CN106675537A - Fiber flexibilizer for well cementing slurry and preparation method of fiber flexibilizer - Google Patents
Fiber flexibilizer for well cementing slurry and preparation method of fiber flexibilizer Download PDFInfo
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- CN106675537A CN106675537A CN201611089451.2A CN201611089451A CN106675537A CN 106675537 A CN106675537 A CN 106675537A CN 201611089451 A CN201611089451 A CN 201611089451A CN 106675537 A CN106675537 A CN 106675537A
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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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
Abstract
The invention provides a fiber flexibilizer for well cementing slurry and a preparation method of the fiber flexibilizer. The fiber flexibilizer is prepared from the following raw materials in parts by weight: 20-60 parts of whisker material, 5-10 parts of surfactant, 5-10 parts of silane coupling agent, 1-5 parts of defoaming agent, 10-25 parts of stabilizer, 100 parts of water and 250-1,000 parts of absolute ethyl alcohol. The preparation method of the fiber flexibilizer comprises the following steps of preparing the silane coupling agent into 1-2wt% diluent by using the absolute ethyl alcohol; pouring the whisker material, the surfactant, the defoaming agent and the prepared silane coupling agent diluent into a container containing water, stirring for 20-40 minutes, dispersing under ultrasonic waves for 20-40 minutes and carrying out suction filtration to obtain a modified whisker; and drying the modified whisker and blending with a stabilizer to obtain the fiber flexibilizer. The fiber flexibilizer can be uniformly dispersed into the slurry, the tenacity of set cement is relatively well improved and the construction security is not affected.
Description
Technical field
The present invention relates to a kind of cementing slurry belongs to the oil of field of petroleum exploitation with fiber reinforced dose and preparation method thereof
Gas well cementing technical field.
Background technology
The permanently effective Inter-zonal packing ability of cement sheath is to realize the premise that oil-gas field development increases production in pit shaft, is also oil gas
The guarantee of the long-term production life of well of well.However, well-cementing cement is a kind of fragile material for having a congenital microdefect, it has deformation
The inherent shortcoming such as ability, tensile strength are low, impact resistance is poor.It is in subsequent construction such as pressure testing, perforation, pressure break and exploitation life
During product etc., due to being affected by temperature, pressure change, impact, vibrations etc., easily rupture, cause the mechanics of cement sheath complete
Property destroyed, so gently then cause that annular space is with pressure, oil gas water breakthrough, it is heavy then cause Oil/gas Well to be scrapped.
At present, in well cementation field, the mechanical property of Behavior of Hardened Cement Paste is improved using fiber more.Fiber can be between cement stone substrate
" bridging " effect is played, hardened oilwell cement mechanical property is improved with the mode of action of " lacing wire ".
The fibrous material commonly used in mortar architecture has inorfil, such as glass fibre, carbon fiber；Synthetic fibers, such as
The fibers such as nylon fiber, polyester, polypropylene；String, such as bamboo fibre, flaxen fiber.However, these fibers also exist it is following
Defect：One is that density is relatively low, is disperseed not open after slurry, is suspended in slurry surface；Two is that surface hydrophobicity, wettability are poor, slurry
When easily reunite, pipeline is easily blocked during pumping, cause to suppress pump, affect construction safety.
The content of the invention
For solve above-mentioned technical problem, it is an object of the invention to provide a kind of cementing slurry with fiber reinforced dose and its
Preparation method.Fiber reinforced dose of the present invention can be homogeneously dispersed in cement mortar, had to the toughness of Behavior of Hardened Cement Paste and preferably changed
It is kind, and do not affect construction safety.
To reach above-mentioned purpose, present invention firstly provides a kind of cementing slurry is with fiber reinforced dose, in parts by weight,
Its raw material composition includes：20~60 parts of crystal whisker materials, 5~10 parts of surfactants, 5~10 parts of silane couplers, 1~5 part disappear
Infusion, 10~25 parts of stabilizers, 100 parts of water and 250~1000 parts of absolute ethyl alcohols.
In the present invention, crystal whisker materials refer to self-assembling formation or under manual control condition (principal mode) with monocrystalline
A kind of fiber that formula grows into, its diameter very little (the micron order of magnitude), do not contain defect present in usual material (crystal boundary,
Dislocation, hole etc.), its atomic arrangement high-sequential, thus its intensity is close to the theoretical value of perfect crystal.Its mechanical strength etc.
