CN109097013A - A kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent and preparation method thereof - Google Patents
A kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent and preparation method thereof Download PDFInfo
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- CN109097013A CN109097013A CN201811039787.7A CN201811039787A CN109097013A CN 109097013 A CN109097013 A CN 109097013A CN 201811039787 A CN201811039787 A CN 201811039787A CN 109097013 A CN109097013 A CN 109097013A
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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
- C09K8/502—Oil-based compositions
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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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/12—Monomers containing a branched unsaturated aliphatic radical or a ring substituted by an alkyl radical
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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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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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
- C09K2208/18—Bridging agents, i.e. particles for temporarily filling the pores of a formation; Graded salts
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Abstract
This application discloses a kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agents, by the pressure-bearing sealing agent be 100 parts by weight in terms of, the pressure-bearing sealing agent include 5~15 parts by weight oxidized asphalts, the sulfonated gilsonite of 5~20 parts by weight hydrophobically modifieds, 3~5 parts by weight hards grades of bitumen, 2~5 parts by weight asphaltic resins, the nanoscale of 5~20 parts by weight hydrophobically modifieds or micron order graphite oxide, 5~30 parts by weight replace styrene-acrylic copolymer and surplus hydrophobically modified nanoscale or micron order rigid solid granular materials.The preparation method of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent as described above is also disclosed in the application.The high temperature resisting type oil base drilling fluid pressure-bearing sealing agent of the application can block the crack of wide size range, resistant to high temperatures, and shut-off capacity and bearing capacity height, filtrate reducing effect are good, applied widely.
Description
Technical field
This application involves but be not limited to oil and gas well drilling technical field, be particularly, but not limited to a kind of high temperature resisting type
Oil base drilling fluid pressure-bearing sealing agent and preparation method thereof.
Background technique
Oil base drilling fluid is because contamination resistance is strong, and lubricity is good, strong inhibition capability, is conducive to keep wellbore stability, can be maximum
Oil-gas Layer is protected to limit, is increasingly becoming and drills highly difficult high temperature deep well, offshore drilling, high-inclination directional well, horizontal well, each
The important means of kind complicated well section and protection reservoir.But it is boring the hard brittleness for meeting some stratifications and microcrack development and is being crushed
Property stratum when, the filter loss of oil base drilling fluid can greatly increase, oil mutually enter stratum reservoir stress can be caused to change, thus
Lead to weak consolidated formation collapsing or causes other complex accidents.In addition, hydraulic pressure is that the borehole wall is caused to lose by microcrack transmitting
The main reason for steady.As the drillng operation of deep-well and ultradeep well is more and more, the unstability of the borehole wall increases and bottom hole temperature (BHT)
Increase, it is higher and higher with the requirement of pressure-bearing sealing agent to oil base drilling fluid, such as, it is desirable that oil base drilling fluid with pressure-bearing sealing agent not
Only there is good plugging effect, and can (generally requiring high temperature resistant property at 150 DEG C or more) resistant to high temperatures, while also to have
There is the molten object content of higher oil.
A large amount of research work has been done in terms of improving oil base drilling fluid seal-off effect by the country at present, and oil base drilling fluid blocks
Most of agent is made of emulsified asphalt, asphaltic resin, rubber powder, calcium carbonate superfine powder and graphite bead etc., most of these materials
There is no chemical activity, is usually to be randomly dispersed in oil base drilling fluid.When in the microcrack on stratum leak-off occurs for drilling fluid
When, sealing agent forms some mud solid phase blocking, and it is embedded in crack therewith, plays certain physics plugging action, but only
There is plugging effect to the hole of certain size, when there are the hole of sizes and crack, acts on limited.Moreover, high temperature
Such lower sealing agent is easily assembled in oil base drilling fluid, so as to cause that can not block small size microcrack.
Therefore, it is necessary to develop a kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent.
Summary of the invention
It is the general introduction to the theme being described in detail herein below.This general introduction is not the protection model in order to limit claim
It encloses.
This application provides a kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent and preparation method thereof, the pressure-bearing sealing agents
A variety of various sizes of cracks can be blocked, and resistant to high temperatures, be suitable for various complex environments.
Specifically, this application provides a kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agents, with the pressure-bearing sealing agent
For 100 parts by weight meters, the pressure-bearing sealing agent includes the sulfonation of 5~15 parts by weight oxidized asphalts, 5~20 parts by weight hydrophobically modifieds
Pitch, 3~5 parts by weight hards grades of bitumen, 2~5 parts by weight asphaltic resins, 5~20 parts by weight hydrophobically modifieds nanoscale or micron
The nanoscale or micro- of the hydrophobically modified of grade graphite oxide, the styrene-acrylic copolymer that 5~30 parts by weight replace and surplus
Meter level rigid solid granular materials.
