CN110229266A - A kind of preparation method of cross-linked polymer, modified calcium carbonate particle and sealing agent - Google Patents
A kind of preparation method of cross-linked polymer, modified calcium carbonate particle and sealing agent Download PDFInfo
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- CN110229266A CN110229266A CN201910317917.7A CN201910317917A CN110229266A CN 110229266 A CN110229266 A CN 110229266A CN 201910317917 A CN201910317917 A CN 201910317917A CN 110229266 A CN110229266 A CN 110229266A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- 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
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/08—Fiber-containing well treatment fluids
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Abstract
The present invention provides a kind of preparation method of cross-linked polymer, modified calcium carbonate particle and sealing agents.The preparation method of cross-linked polymer comprising following steps: 1) mixing acrylic acid, 2- acrylamide-2-methyl propane sulfonic and water, adjusts pH value, obtains the first mixed liquor；2) crosslinking agent is added in the first mixed liquor of Xiang Suoshu, after heating, initiator is added, stirring obtains the cross-linked polymer.Modified calcium carbonate particle includes shell and core material, wherein shell is the cross-linked polymer that method produced above obtains, and core material is calcium carbonate granule.Host agent in sealing agent of the invention is modified calcium carbonate, and reduce original calcium carbonate granule answers brittleness, to improve bearing capacity.The modified calcium carbonate particle of different-grain diameter is subjected to Size Matching, is aided with other plugging materials and sealing agent is made, so that it is strong so that acid-soluble ratio is up to 75%, temperature resistance ability.(2) sealing agent use of the invention is more convenient.
Description
Technical field
The present invention provides a kind of preparation methods of cross-linked polymer and the cross-linked polymer as made from this method to change
The calcium carbonate granule of property, more particularly to a kind of sealing agent containing the modified calcium carbonate particle.
Background technique
For cap rock, reservoir porosity and permeability with higher.The quality of porosity directly determines rock stratum
The quantity of oil gas is stored, infiltrative quality then controls the production capacity of contained oil gas in reservoir.Reservoir pore space is both to preserve sky
Between be important percolating channels again, during exploration and development, for reservoir since cementing properties is relatively poor, hole is abundant, easily sends out
Raw leakage, the solid phase in drilling fluid enter oil-gas Layer and pore throat are caused to block, liquid phase enter oil-gas Layer and oil-gas Layer rock and
Fluid matasomatism destroys the original balance of oil-gas Layer to induce oil-gas Layer potential damage factors and causes permeability decrease, thus
Influence reservoir yield.Carbonate reservoir is important reservoir of oil and gas, and the oil and gas reserves in carbonate reservoir accounts for generation
The half or so of boundary's oil gas gross reserves, yield has reached 60% of total output or more.Fracture reservoir is that carbonate rock preserves
The main Storage category of layer, while it being also important leakage channel, the sealing agent for the stratum not only wants shut-off capacity strong, also
Focus on that reservoir cannot be polluted.Therefore the carbonate reservoir fractured leakage of research " firmly stifled " and " opening for solution "
Sealing agent has important practical significance.
Reservoir sealing agent huge number at present, but acid soluble leak stopping agent can be acidified in the carbonate formation later period and press
De-plugging during splitting, simple process, therefore be more suitable for carbonate formation leak stopping, the molten sealing agent of existing acid or formula make mostly
Use calcium carbonate granule as bridging materials, and calcium carbonate granule bearing capacity is low, causes the matched whole bearing capacity of leak stopping slurry low,
Plugging effect is influenced, and most of molten sealing agents of acid cannot be used separately as plugging formula, the plugging formula acid after compounding is molten
For rate substantially 50% or so, de-plugging rate is not high, therefore needs to research and develop the sealing agent that bearing capacity is strong, acid-soluble ratio is high.
Summary of the invention
One of present invention provides a kind of preparation method of cross-linked polymer comprising following steps:
1) acrylic acid, 2- acrylamide-2-methyl propane sulfonic and water are mixed, adjusts pH value, obtains the first mixed liquor；
2) crosslinking agent is added in the first mixed liquor of Xiang Suoshu, after heating, the first initiator and the second initiator is added, stirs
It mixes, obtains the cross-linked polymer.
