterised in that described compositions include by weight with
Lower component:
Compositions the most according to claim 2, it is characterised in that described cationic alkenyl monomer is selected from third
Alkene acyloxyethyl trimethyl ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl chlorine
Change one or more in ammonium, preferably acrylyl oxy-ethyl-trimethyl salmiac；Described alginate is selected from Sargassum
One or more in acid sodium, potassium alginate and ammonium alginate, preferably sodium alginate；Described calcium carbonate is ultra-fine
Calcium carbonate, its mean diameter is 300-800 mesh.
4. according to the compositions described in any one in claim 1-3, it is characterised in that described organic acid is selected from
One or more in acetic acid, propanoic acid and n-butyric acie.
5. the method preparing down-hole crosslinking pluralgel, said method comprising the steps of:
Acrylamide, cationic alkenyl monomer, N, N '-methylene-bisacrylamide are added to the water, stirring；
Add alginate, stirring；Add calcium carbonate, stirring；Add initiator and organic acid, stirring；Finally,
Mixed system reacting by heating is formed gel；Wherein, each component is calculated as by weight:
Method the most according to claim 5, it is characterised in that described cationic alkenyl monomer is selected from propylene
Acyloxyethyl trimethyl ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and dimethyl diallyl chlorination
One or more in ammonium, preferably acrylyl oxy-ethyl-trimethyl salmiac；Described alginate is selected from alginic acid
One or more in sodium, potassium alginate and ammonium alginate, preferably sodium alginate；Described initiator is selected from over cure
One or more in acid ammonium, potassium peroxydisulfate, sodium peroxydisulfate, initiator system of ammonium persulfate；Described calcium carbonate is ultra-fine
Calcium carbonate, its mean diameter is 300-800 mesh.
7. according to the method described in claim 5 or 6, it is characterised in that described organic acid selected from acetic acid, third
One or more in acid and n-butyric acie.
8. according to the method described in any one in claim 5-7, it is characterised in that described reacting by heating
Temperature is 50 DEG C-90 DEG C, preferably 50 DEG C-60 DEG C, and the response time of reacting by heating is 1-5 hour, preferably
2-3 hour.
9. the down-hole crosslinking pluralgel prepared according to the method described in any one in claim 5-8.
Down-hole the most according to claim 9 cross-links pluralgel as loss circulation material in drilling leakage blockage field
Application.
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| CN110105933A (en) * | 2019-05-15 | 2019-08-09 | 中国石油大学(华东) | Gel particle sealing agent and its preparation method and application |
| CN110229266A (en) * | 2019-04-19 | 2019-09-13 | 中国石油化工股份有限公司 | A kind of preparation method of cross-linked polymer, modified calcium carbonate particle and sealing agent |
| CN110358513A (en) * | 2018-03-26 | 2019-10-22 | 中国石油化工股份有限公司 | A kind of bridge joint leak stopping slurry and preparation method thereof |
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| CN115926073A (en) * | 2022-12-02 | 2023-04-07 | 西南石油大学 | Nano calcium carbonate modified acrylamide amphoteric copolymer and preparation method thereof |
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