In presently filed embodiment, the nanoscale or micron order rigid solid granular materials of the hydrophobically modified can be with
The oxidation of nanoscale four three of the nanometer grade silica, hydrophobically modified of nanometer grade calcium carbonate, hydrophobically modified selected from hydrophobically modified
In iron any one or more.
In presently filed embodiment, the substituent group in the substituted styrene-acrylic copolymer can be uncle
Butyl, methyl or isopropyl.
In presently filed embodiment, the substituted styrene-acrylic copolymer can be selected from 2- methyl -2-
12 ester copolymer of styrene acrylic, 2- tert-butyl-styrene-octadecyl acrylate copolymer, 2- isopropyl-styrene-
Tetradecyl methylacrylate copolymer, 2- methyl-styrene-hexadecyl metrhacrylate copolymer, 4- tert-butyl-styrene-
Octadecyl methacrylate copolymer, 2- isopropyl -12 ester copolymer of styrene-t, 4- isopropyl-benzene second
In alkene-butyl methacrylate copolymer and 4- tert-butyl-styrene-octadecyl acrylate copolymer any one or more
Kind.
Present invention also provides the preparation method of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent as described above, the sides
Method is the following steps are included: by the oxidized asphalt, the sulfonated gilsonite of the hydrophobically modified, the hard grades of bitumen, the pitch tree
Rouge, the nanoscale of the hydrophobically modified or micron order graphite oxide, the substituted styrene-acrylic copolymer and described
The nanoscale or micron order rigid solid granular materials of hydrophobically modified mix, and stir evenly, and obtain the high temperature resisting type oil base and bore
Well liquid pressure-bearing sealing agent.
In presently filed embodiment, the method can with the following steps are included:
A) emulsifier, acrylate, substituted styrene and water are mixed, shear agitation brings it about emulsification, heats shape
At pre-emulsion；
B) initiator is added, brings it about emulsion polymerization；
C) cool down, stop reaction, defoaming agent is added, obtains micelle lotion；
D) the micelle lotion is dried to powder, obtains the substituted styrene-acrylic copolymer.
In presently filed embodiment, the acrylate can be selected from lauryl methacrylate, acrylic acid 12
Ester, butyl methacrylate, tetradecyl methylacrylate, hexadecyl metrhacrylate, octadecyl methacrylate, acrylic acid ten
In diester and octadecyl acrylate any one or more.
In presently filed embodiment, in step a), by the weight of pre-emulsion to be formed be 100 parts by weight in terms of, institute
The additive amount for stating emulsifier is 2~5 parts by weight, and the additive amount of the acrylate is 5~10 parts by weight, the substituted benzene second
The additive amount of alkene is 20~27 parts by weight, and the additive amount of the water is surplus.
In presently filed embodiment, the time of the emulsification can be 20~30min.
In presently filed embodiment, the pre-emulsion that is thermally formed is to be heated to 80~90 DEG C of formation pre-emulsions.
In presently filed embodiment, the emulsifier can be NaLS.
In presently filed embodiment, step b) may include: addition initiator, under agitation, 78 DEG C~
30~50min is kept the temperature at 82 DEG C, makes to continue that emulsion polymerization occurs.
In presently filed embodiment, in order to make system that emulsion polymerization occur, friendship can also be added in step b)
Join agent.The crosslinking agent can use N, N '-methylene-bisacrylamide.
In presently filed embodiment, be 100 parts by weight by the pre-emulsion in terms of, the additive amount of the initiator can be with
For 1~3 parts by weight, the initiator is added by way of being slowly added dropwise, be added dropwise the initiator time can for 50~
70min。
In presently filed embodiment, the initiator can be ammonium persulfate.
In presently filed embodiment, in step c), the cooling can be to be cooled to room temperature.
In presently filed embodiment, the defoaming agent can be acetone.
In presently filed embodiment, stop emulsion polymerization, chain terminating agent can also be added in step c).Chain
Terminator can use tert-butyl hydroperoxide.