In a specific embodiment, in terms of mass parts, 30 to 45 parts of the acrylic acid, the 2- acrylamide -2-
10 to 15 parts of methyl propane sulfonic acid, 100 to 120 parts of the water, 0.05 to 0.1 part of the crosslinking agent, first initiator 0.15
To 0.2 part, described 0.15 to 0.2 part of second initiator.
In a specific embodiment, in step 1), the pH value is 6.8 to 7.2, such as pH value is 7.
In a specific embodiment, in step 2), the temperature after heating is 50 to 60 DEG C.
In a specific embodiment, in step 2), the time of stirring is 20 minutes to 30 minutes.
In a specific embodiment, the crosslinking agent is N, N '-methylene-bisacrylamide.
In a specific embodiment, first initiator is potassium peroxydisulfate, and second initiator is sulfurous acid
Hydrogen sodium.
The two of the present invention provide a kind of modified calcium carbonate particle, and the modified calcium carbonate particle includes shell and core material,
Wherein, the shell is the cross-linked polymer that the preparation method as described in any one of one of present invention obtains, described
Core material is calcium carbonate granule.
In a specific embodiment, the partial size of the calcium carbonate granule is 0.8 to 5mm, using it as the modification of core material
The partial size of calcium carbonate granule is 0.8 to 5mm.
In a specific embodiment, the partial size of the calcium carbonate granule is 0.8 to 1mm, using it as the modification of core material
The partial size of calcium carbonate granule is 0.8 to 1mm.
In a specific embodiment, the partial size of the calcium carbonate granule is 3 to 5mm, using it as the carbon modified of core material
The partial size of sour calcium particle is 3 to 5mm.
In a specific embodiment, the partial size of the calcium carbonate granule is 3.35 to 4.75mm, using it as core material
The partial size of modified calcium carbonate particle is 3.35 to 4.75mm.
The three of the present invention provide a kind of sealing agent comprising modified calcium carbonate particle as described in the two of the present invention is filled out
Fill particle and fiber.
In a specific embodiment, the modified calcium carbonate particle includes that the first modified calcium carbonate particle and second changes
Property calcium carbonate granule, wherein the partial size of the first modified calcium carbonate particle be 3 to 5mm, the second modified calcium carbonate particle
Partial size be 0.8 to 1mm.
In a specific embodiment, the partial size of the first modified calcium carbonate particle is 3.35 to 4.75mm.
It in a specific embodiment, is first modified calcium carbonate in terms of 100% by the quality of the sealing agent
The dosage of grain and the second modified calcium carbonate particle independently is 23% to 25%.
In a specific embodiment, the calcium carbonate powder that the filler particles are 58 to 75 μm, with the sealing agent
Quality be 100% meter, dosage be 35% to 38%.
In a specific embodiment, the fiber is the polyester fiber and sepiolite matter that breaking strength is greater than 4 lis of oxen
The sepiolite fibre that content is greater than 60% is measured, wherein being in terms of 100% by the quality of the sealing agent, the amount of the polyester fiber is
0.2% to 0.3%, the dosage of the sepiolite fibre is 11.7% to 18.8%.
In a specific embodiment, the length of the polyester fiber is 8-12mm (such as 10nm).
In a specific embodiment, range of the breaking strength of the fiber in 10 lis of wild marjorams, 35 lis of oxen.
In a specific embodiment, model of the sepiolite mass content in the sepiolite fibre 60% to 66%
It encloses.
Beneficial effects of the present invention:
Carbonate reservoir slit formation leakage sealing agent of the invention has the advantage that compared to existing reservoir sealing agent
(1) host agent in sealing agent of the invention is modified calcium carbonate, by reducing in sodium carbonate surface polymer attached
Original calcium carbonate granule answers brittleness, to improve bearing capacity, thus its leakage for being more suitable for solving low pressure reservoir
Problem.The modified calcium carbonate particle of different-grain diameter is subjected to Size Matching, is aided with other plugging materials, sealing agent is made, thus
So that acid-soluble ratio is up to 75%, temperature resistance ability strong, can be used directly to block the crack 5-8mm.