In adjacent interatomic force.The height-oriented structure of whisker makes it have high intensity, high-modulus and high elongation rate, is mainly used as being combined
The reinforcement of material, for manufacturing high strength composite.
In above-mentioned cementing slurry with fiber reinforced dose, it is preferable that the crystal whisker materials include potassium titanate crystal whisker, boron
The combination of one or more in sour al whisker, magnesium sulfate crystal whisker, silicon carbide whisker and magnesium borate crystal whisker etc..
In above-mentioned cementing slurry with fiber reinforced dose, it is preferable that the length of the crystal whisker materials is 10-500 μm,
A diameter of 0.1-10 μm, draw ratio is 1-5000.
In above-mentioned cementing slurry with fiber reinforced dose, it is preferable that the surfactant includes styryl benzene
The combination of one or more in phenol polyethenoxy ether, dodecyl sodium sulfate and aliphatic acid polyethenoxy ether etc..
In above-mentioned cementing slurry with fiber reinforced dose, it is preferable that the silane coupler include KH-550 and/or
KH-560 etc..
In above-mentioned cementing slurry with fiber reinforced dose, it is preferable that the defoamer is including tributyl phosphate etc..
In above-mentioned cementing slurry with fiber reinforced dose, it is preferable that the stabilizer includes ultrafine slag, hard charcoal
The combination of one or more in black, SILICA FUME, wollastonite in powder, nano silicon and xanthans etc..
In above-mentioned cementing slurry with fiber reinforced dose, it is preferable that the water is distilled water.
Specific embodiment of the invention, it is preferable that above-mentioned cementing slurry is by following with fiber reinforced dose
Prepared by step：
(1) preparation of silane coupler dilution：In parts by weight, by 5~10 parts of silane couplers with 250~1000 parts
Absolute ethyl alcohol is made into the dilution that mass fraction is 1~2%；
(2) surface of whisker is modified：In parts by weight, by 20~60 parts of crystal whisker materials, 5~10 parts of surfactants, 1~
The silane coupler dilution that 5 parts of defoamers and step (1) are prepared is poured into successively in the container for filling 100 parts of water, stirring 20
~40min, then 20~40min of dispersion in ultrasonic wave is placed in, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are in 100~150 DEG C of bars
48~96h is dried under part, then dried modified crystal whiskers are blended with 10~25 parts of stabilizers, obtain described well cementation water
Mud is with fiber reinforced dose.
In above-mentioned preparation process, it is preferable that step (2) also includes：Reusability distilled water flushing changes during suction filtration
Property whisker crude product, to remove unnecessary surfactant, silane coupler and defoamer, obtain described modified crystal whiskers.
Whisker is a kind of chopped strand, and with preferably wettability, the Jing present invention's is modified, can be homogeneously dispersed in
In cement mortar, there is preferably improvement to the toughness of Behavior of Hardened Cement Paste, and do not affect construction safety.
In the recovery process of oil, in order to increase production capacity, it is often necessary to which reservoir is transformed, acid fracturing is exactly it
A kind of middle most effective also the most frequently used measure.Therefore require that Behavior of Hardened Cement Paste and its composition material have the characteristic of acid corrosion-resistant, this
Invention is using the one kind or several in potassium titanate crystal whisker, aluminium borate whisker, magnesium sulfate crystal whisker, silicon carbide whisker and magnesium borate crystal whisker
Kind combination, good acid resistance is respectively provided with, and do not adopt easy with the magnesium carbonate whisker of sour generation chemical reaction etc., without the need for right
Whisker carries out further cladding process, you can reach the effect of resistance to sour.