The application can obtain it is following the utility model has the advantages that
1, the oil base drilling fluid resistant to high temperatures of the application is with pressure-bearing sealing agent by rigid material, the deformable softwood of more softening points
Material, elastic material and substituted styrene-acrylic copolymer composition, wherein rigid material by hydrophobically modified nanoscale or
Micron order rigid solid granular materials composition, the deformable soft materials of more softening points is by the different oxidized asphalt of softening point, hydrophobic
Modified sulfonated gilsonite, hard grades of bitumen and asphaltic resin composition, and the collaboration heat-resisting property after combining is at 200 DEG C or more, bullet
Property material be hydrophobically modified nanoscale or micron order graphite oxide, form a variety of softening points and a variety of mechanical fractions, and soft
Scleroma is closed, and the crack of wide size range can be blocked, resistant to high temperatures, and closure efficiency greatly improved, applied widely.
2, the high temperature resisting type oil base drilling fluid of the application is built bridge with pressure-bearing sealing agent using rigid material, more softening points
Deformable soft material, elastic material and substituted styrene-acrylic copolymer carry out soft filling, form physics and block, can
To block various sizes of microcrack and joint；Since modified sulfonated gilsonite had both had longer alkyl chain preferable
Ground is dispersed in oily phase, is also had a small amount of sulfonic acid group, is dispersed in water its part.Sulfonic acid in modified sulfonated gilsonite
Group is adsorbable as effect group, is coated in positively charged shale ruptures end face, and alkyl chain-unfolding is dispersed in oily phase,
To form membrane structure, which had not only participated in the micropore between the closure at microcrack and joint, but also blocking rigid particles, realized
Physics blocks and chemical plugging combines, to effectively improve plugging effect and Formation bearing pressure, improves borehole wall stability.
Moreover, the particle size distribution of modified sulfonated gilsonite is wide, to play preferable plugging effect.
3, the high temperature resisting type oil base drilling fluid of the application is good with the compatibility of pressure-bearing sealing agent and oil base drilling fluid, resistant to high temperatures
Effect is good, can apply at a high temperature of 200 DEG C, influences on rheological property of oil base drilling fluid smaller.
4, under the conditions of identical dosage, the high temperature resisting type oil base drilling fluid of the application is with pressure-bearing sealing agent than other sealing agents
With higher shut-off capacity, the effect for reducing filter loss and fluid loss rate is more preferable, and bearing capacity is up to 20MPa or more.
5, under the high temperature conditions, the high temperature resisting type oil base drilling fluid of the application is equal in oil base drilling fluid with pressure-bearing sealing agent
Even dispersion, will not mass settlement.Therefore, the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent of the application can be used for preparing and have
The oil base drilling fluid system of strong shut-off capacity resistant to high temperatures, for example, highly difficult high temperature deep well, offshore drilling, high-inclination directional well,
The strong closure oil base drilling fluid system of horizontal well, various complicated well sections.
6, the synthesis material for the substituted styrene-acrylic copolymer that the application uses comes for general chemical products
Source is very extensive, and synthesis technology is simple, safety and environmental protection, is convenient for industrialized production.
Other features and advantage will illustrate in the following description, also, partly become from specification
It obtains it is clear that being understood and implementing the application.The purpose of the application and other advantages can be by specifications, right
Specifically noted structure is achieved and obtained in claim and attached drawing.
Detailed description of the invention
Attached drawing is used to provide to further understand technical scheme, and constitutes part of specification, with this
The embodiment of application is used to explain the technical solution of the application together, does not constitute the limitation to technical scheme.
Fig. 1 is the schematic diagram that the high temperature and pressure infiltration that the embodiment of the present application uses blocks instrument.
The oil base of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent and comparative example 1-3 that Fig. 2 is the embodiment of the present application 1-3 bores
The filter loss curve of well liquid sealing agent and other type sealing agents.
The oil base of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent and comparative example 1-3 that Fig. 3 is the embodiment of the present application 1-3 bores
The fluid loss rate curve of well liquid sealing agent and other type sealing agents.
Specific embodiment
For the purposes, technical schemes and advantages of the application are more clearly understood, below in conjunction with attached drawing to the application
Embodiment be described in detail.It should be noted that in the absence of conflict, in the embodiment and embodiment in the application
Feature can mutual any combination.
Raw material employed in following embodiment is ordinary commercial products, and the softening point of oxidized asphalt is 140~170
DEG C, the softening point of the sulfonated gilsonite of hydrophobically modified is 230~260 DEG C, and the softening point of hard grades of bitumen is 100~120 DEG C, pitch tree
The softening point of rouge is 130~180 DEG C, and the collaboration heat-resisting property after their combinations is at 200 DEG C or more.