(2) two kinds of fibers of polyester fiber and sepiolite fibre are used simultaneously；Polyester fiber intensity is high, and can wrap big
Particle and other materials can improve the compactness of plugged zone to enhance the shut-off capacity of plugging material；Sepiolite fibre can
It is dispersed in soil paste and forms fibrous reticular structure, improve suspension of the plugging material in soil paste, keep Size Matching uniform,
Improve shut-off capacity.
(3) sealing agent use of the invention is more convenient, and without carrying out Size Matching, drilling fluid can be directly added into when with slurry
In, or prepared with 5% bentonite slurry.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but the exemplary only explanation of the embodiment of the present invention, should
No matter embodiment does not constitute a limitation of the invention under any circumstance.
Unless otherwise instructed, material used in the following embodiment is commercially available.
Embodiment 1
The preparation of cross-linked polymer, modified calcium carbonate particle and sealing agent
The preparation of cross-linked polymer: 30 parts of acrylic acid, 10 parts of 2- acrylamide-2-methyl propane sulfonics are accurately weighed in 100
In part distilled water, it is 7 that 20% sodium hydroxide solution is added while stirring and is adjusted to pH value, and 0.05 part of N, N '-di-2-ethylhexylphosphine oxide third is added
Acrylamide is warming up to 50 DEG C, and 0.15 part of potassium peroxydisulfate and 0.15 part of sodium hydrogensulfite is added, and continues stirring after twenty minutes, pours into
To get cross-linked polymer 1# in pallet.
The preparation of first modified calcium carbonate particle: with the standard screen of 3.35mm and 4.75mm, 3.35 are sifted out to 4.75mm's
It is dipped in the cross-linked polymer 1# in pallet by calcium carbonate granule 1-1A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
It is uniformly wrapped up, after standing 1 minute, is pulled out with the sieve of 0.60mm, taking-up nature cools after 2h is toasted in 105 DEG C of baking oven
To room temperature to get 3.35 to 4.75mm modified calcium carbonate particle 1-1B#.
The preparation of second modified calcium carbonate particle: with the standard screen of 0.83mm and 1.00mm, 0.83 is sifted out to 1.00mm's
It is dipped in the cross-linked polymer 1# in pallet by calcium carbonate granule 1-2A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
Uniformly wrapped up, stand 1 minute after, pulled out with 0.60mm sieve, in 105 DEG C of baking oven toast 2h after take out nature cool to
Room temperature to get 0.83 to 1.00mm modified calcium carbonate particle 1-2B#.
The preparation of sealing agent: to be modified carbonic acid for the first of 23wt% at mixture as following formula to obtain the final product 1#:25 DEG C of sealing agent
Second modified calcium carbonate particle 1-2B#, 38wt%58 to 75 μm of the calcium carbonate granule of calcium particle 1-1B#, 23wt% are in mixing
It is stirred until homogeneous in machine, is slow added into the polyester fiber and 15.7wt% that 0.3wt% length is 12 lis of 8mm, breaking strength oxen
Sepiolite fibre (sepiolite mass content is 65%), is stirred until homogeneous.
Embodiment 2
The preparation of cross-linked polymer, modified calcium carbonate particle and sealing agent
The preparation of cross-linked polymer: 40 parts of reaction acrylic acid, 15 parts of reaction 2- acrylamide -2- methyl-prop sulphurs are accurately weighed
For acid in 110 parts of distilled water, it is that be adjusted to pH value be 7 to 20% sodium hydroxide solution that concentration is added while stirring, and 0.08 part of N is added,
N '-methylene-bisacrylamide is warming up to 55 DEG C, and 0.2 part of potassium peroxydisulfate and 0.2 part of sodium hydrogensulfite is added, continues stirring 25
After minute, pour into pallet to get cross-linked polymer 2#.