Crystal whisker materials are because with ultra-fine size, surface energy is easily assembled agglomerating, causes it to disperse in the base than larger
Property is poor, and the deployment conditions of non-modified crystal whisker materials in water are shown in Fig. 1.The surfactant that the present invention is adopted can be reduced
The surface energy of crystal whisker materials, makes crystal whisker materials disperse in the base evenly；Using defoamer can suppress because add surface
Activating agent and the bubble problem that causes, eliminate cement mortar because cause to pile up containing a large amount of bubbles it is tight do not make under cement strength
This problem drops；Because of aluminium borate whisker (2.93g/cm3), magnesium sulfate crystal whisker (2.69g/cm3), silicon carbide whisker (3.21g/cm3)
And magnesium borate crystal whisker (2.91g/cm3) etc. material density it is of a relatively high, easily settle in cement mortar, cause toughness reinforcing material
Material disperses heterogeneity in cement mortar, so as to affect toughening effect, therefore adopts the stabilizer of the present invention to solve the problem；Together
When, the part composition in stabilizer such as ultrafine slag, SILICA FUME etc. can also improve the interface performance of whisker-cement matrix, increase
Big matrix wraps up power to the bonding of whisker.By the synergy of fiber reinforced dose provided by the present invention of each raw material, the fibre
Dimension toughener is added in cementing slurry, can be homogeneously dispersed in cement mortar, so as to be effectively improved the power of hardened oilwell cement
Performance is learned, compression strength, tensile splitting strength to hardened oilwell cement, shock resistance all have and be greatly increased, together
When reduce Behavior of Hardened Cement Paste Young's modulus, and do not affect construction safety.
On the other hand, present invention also offers a kind of above-mentioned cementing slurry is with fiber reinforced dose of preparation method, its
Comprise the following steps：
(1) preparation of silane coupler dilution：In parts by weight, by 5~10 parts of silane couplers with 250~1000 parts
Absolute ethyl alcohol is made into the dilution that mass fraction is 1~2%；
(2) surface of whisker is modified：In parts by weight, by 20~60 parts of crystal whisker materials, 5~10 parts of surfactants, 1~
The silane coupler dilution that 5 parts of defoamers and step (1) are prepared is poured into successively in the container for filling 100 parts of water, stirring 20
~40min, then 20~40min of dispersion in ultrasonic wave is placed in, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are in 100~150 DEG C of bars
48~96h is dried under part, then dried modified crystal whiskers are blended with 10~25 parts of stabilizers, obtain described well cementation water
Mud is with fiber reinforced dose.
In above-mentioned preparation method, it is preferable that step (2) also includes：Reusability distilled water flushing changes during suction filtration
Property whisker crude product, to remove unnecessary surfactant, silane coupler and defoamer, obtain described modified crystal whiskers.
The preparation process is simple of fiber reinforced dose of present invention offer, it is easy to accomplish industrialized production.This fiber reinforced dose
With preferably hydrophilicity, the wettability in water is good, can be evenly dispersed in oil well cement paste, does not affect construction peace
Entirely.Fiber reinforced dose of compression strength that can effectively improve hardened oilwell cement, tensile splitting strength, the shock resistance, while
Reduce Behavior of Hardened Cement Paste Young's modulus.
In sum, fiber reinforced dose of present invention offer, with preferably hydrophilicity, the wettability in water
It is good, can be evenly dispersed in oil well cement paste.Fiber reinforced dose of the present invention is added in cementing slurry, water is not interfered with
The working security of mud, and the mechanical property of hardened oilwell cement can be effectively improved, the compression strength, splitting to hardened oilwell cement
Tensile strength, shock resistance have largely improve, while reduce Behavior of Hardened Cement Paste Young's modulus.The fiber that the present invention is provided
Toughener is applied to oil gas well cementing operation operation, has broad application prospects.
With fiber reinforced dose compared with the prior art, its main advantage is the cementing slurry that the present invention is provided：
(1) surface modification technology of whisker and fiber reinforced dose of preparation process is simple, it is easy to accomplish industrialized production；
(2) this fiber reinforced dose has preferably hydrophilicity, and the wettability in water is good, can be evenly dispersed in oil
In cementing slurry for well, construction safety is not affected；
(3) fiber reinforced dose of compression strength that can effectively improve hardened oilwell cement, tensile splitting strength, the shock resistance
Performance；
(4) after is added in cement for this fiber reinforced dose, make cement that there is the strong characteristic of impact resistance, perforation is to water
The destruction of mud ring is little, fundamentally solves " secondary channelling " problem.
Description of the drawings
Fig. 1 is deployment conditions figure of the non-modified crystal whisker materials in water.