Embodiment 1
A kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent, with the weight of the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent
Amount is that 100g is counted, and is made of following raw material: 5g oxidized asphalt, the sulfonated gilsonite of 5g hydrophobically modified, 3g hard grades of bitumen, 2g pitch
Resin, the nanoscale of 5g hydrophobically modified or micron order graphite oxide, 5g 2- methyl-styrene-hexadecyl metrhacrylate copolymerization
The nanometer grade calcium carbonate of object and the hydrophobically modified of surplus.
The high temperature resisting type oil base drilling fluid pressure-bearing sealing agent is prepared by the following method to obtain:
A) 2g NaLS, 5g hexadecyl metrhacrylate, 20g 2- methyl-styrene and 73g distilled water are added
Enter into shear mixer, stir 25min, be heated to 80 DEG C, forms pre-emulsion；
B) 1g ammonium persulfate is slowly added dropwise, is dripped in 50min, and be kept stirring speed, keeps the temperature 35min at 82 DEG C,
Make to continue that emulsion polymerization occurs；
C) it is cooled to room temperature, defoaming agent acetone is added, obtains micelle lotion；
D) the micelle lotion is dried to powder with spray drying device, obtains the 2- methyl-styrene-methyl-prop
Then olefin(e) acid hexadecyl ester copolymer pellet drips it with the oxidized asphalt, the sulfonated gilsonite of the hydrophobically modified, the hard
The nano-scale carbon of green, the described asphaltic resin, the nanoscale of the hydrophobically modified or micron order graphite oxide and the hydrophobically modified
Sour calcium mixing, stirs evenly to get the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent is arrived.
Embodiment 2
A kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent, with the weight of the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent
Amount is that 100g is counted, and is made of following raw material: 15g oxidized asphalt, the sulfonated gilsonite of 20g hydrophobically modified, 5g hard grades of bitumen, 5g drip
Green resin, the nanoscale of 20g hydrophobically modified or micron order graphite oxide, 30g 4- tert-butyl-styrene-methacrylic acid 18
The nanoscale ferroso-ferric oxide of ester copolymer and the hydrophobically modified of surplus.
The high temperature resisting type oil base drilling fluid pressure-bearing sealing agent is prepared by the following method to obtain:
A) by 5g NaLS, 10g octadecyl methacrylate, 27g 4- tert-butyl-styrene and 58g distilled water
It is added in shear mixer, stirs 30min, be heated to 90 DEG C, form pre-emulsion；
B) 2g ammonium persulfate is slowly added dropwise, is dripped in 55min, and be kept stirring speed, keeps the temperature 31min at 78 DEG C,
Make to continue that emulsion polymerization occurs；
C) it is cooled to room temperature, defoaming agent acetone is added, obtains micelle lotion；
D) the micelle lotion is dried to powder with spray drying device, obtains the 4- tert-butyl-styrene-methyl
Octadecyl acrylate copolymer pellet, then by itself and the oxidized asphalt, the sulfonated gilsonite of the hydrophobically modified, the hard
Pitch, the asphaltic resin, the nanoscale of the hydrophobically modified or micron order graphite oxide and the hydrophobically modified nanoscale
Ferroso-ferric oxide mixing stirs evenly to get the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent is arrived.
Embodiment 3
A kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent, with the weight of the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent
Amount is that 100g is counted, and is made of following raw material: 10g oxidized asphalt, the sulfonated gilsonite of 15g hydrophobically modified, 4g hard grades of bitumen, 3g drip
Green resin, the nanoscale of 15g hydrophobically modified or micron order graphite oxide, 15g 2- isopropyl-styrene-t 14
The nanometer grade silica of ester copolymer and the hydrophobically modified of surplus.
The high temperature resisting type oil base drilling fluid pressure-bearing sealing agent is prepared by the following method to obtain:
A) 3.5g NaLS, 7.5g tetradecyl methylacrylate, 25g 2- isopropyl-styrene and 64g are steamed
Distilled water is added in shear mixer, stirs 20min, is heated to 85 DEG C, forms pre-emulsion；
B) 1.5g ammonium persulfate is slowly added dropwise, is dripped in 60min, and be kept stirring speed, is kept the temperature at 80 DEG C
30min makes to continue that emulsion polymerization occurs；
C) it is cooled to room temperature, defoaming agent acetone is added, obtains micelle lotion；
D) the micelle lotion is dried to powder with spray drying device, obtains the 2- isopropyl-styrene-methyl
Tetradecyl acrylate copolymer pellet, then by itself and the oxidized asphalt, the sulfonated gilsonite of the hydrophobically modified, the hard
Pitch, the asphaltic resin, the nanoscale of the hydrophobically modified or micron order graphite oxide and the hydrophobically modified nanoscale
Silica mixing stirs evenly to get the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent is arrived.