The preparation of first modified calcium carbonate particle: with the standard screen of 3.35mm and 4.75mm, 3.35 are sifted out to 4.75mm's
It is dipped in the cross-linked polymer 2# in pallet by calcium carbonate granule 2-1A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
It is uniformly wrapped up, after standing 1 minute, is pulled out with the sieve of 0.60mm, taking-up nature cools after 2h is toasted in 105 DEG C of baking oven
To room temperature to get the modified calcium carbonate particle 2-1B# of 3.35-4.75mm.
The preparation of second modified calcium carbonate particle: with the standard screen of 0.83mm and 1.00mm, 0.83 is sifted out to 1.00mm's
It is dipped in the cross-linked polymer 2# in pallet by calcium carbonate granule 2-2A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
Uniformly wrapped up, stand 1 minute after, pulled out with 0.60mm sieve, in 105 DEG C of baking oven toast 2h after take out nature cool to
Room temperature to get 0.83-1.00mm modified calcium carbonate particle 2-2B#.
The preparation of sealing agent: with mixture as following formula up at 2#:20 DEG C of sealing agent by the first modified calcium carbonate of 24wt%
Second modified calcium carbonate particle 2-2B#, 36wt%58 to 75 μm of the calcium carbonate granule of particle 2-1B#, 25wt% are in batch mixer
In be stirred until homogeneous, be slow added into 0.2wt% length be 10mm, the polyester fiber of 10 lis of oxen of breaking strength and 14.8wt% sea
Afrodite fiber (sepiolite mass content is 60%), is stirred until homogeneous.
Embodiment 3
The preparation of cross-linked polymer, modified calcium carbonate particle and sealing agent
The preparation of cross-linked polymer: 45 parts of reaction acrylic acid, 15 parts of reaction 2- acrylamide -2- methyl-prop sulphurs are accurately weighed
For acid in 120 parts of distilled water, it is 7.2 that 20% sodium hydroxide solution is added while stirring and is adjusted to pH value, 0.1 part of N is added, N '-is sub-
Bisacrylamide is warming up to 60 DEG C, and 0.2 part of potassium peroxydisulfate and 0.15 part of sodium hydrogensulfite is added, and continues stirring 30 minutes,
Up to cross-linked polymer 3#.
The preparation of first modified calcium carbonate particle: with the standard screen of 3.35mm and 4.75mm, 3.35 are sifted out to 4.75mm's
It is dipped in the cross-linked polymer 3# in pallet by calcium carbonate granule 3-1A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
It is uniformly wrapped up, after standing 1 minute, is pulled out with the sieve of 0.60mm, taking-up nature cools after 2h is toasted in 105 DEG C of baking oven
To room temperature to get 3.35 to 4.75mm modified calcium carbonate particle 3-1B#.
The preparation of second modified calcium carbonate particle: with the standard screen of 0.83mm and 1.00mm, 0.83 is sifted out to 1.00mm's
It is dipped in the cross-linked polymer 3# in pallet by calcium carbonate granule 3-2A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
Uniformly wrapped up, stand 1 minute after, pulled out with 0.60mm sieve, in 105 DEG C of baking oven toast 2h after take out nature cool to
Room temperature to get 0.83 to 1.00mm modified calcium carbonate particle 3-2B#.
The preparation of sealing agent: to be modified carbonic acid for the first of 23wt% at mixture as following formula to obtain the final product 3#:30 DEG C of sealing agent
Second modified calcium carbonate particle 3-2B#, 38wt%58 to 75 μm calcium carbonate granule of calcium particle 3-1B#, 25wt% are in batch mixer
In be stirred until homogeneous, be slow added into the polyester fiber and 13.8wt% that 0.2wt% length is 12mm, breaking strength is 29 lis of oxen
Sepiolite fibre (sepiolite mass content is 62.5%), is stirred until homogeneous.
Embodiment 4
The preparation of cross-linked polymer, modified calcium carbonate particle and sealing agent
The preparation of cross-linked polymer: 38 parts of reaction acrylic acid, 12 parts of reaction 2- acrylamide -2- methyl-prop sulphurs are accurately weighed
For acid in 120 parts of distilled water, it is 7 that 20% sodium hydroxide solution is added while stirring and is adjusted to pH value, and 0.1 part of N, N '-methylene is added
Base bisacrylamide is warming up to 58 DEG C, and 0.2 part of potassium peroxydisulfate and 0.15 part of sodium hydrogensulfite is added, and continues stirring 30 minutes, i.e.,
Obtain cross-linked polymer 4#.