Fig. 2 is the fiber reinforced dose of deployment conditions figure in water that embodiment 1 is provided.
Fig. 3 is deployment conditions figure of the traditional polymer fiber toughener in water.
Specific embodiment
In order to be more clearly understood to the technical characteristic of the present invention, purpose and beneficial effect, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
A kind of cementing slurry is present embodiments provided with fiber reinforced dose, it is through the following steps that prepare：
(1) preparation of silane coupler dilution：In parts by weight, it is 5 parts of silane resin acceptor kh-550s are anhydrous with 500 parts
Ethanol is made into the dilution that mass fraction is 1%；
(2) surface of whisker is modified：In parts by weight, by 20 parts of crystal whisker materials, (it is by 10 parts of magnesium sulfate crystal whiskers, 5 parts of carbon
SiClx whisker, 5 parts of magnesium borate crystal whisker compositions；Wherein, the length of magnesium sulfate crystal whisker is 10-60 μm, a diameter of 0.1-1 μm, carbonization
The length of silicon wafer palpus is 50-100 μm, a diameter of 0.1-0.6 μm, and the length of magnesium borate crystal whisker is 10-100 μm, a diameter of 0.1-
2.0 μm), 5 parts of surfactant styrylphenol polyoxyethylene ethers, 1 part of defoamer tributyl phosphate and steps (1) prepare
Silane coupler dilution pour into successively in the beaker for filling 100 parts of distilled water, stir 20min, then be placed in ultrasonic wave point
Scattered 20min, then carries out suction filtration, and the Reusability distilled water flushing modified crystal whiskers crude product during suction filtration, unnecessary to remove
Surfactant, silane coupler and defoamer, obtain modified crystal whiskers；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are done under the conditions of 150 DEG C
Dry 48h, then dried modified crystal whiskers and 10 parts of stabilizers (it is made up of 9 parts of wollastonites in powder, 1 part of xanthans) are carried out altogether
It is mixed, described cementing slurry is obtained with fiber reinforced dose, it is designated as XWZR-1.
The fiber reinforced dose of XWZR-1 that the present embodiment is provided is added to the water, its deployment conditions is as shown in Figure 2.
By polymer-based fiber toughener (polypropylene fibre, molecular structural formula
Length 1.5-50mm) it is added to the water in the same scale, its deployment conditions is as shown in Figure 3.Can be seen by the contrast of Fig. 2-3
Go out, fiber reinforced dose of the present embodiment offer has preferably hydrophilicity, and the wettability in water is good, can be uniformly dispersed
In water.
Embodiment 2
A kind of cementing slurry is present embodiments provided with fiber reinforced dose, itself through the following steps that prepare：
(1) preparation of silane coupler dilution：In parts by weight, it is 5 parts of silane resin acceptor kh-550s are anhydrous with 250 parts
Ethanol is made into the dilution that mass fraction is 2%；
(2) surface of whisker is modified：In parts by weight, by 60 parts of crystal whisker materials, (it is by 30 parts of magnesium sulfate crystal whiskers, 10 parts of carbon
SiClx whisker, 20 parts of magnesium borate crystal whisker compositions；Wherein, the length of magnesium sulfate crystal whisker is 10-60 μm, a diameter of 0.1-1.0 μm, carbon
The length of SiClx whisker is 50-100 μm, a diameter of 0.1-0.6 μm, and the length of magnesium borate crystal whisker is 10-100 μm, a diameter of
0.1-2.0 μm), 10 parts of surfactant sodium dodecyl base sodium sulfonates, 5 parts of defoamer tributyl phosphates and steps (1) prepare
Silane coupler dilution is poured into successively in the beaker for filling 100 parts of distilled water, stirs 20min, then is placed in dispersion in ultrasonic wave
20min, then carries out suction filtration, and the Reusability distilled water flushing modified crystal whiskers crude product during suction filtration, unnecessary to remove
Surfactant, silane coupler and defoamer, obtain modified crystal whiskers；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are done under the conditions of 120 DEG C
Dry 72h, then by dried modified crystal whiskers and 25 parts of stabilizers (its by 10 parts of ultrafine slags, 5 parts of white carbons, 5 parts of SILICA FUMEs, 3
Part wollastonite in powder, 1 part of nano silicon, 1 part of xanthans composition) it is blended, obtain described cementing slurry fiber
Toughener, is designated as XWZR-2.