Comparative example 1
A kind of oil base drilling fluid sealing agent, by the weight of the oil base drilling fluid sealing agent for 100g in terms of, by following raw material
Composition: 10g oxidized asphalt, the sulfonated gilsonite of 15g hydrophobically modified, the nanoscale of 15g hydrophobically modified or micron order graphite oxide,
The nanometer grade silica of 15g 2- isopropyl -14 ester copolymer of styrene-t and the hydrophobically modified of surplus.
The oil base drilling fluid sealing agent is prepared by the following method to obtain:
A) 3.5g NaLS, 7.5g tetradecyl methylacrylate, 25g 2- isopropyl-styrene and 64g are steamed
Distilled water is added in shear mixer, stirs 20min, is heated to 85 DEG C, forms pre-emulsion；
B) 1.5g ammonium persulfate is slowly added dropwise, is dripped in 60min, and be kept stirring speed, is kept the temperature at 80 DEG C
30min makes to continue that emulsion polymerization occurs；
C) it is cooled to room temperature, defoaming agent acetone is added, obtains micelle lotion；
D) the micelle lotion is dried to powder with spray drying device, obtains the 2- isopropyl-styrene-methyl
Tetradecyl acrylate copolymer pellet, then by it with the oxidized asphalt, it is the sulfonated gilsonite of the hydrophobically modified, described hydrophobic
The nanometer grade silica of modified nanoscale or micron order graphite oxide and the hydrophobically modified mixes, stir evenly to get
To the oil base drilling fluid sealing agent.
Comparative example 2
A kind of oil base drilling fluid sealing agent, by the weight of the oil base drilling fluid sealing agent for 100g in terms of, by following raw material
Composition: 10g oxidized asphalt, 15g emulsified asphalt, 4g hard grades of bitumen, 3g asphaltic resin, 15g hydrophobically modified nanoscale or micron
The nanoscale of the hydrophobically modified of grade graphite oxide, 15g 2- isopropyl -14 ester copolymer of styrene-t and surplus
Silica.
The oil base drilling fluid sealing agent is prepared by the following method to obtain:
A) 3.5g NaLS, 7.5g tetradecyl methylacrylate, 25g 2- isopropyl-styrene and 64g are steamed
Distilled water is added in shear mixer, stirs 20min, is heated to 85 DEG C, forms pre-emulsion；
B) 1.5g ammonium persulfate is slowly added dropwise, is dripped in 60min, and be kept stirring speed, is kept the temperature at 80 DEG C
30min makes to continue that emulsion polymerization occurs；
C) it is cooled to room temperature, defoaming agent acetone is added, obtains micelle lotion；
D) the micelle lotion is dried to powder with spray drying device, obtains the 2- isopropyl-styrene-methyl
Tetradecyl acrylate copolymer pellet, then by it with the oxidized asphalt, it is the emulsified asphalt, the hard grades of bitumen, described
The nanometer grade silica of asphaltic resin, the nanoscale of the hydrophobically modified or micron order graphite oxide and the hydrophobically modified is mixed
It closes, stirs evenly to get the oil base drilling fluid sealing agent is arrived.
Comparative example 3
A kind of oil base drilling fluid sealing agent, by the weight of the oil base drilling fluid sealing agent for 100g in terms of, by following raw material
Composition: the sulfonated gilsonite of 15g hydrophobically modified, 4g hard grades of bitumen, 3g asphaltic resin, 15g hydrophobically modified nanoscale or micron order
The nanoscale two of the hydrophobically modified of graphite oxide, 15g 2- isopropyl -14 ester copolymer of styrene-t and surplus
Silica.