The preparation of first modified calcium carbonate particle: with the standard screen of 3.35mm and 4.75mm, 3.35 are sifted out to 4.75mm's
It is dipped in the cross-linked polymer 4# in pallet by calcium carbonate granule 4-1A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
It is uniformly wrapped up, after standing 1 minute, is pulled out with the sieve of 0.60mm, taking-up nature cools after 2h is toasted in 105 DEG C of baking oven
To room temperature to get 3.35 to 4.75mm modified calcium carbonate particle 4-1B#.
The preparation of second modified calcium carbonate particle: with the standard screen of 0.83mm and 1.00mm, 0.83 is sifted out to 1.00mm's
It is dipped in the cross-linked polymer 4# in pallet by calcium carbonate granule 4-2A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
Uniformly wrapped up, stand 1 minute after, pulled out with 0.60mm sieve, in 105 DEG C of baking oven toast 2h after take out nature cool to
Room temperature to get 0.83 to 1.00mm modified calcium carbonate particle 4-2B#.
The preparation of sealing agent: to be modified carbonic acid for the first of 23wt% at mixture as following formula to obtain the final product 4#:25 DEG C of sealing agent
Second modified calcium carbonate particle 4-2B#, 35wt%58 to 75 μm calcium carbonate granule of calcium particle 4-1B#, 23wt% are in batch mixer
In be stirred until homogeneous, be slow added into the polyester fiber and 18.8wt% that 0.2wt% length is 10mm, breaking strength is 35 lis of oxen
Sepiolite fibre (sepiolite mass content is 65%), is stirred until homogeneous.
Embodiment 5
The preparation of cross-linked polymer, modified calcium carbonate particle and sealing agent
The preparation of cross-linked polymer: 38 parts of reaction acrylic acid, 12 parts of reaction 2- acrylamide -2- methyl-prop sulphurs are accurately weighed
For acid in 120 parts of distilled water, it is 6.8 that 20% sodium hydroxide solution is added while stirring and is adjusted to pH value, 0.1 part of N is added, N '-is sub-
Bisacrylamide is warming up to 60 DEG C, and 0.2 part of potassium peroxydisulfate and 0.15 part of sodium hydrogensulfite is added, and continues stirring 28 minutes,
Up to cross-linked polymer 5#.
The preparation of first modified calcium carbonate particle: with the standard screen of 3.35mm and 4.75mm, 3.35 are sifted out to 4.75mm's
It is dipped in the cross-linked polymer 5# in pallet by calcium carbonate granule 5-1A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
It is uniformly wrapped up, after standing 1 minute, is pulled out with the sieve of 0.60mm, taking-up nature cools after 2h is toasted in 105 DEG C of baking oven
To room temperature to get 3.35 to 4.75mm modified calcium carbonate particle 5-1B#.
The preparation of second modified calcium carbonate particle: with the standard screen of 0.83mm and 1.00mm, 0.83 is sifted out to 1.00mm's
It is dipped in the cross-linked polymer 5# in pallet by calcium carbonate granule 5-2A# immediately, shakes pallet 5 minutes, makes calcium carbonate granule
Uniformly wrapped up, stand 1 minute after, pulled out with 0.60mm sieve, in 105 DEG C of baking oven toast 2h after take out nature cool to
Room temperature to get 0.83 to 1.00mm modified calcium carbonate particle 5-2B#.
The preparation of sealing agent: to be modified carbonic acid for the first of 25wt% at mixture as following formula to obtain the final product 5#:25 DEG C of sealing agent
Second modified calcium carbonate particle 5-2B#, 38wt%58 to 75 μm calcium carbonate granule of calcium particle 5-1B#, 25wt% are in batch mixer
In be stirred until homogeneous, be slow added into the polyester fiber and 11.7wt% that 0.3wt% length is 10mm, breaking strength is 35 lis of oxen
Sepiolite fibre (sepiolite mass content is 66%), is stirred until homogeneous.