Embodiment 3
A kind of cementing slurry is present embodiments provided with fiber reinforced dose, itself through the following steps that prepare：
(1) preparation of silane coupler dilution：In parts by weight, by 10 parts of silane coupler KH-560 with 1000 parts of nothings
Water-ethanol is made into the dilution that mass fraction is 1%；
(2) surface of whisker is modified：In parts by weight, by 30 parts of crystal whisker materials, (it is by 5 parts of potassium titanate crystal whiskers, 5 parts of boric acid
Al whisker, 5 parts of silicon carbide whiskers, 15 parts of magnesium sulfate crystal whisker compositions；Wherein, the length of potassium titanate crystal whisker is 10-100 μm, diameter
For 0.1-1.0 μm, the length of aluminium borate whisker is 10-100 μm, a diameter of 0.1-2.0 μm, and the length of silicon carbide whisker is 50-
100 μm, a diameter of 0.1-0.6 μm, the length of magnesium sulfate crystal whisker is 10-60 μm, a diameter of 0.1-1 μm), 5 parts of surfactants
The silane coupler dilution that aliphatic acid polyethenoxy ether, 3 parts of defoamer tributyl phosphates and step (1) are prepared is poured into successively
In filling the beaker of 100 parts of distilled water, 20min is stirred, then be placed in ultrasonic wave and disperse 20min, then carry out suction filtration, and taken out
Reusability distilled water flushing modified crystal whiskers crude product during filter, to remove unnecessary surfactant, silane coupler and disappear
Infusion, obtains modified crystal whiskers；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are done under the conditions of 130 DEG C
Dry 72h, then (it is by 10 parts of SILICA FUMEs, 8 parts of wollastonites in powder, 1 part of nano-silica by dried modified crystal whiskers and 20 parts of stabilizers
SiClx, 1 part of xanthans composition) it is blended, described cementing slurry is obtained with fiber reinforced dose, it is designated as XWZR-3.
Embodiment 4
A kind of cementing slurry is present embodiments provided with fiber reinforced dose, itself through the following steps that prepare：
(1) preparation of silane coupler dilution：In parts by weight, by 10 parts of silane coupler KH-560 with 500 parts of nothings
Water-ethanol is made into the dilution that mass fraction is 2%；
(2) surface of whisker is modified：In parts by weight, by 50 parts of crystal whisker materials, (it is by 5 parts of potassium titanate crystal whiskers, 5 parts of boric acid
Al whisker, 10 parts of magnesium sulfate crystal whiskers, 15 parts of silicon carbide whiskers, 15 parts of magnesium borate crystal whisker compositions；Wherein, the length of potassium titanate crystal whisker
For 10-100 μm, a diameter of 0.1-1.0 μm, the length of aluminium borate whisker is 10-100 μm, a diameter of 0.1-2.0 μm, magnesium sulfate
The length of whisker is 10-60 μm, a diameter of 0.1-1.0 μm, and the length of silicon carbide whisker is 50-100 μm, a diameter of 0.1-0.6 μ
M, the length of magnesium borate crystal whisker is 10-100 μm, a diameter of 0.1-2.0 μm), 10 parts of surfactant fatty acid APEOs,
The silane coupler dilution that 5 parts of defoamer tributyl phosphates and step (1) are prepared is poured into fill 100 parts of distilled water successively
In beaker, 20min is stirred, then be placed in ultrasonic wave and disperse 20min, then carry out suction filtration, and Reusability steams during suction filtration
Distilled water rinses modified crystal whiskers crude product, to remove unnecessary surfactant, silane coupler and defoamer, obtains modified crystalline substance
Palpus；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are done under the conditions of 100 DEG C
Dry 96h, then by dried modified crystal whiskers and 25 parts of stabilizers (its by 1 part of ultrafine slag, 1 part of white carbon, 10 parts of SILICA FUMEs,
10 parts of wollastonites in powder, 2 parts of nano silicons, 1 part of xanthans composition) it is blended, obtain described cementing slurry fine
Dimension toughener, is designated as XWZR-4.