The oil base drilling fluid sealing agent is prepared by the following method to obtain:
A) 3.5g NaLS, 7.5g tetradecyl methylacrylate, 25g 2- isopropyl-styrene and 64g are steamed
Distilled water is added in shear mixer, stirs 20min, is heated to 85 DEG C, forms pre-emulsion；
B) 1.5g ammonium persulfate is slowly added dropwise, is dripped in 60min, and be kept stirring speed, is kept the temperature at 80 DEG C
30min makes to continue that emulsion polymerization occurs；
C) it is cooled to room temperature, defoaming agent acetone is added, obtains micelle lotion；
D) the micelle lotion is dried to powder with spray drying device, obtains the 2- isopropyl-styrene-methyl
Tetradecyl acrylate copolymer pellet, then by the sulfonated gilsonite, the hard grades of bitumen, the pitch of itself and the hydrophobically modified
The mixing of the nanometer grade silica of resin, the nanoscale of the hydrophobically modified or micron order graphite oxide and the hydrophobically modified,
It stirs evenly to get the oil base drilling fluid sealing agent is arrived.
Performance detection
Below by way of description of test the application's the utility model has the advantages that
Using high temperature and pressure permeate block instrument can simulate with the static filtration of precise measurement underground, 3000psi pressure is provided
The infiltration plugging device of (about 21MPa) can there are Accurate Prediction drilling fluid under differential pressure conditions how to be formed permeability filter cake from
And it is used to block leakage leak-off.The high temperature and pressure infiltration that the application uses is blocked instrument and is simulated using traditional high temperature and pressure heating mantle
Formation temperature, mud cap is oppositely positioned, and pressure enters from mud cap bottom, and a variety of holes can be used from upper collection in filtrate
The crack of the ceramic filter disc simulation Different porosities of degree, as shown in Figure 1.
Based on live common oil base drilling fluid basic recipe, the high temperature resisting type oil base drilling well of measurement embodiment preparation
The sealing characteristics of liquid pressure-bearing sealing agent.
The basic recipe of oil base drilling fluid are as follows: 315mL Saraline185V gas liquefaction+35mL CaCl2(25%)+3 weight
Amount auxiliary+3 weight %CaO+ barite of+2 weight % organoclay of emulsifier of+2 weight % of % primary emulsion is weighed out to 2g/cm3It is denoted as
The high temperature resisting type oil base drilling fluid pressure-bearing sealing agent of 2 weight % embodiments preparation is added on the basis of 1# slurry, investigates it for 1# slurry
The variation of filtration property is blocked after rolling 16 hours at 200 DEG C, test condition is 200 DEG C of temperature, pressure difference 3000psi.
1, the sealing agent of high temperature resisting type the oil base drilling fluid pressure-bearing sealing agent and comparative example of embodiment is investigated according to the above method
To the infiltration plugging effect in different scale crack, the results are shown in Table 1 for investigation.
1 oil base drilling fluid performance test results of table (200 DEG C).
As can be seen from the data in table 1, compared with comparative example 1-3, the high temperature resisting type oil base drilling well of the embodiment of the present application 1-3 preparation
Liquid pressure-bearing sealing agent can block crack well, can block microcrack hole of the size from 3 μm to 10 μm, the size in crack
Wider range, therefore can be effectively reduced the filter loss of oil base drilling fluid.Moreover, the filter loss in table 1 be about 21MPa very
The numerical value measured under high pressure, in the very high situation of pressure (general good bearing capacity is up to about 18-21MPa), drilling fluid
Filter loss still very little, illustrate the bearing capacity of the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent of the embodiment of the present application compared with
By force.The embodiment of the present application 1-3 preparation high temperature resisting type oil base drilling fluid pressure-bearing sealing agent rolled at 200 DEG C after sealing characteristics
Still preferably, illustrate that it is suitable for hot environments.
Meanwhile compared to the pressure-bearing sealing agent of embodiment 3, the sealing agent of comparative example 1-3 be the addition type of pitch not
Together, hard grades of bitumen and asphaltic resin are not added for comparative example 1, and the sulfonated gilsonite of hydrophobically modified is not added for comparative example 2, are changed to that cream is added
Change pitch, oxidized asphalt is not added for comparative example 3, and other components are identical with embodiment 3.But the sealing agent of comparative example 1-3
The sealing agent that plugging effect is obviously not so good as embodiment 3 is good, the effective compounding for illustrating in the embodiment of the present application four kinds of pitches be so that
Sealing agent can be realized the microcrack hole blocked size from 3 μm to 10 μm and be suitable for one of the key of hot environment.
2, the high temperature resisting type oil base drilling fluid pressure-bearing sealing agent of embodiment 1-3 and the sealing agent of comparative example 1-3 and other classes
The plugging effect of type sealing agent compares
It is the embodiment 1 of 2 weight %, the sealing agent of embodiment 2 and embodiment 3, business sealing agent, emulsification drip by concentration
Blueness, rubber powder, comparative example 1, comparative example 2 and comparative example 3 sealing agent be added separately in the 1# slurry of 9 parts of 400ml, investigate 200
DEG C roll 16 hours after block filtration property variation, test condition be 200 DEG C, the emery disc of 5um, pressure difference be 3000psi (about
21MPa), test result is as Figure 2-3.