Embodiment 6
The test of modified calcium carbonate particle bearing capacity
By 500g before modified after calcium carbonate granule 1-1A#, 2-1A#, 3-1A#, 1-1B#, 2-1B# and 3-1B# (quality meter
Make M1, unit: g) being added separately to after impregnating 16h in 2000mL water, take out, blot surface moisture, be put into pressure breaking machine,
5min is pushed in 3.5Mpa pressure, is taken out, (quality is counted as the particle among weighing 3.35mm standard screen and 4.75mm standard screen
Unit: M2 g), is calculated by formula 1 percentage of damage P, is indicated with percentage.Test result such as table 1.
The calculation method of percentage of damage P is as follows: P=(M1-M2)/M1*100% (formula 1)
The percentage of damage of 1: three group of modified calcium carbonate particle of table and before modified calcium carbonate granule is tested
It can be obtained by test result: this five groups of modified calcium carbonate particle lower than the percentage of damage of calcium carbonate granule before modified 20%
Left and right, it was demonstrated that modified calcium carbonate particle is stronger than bearing capacity before modified.
Embodiment 7
The test of sealing agent bearing capacity
Experimental method: the dynamic analog device that experiment instrument is Hubei Jing Zhou wound connection is blocked, in embodiment 1 to 5
Sealing agent 1#, 2#, 3#, 4# and 5# obtained are respectively adopted the wedge of the different size in table 2 such as and are tested, and test maximum is held
Pressure energy power.Specific value is shown in Table 2.
The bearing capacity test of 2 three groups of carbonate reservoir slit formation leakage sealing agents of table
Find out from experimental data, a kind of carbonate reservoir slit formation leakage sealing agent of the present invention can block 5-
The crack 8mm, bearing capacity are all larger than 10MPa, and bearing capacity is strong.
Embodiment 8
Acid-soluble test
Test method: sealing agent 1#, 2# and 3# obtained in 20g embodiment 1 to 5 are weighed respectively, is accurate to 0.1g (quality
It is counted as M3, unit: g), and be respectively placed in 1000mL beaker, little water is added to soak sample, 15% hydrochloric acid 200mL is added dropwise, to play
It after strong reaction stops, being stirred with glass bar, is placed in 60 DEG C of thermostat water bath constant temperature, the reaction was continued is extremely produced as without any bubble
Only, with filter paper, (quality is counted as M4, unit: g) filtering, distilled water cleaning beaker to noresidue, then wash with distilled water on filter paper
Residue, until filtrate is neutral.Residue and filter paper are placed in evaporating dish, and (quality is counted as M5, unit: in g), putting
Enter and dries 6h in 105 DEG C ± 3 DEG C of drying box, weighing residue+filter paper+evaporating dish quality (quality is counted as M6, unit: g),
It is accurate to 0.1g.
Acid-soluble ratio: S=(M6-M5-M4)/M3*100% (formula 2) is calculated by formula (2)
Wherein, S is hydrochloric acid insoluble substance content in formula, is indicated with percentage.
It is measured 3 times by above-mentioned hydrochloric acid insoluble substance content test method, parallel test measurement result difference should be no more than
0.5%, take arithmetic mean of instantaneous value, as hydrochloric acid insoluble substance content.Specific test number such as table 3.
The acid-soluble ratio test of 3 five groups of carbonate reservoir slit formation leakage sealing agents of table
| Embodiment | Acid-soluble ratio % |
| Embodiment 1 | 78.58 |
| Embodiment 2 | 82.05 |
| Embodiment 3 | 80.70 |
| Embodiment 4 | 76.20 |
| Embodiment 5 | 78.92 |
Find out from experimental data, carbonate reservoir slit formation leakage sealing agent acid-soluble ratio of the present invention is all larger than
75%.
Although the present invention is described referring to specific embodiment, it should be appreciated by those skilled in the art
It is no be detached from real spirit and scope of the invention in the case where, the various changes that can carry out.Furthermore, it is possible to this hair
Bright main body, spirit and scope are variously changed to adapt to specific situation, material, material compositions and method.All
These changes are included in the scope of the claims of the invention.