Comparative example 1 (is not added with defoamer, contrast with embodiment 2)
This comparative example provide a kind of cementing slurry with fiber reinforced dose, itself through the following steps that preparation：
(1) preparation of silane coupler dilution：In parts by weight, it is 5 parts of silane resin acceptor kh-550s are anhydrous with 250 parts
Ethanol is made into the dilution that mass fraction is 2%；
(2) surface of whisker is modified：In parts by weight, by 60 parts of crystal whisker materials, (it is by 30 parts of magnesium sulfate crystal whiskers, 10 parts of carbon
SiClx whisker, 20 parts of magnesium borate crystal whisker compositions；Wherein, the length of magnesium sulfate crystal whisker is 10-60 μm, a diameter of 0.1-1.0 μm, carbon
The length of SiClx whisker is 50-100 μm, a diameter of 0.1-0.6 μm, and the length of magnesium borate crystal whisker is 10-100 μm, a diameter of
0.1-2.0 μm), the silane coupler dilution for preparing of 10 parts of surfactant sodium dodecyl base sodium sulfonates and step (1) successively
In pouring the beaker for filling 100 parts of distilled water into, 20min is stirred, then be placed in ultrasonic wave and disperse 20min, then carry out suction filtration, and
The Reusability distilled water flushing modified crystal whiskers crude product during suction filtration, to remove unnecessary surfactant and silane coupled
Agent, obtains modified crystal whiskers；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are done under the conditions of 120 DEG C
Dry 72h, then by dried modified crystal whiskers and 25 parts of stabilizers (its by 10 parts of ultrafine slags, 5 parts of white carbons, 5 parts of SILICA FUMEs, 3
Part wollastonite in powder, 1 part of nano silicon, 1 part of xanthans composition) it is blended, cementing slurry is obtained with fiber reinforced dose,
It is designated as XWZR-5.
Comparative example 2 (is not added with stabilizer, contrast with embodiment 3)
This comparative example provides a kind of cementing slurry with fiber reinforced dose, and it is through the following steps that prepare：
(1) preparation of silane coupler dilution：In parts by weight, by 10 parts of silane coupler KH-560 with 1000 parts of nothings
Water-ethanol is made into the dilution that mass fraction is 1%；
(2) surface of whisker is modified：In parts by weight, by 30 parts of crystal whisker materials, (it is by 5 parts of potassium titanate crystal whiskers, 5 parts of boric acid
Al whisker, 5 parts of silicon carbide whiskers, 15 parts of magnesium sulfate crystal whisker compositions；Wherein, the length of potassium titanate crystal whisker is 10-100 μm, diameter
For 0.1-1.0 μm, the length of aluminium borate whisker is 10-100 μm, a diameter of 0.1-2.0 μm, and the length of silicon carbide whisker is 50-
100 μm, a diameter of 0.1-0.6 μm, the length of magnesium sulfate crystal whisker is 10-60 μm, a diameter of 0.1-1 μm), 5 parts of surfactants
The silane coupler dilution that aliphatic acid polyethenoxy ether, 3 parts of defoamer tributyl phosphates and step (1) are prepared is poured into successively
In filling the beaker of 100 parts of distilled water, 20min is stirred, then be placed in ultrasonic wave and disperse 20min, then carry out suction filtration, and taken out
Reusability distilled water flushing modified crystal whiskers crude product during filter, to remove unnecessary surfactant, silane coupler and disappear
Infusion, obtains modified crystal whiskers；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are done under the conditions of 130 DEG C
Dry 72h, obtains cementing slurry with fiber reinforced dose, is designated as XWZR-6.
The cement-slurry method of table 1 and performance
Remarks：[1]. cement mortar is prepared and determined according to API10A specifications；[2]. tensile splitting strength is real by Brazil's splitting
Test is obtained；[3]. Young's modulus is measured by three-axis force experiment；[4]. shock resistance is measured by pendulum experiment；[5]. in table
BCG-200L is AMPS copolymer class anti-gas channeling fluid loss agent, and BXR-200L is small molecule acids retarder, and G603 is tricresyl phosphate
Butyl ester defoamer, XWZR-1, XWZR-2, XWZR-3, XWZR-4, XWZR-5, XWZR-6 are respectively embodiment 1-4 and comparative example 1-
2 fiber reinforced doses for preparing.