By Fig. 2 and Fig. 3 as it can be seen that under identical dosage, the oil base drilling fluid of the sealing agent preparation of addition the embodiment of the present application 1-3
Filter loss bored significantly less than the oil base of the sealing agent preparation of addition business sealing agent, emulsified asphalt, rubber powder and comparative example 1-3
The filter loss of well liquid, and the fluid loss rate for adding the oil base drilling fluid of the sealing agent preparation of the embodiment of the present application 1-3 sharply subtracts
It is small, illustrate that the plugging effect of the sealing agent of the embodiment of the present application 1-3 is better than other sealing agents.
Although embodiment disclosed by the application is as above, the content only for ease of understanding the application and use
Embodiment is not limited to the application.Technical staff in any the application fields, is taken off not departing from the application
Under the premise of the spirit and scope of dew, any modification and variation, but the application can be carried out in the form and details of implementation
Scope of patent protection, still should be subject to the scope of the claims as defined in the appended claims.
Claims (10)
1. a kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent, be 100 parts by weight by the pressure-bearing sealing agent in terms of, the pressure-bearing
Sealing agent includes 5~15 parts by weight oxidized asphalts, the sulfonated gilsonite of 5~20 parts by weight hydrophobically modifieds, the drip of 3~5 parts by weight hard
Blueness, 2~5 parts by weight asphaltic resins, the nanoscale of 5~20 parts by weight hydrophobically modifieds or micron order graphite oxide, 5~30 parts by weight
The nanoscale or micron order rigid solid granular materials of the hydrophobically modified of substituted styrene-acrylic copolymer and surplus.
2. high temperature resisting type oil base drilling fluid pressure-bearing sealing agent according to claim 1, wherein the nanometer of the hydrophobically modified
Grade or micron order rigid solid granular materials are selected from the nanoscale titanium dioxide of the nanometer grade calcium carbonate of hydrophobically modified, hydrophobically modified
Silicon, hydrophobically modified nanoscale ferroso-ferric oxide in any one or more.
3. high temperature resisting type oil base drilling fluid pressure-bearing sealing agent according to claim 1, wherein the substituted styrene third
Substituent group in olefin(e) acid ester copolymer is tert-butyl, methyl or isopropyl.
4. high temperature resisting type oil base drilling fluid pressure-bearing sealing agent according to claim 1, wherein the substituted styrene third
Olefin(e) acid ester copolymer is selected from 12 ester copolymer of 2- methyl -2- styrene acrylic, 2- tert-butyl-styrene-acrylic acid 18
Ester copolymer, 2- isopropyl -14 ester copolymer of styrene-t, 2- methyl-styrene-methacrylic acid 16
Ester copolymer, 4- tert-butyl-styrene-octadecyl methacrylate copolymer, 2- isopropyl-styrene-t ten
Two ester copolymers, 4- isopropyl-styrene-t acrylate copolymer and 4- tert-butyl-styrene-octadecyl acrylate
In copolymer any one or more.
5. the preparation method of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent described in any one of -4 according to claim 1, institute
Method is stated the following steps are included: by the oxidized asphalt, the sulfonated gilsonite of the hydrophobically modified, the hard grades of bitumen, the drip
Green resin, the nanoscale of the hydrophobically modified or micron order graphite oxide, the substituted styrene-acrylic copolymer and
The nanoscale or micron order rigid solid granular materials of the hydrophobically modified mix, and stir evenly, and obtain the high temperature resisting type oil
Base drilling fluid pressure-bearing sealing agent.
6. according to the method described in claim 5, the method also includes following steps:
A) emulsifier, acrylate, substituted styrene and water are mixed, shear agitation brings it about emulsification, is thermally formed pre-
Lotion；
B) initiator is added, brings it about emulsion polymerization；
C) cool down, stop reaction, defoaming agent is added, obtains micelle lotion；
D) the micelle lotion is dried to powder, obtains the substituted styrene-acrylic copolymer.
7. according to the method described in claim 6, wherein, the acrylate is selected from lauryl methacrylate, acrylic acid ten
Diester, butyl methacrylate, tetradecyl methylacrylate, hexadecyl metrhacrylate, octadecyl methacrylate, acrylic acid
In ten diester and octadecyl acrylate any one or more.