Claims (10)
1. a kind of preparation method of cross-linked polymer comprising following steps:
1) acrylic acid, 2- acrylamide-2-methyl propane sulfonic and water are mixed, adjusts pH value, obtains the first mixed liquor；
2) crosslinking agent is added in the first mixed liquor of Xiang Suoshu, after heating, the first initiator and the second initiator is added, stirring obtains
To the cross-linked polymer.
2. preparation method according to claim 1, which is characterized in that in terms of mass parts, 30 to 45 parts of the acrylic acid, institute
State 10 to 15 parts of 2- acrylamide-2-methyl propane sulfonic, 100 to 120 parts of the water, 0.05 to 0.1 part of the crosslinking agent is described
First 0.15 to 0.2 part of initiator, described 0.15 to 0.2 part of second initiator.
3. preparation method according to claim 1 or 2, which is characterized in that in step 1), the pH value be 6.8 to
7.2。
4. preparation method as claimed in any of claims 1 to 3, which is characterized in that in step 2), after heating
Temperature is 50 to 60 DEG C.
5. preparation method as claimed in any of claims 1 to 4, which is characterized in that in step 2), stirring when
Between be 20 minutes to 30 minutes.
6. preparation method as claimed in any of claims 1 to 5, which is characterized in that the crosslinking agent is N, and N '-is sub-
Bisacrylamide；And/or
First initiator is potassium peroxydisulfate, and second initiator is sodium hydrogensulfite.
7. a kind of modified calcium carbonate particle, the modified calcium carbonate particle includes shell and core material, wherein the shell is as weighed
Benefit require any one of 1 to 6 described in the obtained cross-linked polymer of preparation method, the core material is calcium carbonate granule.
8. modified calcium carbonate particle according to claim 7, which is characterized in that the partial size of the calcium carbonate granule is 0.8
It is 0.8 to 5mm using it as the partial size of the modified calcium carbonate particle of core material to 5mm；
It is preferred that the partial size of the calcium carbonate granule is 0.8 to 1mm, it is 0.8 using it as the partial size of the modified calcium carbonate particle of core material
To 1mm；
It is preferred that the partial size of the calcium carbonate granule be 3 to 5mm, using its as the partial size of the modified calcium carbonate particle of core material be 3 to
5mm；The partial size of the more preferable calcium carbonate granule is 3.35 to 4.75mm, using it as the partial size of the modified calcium carbonate particle of core material
It is 3.35 to 4.75mm.
9. a kind of sealing agent comprising modified calcium carbonate particle, filler particles and fiber as claimed in claim 7 or 8.
10. sealing agent according to claim 9, which is characterized in that the modified calcium carbonate particle includes the first carbon modified
Sour calcium particle and the second modified calcium carbonate particle, wherein the partial size of the first modified calcium carbonate particle is 3 to 5mm, preferably
The partial size of first modified calcium carbonate particle is 3.35 to 4.75mm；The partial size of the second modified calcium carbonate particle be 0.8 to
1mm；
It preferably, is the first modified calcium carbonate particle and second carbon modified in terms of 100% by the quality of the sealing agent
The dosage of sour calcium particle independently is 23% to 25%；
Preferably, the filler particles are 58 to 75 μm of calcium carbonate powder, are in terms of 100% by the quality of the sealing agent,
Amount is 35% to 38%；
Preferably, the fiber is the sea of polyester fiber and sepiolite mass content greater than 60% that breaking strength is greater than 4 lis of oxen
Afrodite fiber, wherein being in terms of 100% by the quality of the sealing agent, the amount of the polyester fiber is 0.2% to 0.3%, described
The dosage of sepiolite fibre is 11.7% to 18.8%；The length of the more preferable polyester fiber is 8 to 12mm；
Range of the breaking strength of the more preferable fiber in 10 lis of wild marjorams, 35 lis of oxen；
Range of the sepiolite mass content 60% to 66% in the more preferable sepiolite fibre.
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