As can be seen from Table 1, the mechanics of fiber reinforced dose of XWZR-1, XWZR-2, XWZR-3, XWZR-4 to hardened oilwell cement
Performance has preferable improvement, can preferably improve compression strength, tensile splitting strength and the shock resistance of hardened oilwell cement
Performance, while the Young's modulus of hardened oilwell cement can also be reduced, and does not interfere with the workability of cement mortar, therefore the present invention is carried
For fiber reinforced dose of cementing slurry can effectively reduce the fragility of Behavior of Hardened Cement Paste, so that it is guaranteed that the long term seal of cement sheath is complete
Property.
Claims (10)
1. with fiber reinforced dose, in parts by weight, its raw material composition includes a kind of cementing slurry：20~60 parts of crystal whisker materials, 5
~10 parts of surfactants, 5~10 parts of silane couplers, 1~5 part of defoamer, 10~25 parts of stabilizers, 100 parts of water and 250
~1000 parts of absolute ethyl alcohols.
2. cementing slurry according to claim 1 is with fiber reinforced dose, wherein, the crystal whisker materials include that potassium titanate is brilliant
The combination of one or more in palpus, aluminium borate whisker, magnesium sulfate crystal whisker, silicon carbide whisker and magnesium borate crystal whisker.
3. cementing slurry according to claim 1 and 2 is with fiber reinforced dose, wherein, the length of the crystal whisker materials is
10-500 μm, a diameter of 0.1-10 μm, draw ratio is 1-5000.
4. cementing slurry according to claim 1 is with fiber reinforced dose, wherein, the surfactant includes styrene
The combination of one or more in base phenol APEO, dodecyl sodium sulfate and aliphatic acid polyethenoxy ether.
5. cementing slurry according to claim 1 is with fiber reinforced dose, wherein, the silane coupler includes KH-550
And/or KH-560.
6. cementing slurry according to claim 1 is with fiber reinforced dose, wherein, the defoamer includes tricresyl phosphate fourth
Ester.
7. cementing slurry according to claim 1 is with fiber reinforced dose, wherein, the stabilizer include ultrafine slag,
The combination of one or more in white carbon, SILICA FUME, wollastonite in powder, nano silicon and xanthans.
8. cementing slurry according to claim 1 is with fiber reinforced dose, and it is through the following steps that prepare：
(1) preparation of silane coupler dilution：In parts by weight, it is 5~10 parts of silane couplers are anhydrous with 250~1000 parts
Ethanol is made into the dilution that mass fraction is 1~2%；
(2) surface of whisker is modified：In parts by weight, by 20~60 parts of crystal whisker materials, 5~10 parts of surfactants, 1~5 part
The silane coupler dilution that defoamer and step (1) are prepared is poured into successively in the container for filling 100 parts of water, and stirring 20~
40min, then 20~40min of dispersion in ultrasonic wave is placed in, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are under the conditions of 100~150 DEG C
48~96h is dried, then dried modified crystal whiskers are blended with 10~25 parts of stabilizers, obtain described cementing slurry
With fiber reinforced dose.
9. with fiber reinforced dose of preparation method, it includes following the cementing slurry described in a kind of any one of claim 1-8
Step：
(1) preparation of silane coupler dilution：In parts by weight, it is 5~10 parts of silane couplers are anhydrous with 250~1000 parts
Ethanol is made into the dilution that mass fraction is 1~2%；
(2) surface of whisker is modified：In parts by weight, by 20~60 parts of crystal whisker materials, 5~10 parts of surfactants, 1~5 part
The silane coupler dilution that defoamer and step (1) are prepared is poured into successively in the container for filling 100 parts of water, and stirring 20~
40min, then 20~40min of dispersion in ultrasonic wave is placed in, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation：In parts by weight, the modified crystal whiskers for step (2) being obtained are under the conditions of 100~150 DEG C
48~96h is dried, then dried modified crystal whiskers are blended with 10~25 parts of stabilizers, obtain described cementing slurry
With fiber reinforced dose.
10. preparation method according to claim 9, wherein, step (2) also includes：The Reusability distillation during suction filtration
Water rinses modified crystal whiskers crude product, to remove unnecessary surfactant, silane coupler and defoamer, obtains described being modified
Whisker.
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