8. according to the method described in claim 6, wherein, in step a), with the weight of pre-emulsion to be formed for 100 parts by weight
Meter, the additive amount of the emulsifier are 2~5 parts by weight, and the additive amount of the acrylate is 5~10 parts by weight, the substitution
The additive amount of styrene be 20~27 parts by weight, the additive amount of the water is surplus；
Optionally, the time of the emulsification is 20~30min, and the pre-emulsion that is thermally formed is to be heated to 80~90 DEG C to be formed in advance
Lotion；
Optionally, the emulsifier is NaLS.
9. according to the method described in claim 6, wherein, step b) includes: addition initiator, under agitation, at 78 DEG C
30~50min is kept the temperature at~82 DEG C, makes to continue that emulsion polymerization occurs；
Optionally, in terms of by the pre-emulsion for 100 parts by weight, the additive amount of the initiator is 1~3 parts by weight, by slow
The initiator is added in the mode of dropwise addition, and the time that the initiator is added dropwise is 50~70min；Optionally, the initiator is
Ammonium persulfate.
10. according to the method described in claim 6, wherein, in step c), the cooling is to be cooled to room temperature；Optionally, described
Defoaming agent is acetone.
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| CN110330957A (en) * | 2019-07-03 | 2019-10-15 | 济源市宏鑫实业有限公司 | A kind of oil base blocks fluid loss additive and preparation method thereof |
| CN111484833A (en) * | 2020-03-27 | 2020-08-04 | 中国石油天然气集团有限公司 | Low-friction film-forming plugging agent for high-temperature oil-based drilling fluid and preparation method and application thereof |
| CN112048288A (en) * | 2020-09-01 | 2020-12-08 | 武汉思越化学技术有限公司 | Oil-based drilling fluid filtration loss reducing plugging agent |
| CN112778984A (en) * | 2021-02-03 | 2021-05-11 | 库尔勒同益工贸有限责任公司 | Low-fluorescence anti-collapse plugging agent for drilling fluid and preparation method thereof |
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| CN111484833A (en) * | 2020-03-27 | 2020-08-04 | 中国石油天然气集团有限公司 | Low-friction film-forming plugging agent for high-temperature oil-based drilling fluid and preparation method and application thereof |
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| CN112048288A (en) * | 2020-09-01 | 2020-12-08 | 武汉思越化学技术有限公司 | Oil-based drilling fluid filtration loss reducing plugging agent |
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| CN113416272B (en) * | 2021-06-22 | 2022-06-07 | 西南石油大学 | Synthesis of nano emulsion plugging agent and oil-based drilling fluid |
| CN113416272A (en) * | 2021-06-22 | 2021-09-21 | 西南石油大学 | Synthesis of nano emulsion plugging agent and oil-based drilling fluid |
| CN113355063A (en) * | 2021-06-22 | 2021-09-07 | 西南石油大学 | Elastic graphite strong-adsorption salt-resistant plugging agent and oil-based drilling fluid |
| CN115820227A (en) * | 2021-09-17 | 2023-03-21 | 中国石油天然气股份有限公司 | Borehole wall sealing pressure-bearing drilling fluid and preparation method thereof |
| CN114276791A (en) * | 2021-12-14 | 2022-04-05 | 成都西油华巍科技有限公司 | High-filtration-loss plugging agent for oil-based drilling fluid |
| CN114686190A (en) * | 2021-12-14 | 2022-07-01 | 中国石油天然气集团有限公司 | High-temperature-resistant and saturated-salt-resistant plugging fluid loss agent and preparation method thereof |
| CN114214046A (en) * | 2022-01-24 | 2022-03-22 | 西南石油大学 | High-temperature-resistant modified manganese dioxide nano plugging agent and oil-based drilling fluid |
| CN114605969A (en) * | 2022-03-15 | 2022-06-10 | 西南石油大学 | Plugging material, plugging type oil-based drilling fluid and preparation method thereof |
| CN114605969B (en) * | 2022-03-15 | 2023-12-08 | 西南石油大学 | Plugging material, plugging type oil-based drilling fluid and preparation method thereof |
| CN116042195A (en) * | 2022-11-10 | 2023-05-02 | 四川康荣石油化工科技有限公司 | Broad-spectrum plugging oil-based drilling fluid and application thereof |
| CN116445138A (en) * | 2023-04-20 | 2023-07-18 | 中石化石油工程技术服务股份有限公司 | Plugging agent and preparation method and application thereof |
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