CN106675537B - A kind of cementing slurry is with fiber reinforced dose and preparation method thereof - Google Patents
A kind of cementing slurry is with fiber reinforced dose and preparation method thereof Download PDFInfo
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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
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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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- 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 cementing slurries with fiber reinforced dose and preparation method thereof.In parts by weight, fiber reinforced dose of raw material composition includes: 20~60 parts of crystal whisker materials, 5~10 parts of surfactants, 5~10 parts of silane coupling agents, 1~5 part of defoaming agent, 10~25 parts of stabilizers, 100 parts of water, 250~1000 parts of dehydrated alcohols.This fiber reinforced dose the preparation method comprises the following steps: silane coupling agent to be made into the dilution of 1~2wt% with dehydrated alcohol；Crystal whisker materials, surfactant, defoaming agent and prepared silane coupling agent dilution are poured into the container for filling water, 20~40min is stirred, then is placed in 20~40min of dispersion in ultrasonic wave, obtains modified crystal whiskers after suction filtration；It will be blended after modified crystal whiskers drying with stabilizer, obtain fiber reinforced dose.Of the invention fiber reinforced dose can be dispersed in cement slurry, and having to the toughness of Behavior of Hardened Cement Paste preferably improves, and does not influence construction safety.
Description
Technical field
The present invention relates to a kind of cementing slurries with fiber reinforced dose and preparation method thereof, belongs to the oil of field of petroleum exploitation
Gas well cementing technical field.
Background technique
The permanently effective Inter-zonal packing ability of cement sheath is to realize the premise and oil gas of oil-gas field development volume increase in pit shaft
The guarantee of the long-term production life of well of well.However, well-cementing cement is a kind of fragile material for having congenital microdefect, with deformation
The inherent shortcomings such as ability is poor, tensile strength is low, impact resistance is poor.It is in subsequent construction such as pressure testing, perforation, pressure break and exploitation life
During producing etc., is influenced due to being changed by temperature, pressure, impacting, shake etc., easily rupture, cause the mechanics of cement sheath complete
Property destroyed, gently then cause that annular space is with pressure, oil gas water breakthrough in this way, it is heavy then oil/gas well is caused to be scrapped.
Currently, mostly using fiber in well cementation field to improve the mechanical property of Behavior of Hardened Cement Paste.Fiber can be between cement stone substrate
Play the role of " putting up a bridge ", hardened oilwell cement mechanical property is improved with the mode of action of " lacing wire ".
Common fibrous material has inorfil, such as glass fibre, carbon fiber in mortar architecture；Synthetic fibers, such as
The fibers such as nylon fiber, polyester, polypropylene；Plant fiber, such as bamboo fibre, flaxen fiber.However, there is also following for these fibers
Defect: first is that density is lower, dispersing not open after slurry, is suspended in slurry surface；Second is that surface hydrophobicity, wettability are poor, slurry
When it is easy to reunite, when pumping, easily blocks pipeline, causes to suppress pump, influences construction safety.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of cementing slurries with fiber reinforced dose and its
Preparation method.Of the invention fiber reinforced dose can be homogeneously dispersed in cement slurry, had to the toughness of Behavior of Hardened Cement Paste and preferably changed
It is kind, and do not influence construction safety.
In order to achieve the above objectives, present invention firstly provides a kind of cementing slurries with fiber reinforced dose, in parts by weight,
Its raw material composition include: 20~60 parts of crystal whisker materials, 5~10 parts of surfactants, 5~10 parts of silane coupling agents, 1~5 part disappear
Infusion, 10~25 parts of stabilizers, 100 parts of water and 250~1000 parts of dehydrated 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 is grown into, diameter is very small (the micron order of magnitude), without containing defect present in usual material (crystal boundary,
Dislocation, hole etc.), 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-intensitive, high-modulus and high elongation rate, is mainly used as compound
The reinforcement of material, for manufacturing high strength composite.
In above-mentioned cementing slurry in fiber reinforced dose, it is preferable that the crystal whisker materials include potassium titanate crystal whisker, boron
The combination of one or more of sour al whisker, magnesium sulfate crystal whisker, silicon carbide whisker and magnesium borate crystal whisker etc..
In above-mentioned cementing slurry in fiber reinforced dose, it is preferable that the length of the crystal whisker materials is 10-500 μm,
Diameter is 0.1-10 μm, draw ratio 1-5000.
In above-mentioned cementing slurry in fiber reinforced dose, it is preferable that the surfactant includes styryl benzene
The combination of one or more of phenol polyethenoxy ether, dodecyl sodium sulfate and aliphatic acid polyethenoxy ether etc..
In above-mentioned cementing slurry in fiber reinforced dose, it is preferable that the silane coupling agent include KH-550 and/or
KH-560 etc..
In above-mentioned cementing slurry in fiber reinforced dose, it is preferable that the defoaming agent includes tributyl phosphate etc..
In above-mentioned cementing slurry in fiber reinforced dose, it is preferable that the stabilizer includes ultrafine slag, hard charcoal
The combination of one or more of black, SILICA FUME, wollastonite in powder, nano silica and xanthan gum etc..
In above-mentioned cementing slurry in fiber reinforced dose, it is preferable that the water is distilled water.
Specific embodiment according to the present invention, it is preferable that above-mentioned cementing slurry is by following with fiber reinforced dose
Step preparation:
(1) preparation of silane coupling agent dilution: in parts by weight, by 5~10 parts of silane coupling agents with 250~1000 parts
Dehydrated 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~
5 parts of defoaming agents and the prepared silane coupling agent dilution of step (1) successively pour into the container for filling 100 parts of water, stirring 20
~40min, then it is placed in 20~40min of dispersion in ultrasonic wave, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are in 100~150 DEG C of items
Dry 48~96h under part, then the modified crystal whiskers after drying are blended with 10~25 parts of stabilizers, obtain the well cementation water
Mud is with fiber reinforced dose.
In above-mentioned preparation step, it is preferable that step (2) further include: Reusability distilled water flushing changes during suction filtration
Property whisker crude product to remove extra surfactant, silane coupling agent and defoaming agent obtain the modified crystal whiskers.
Whisker is a kind of chopped strand, has preferably wettability, through of the invention modified, can be homogeneously dispersed in
In cement slurry, there is preferable improvement to the toughness of Behavior of Hardened Cement Paste, and do not influence construction safety.
In the recovery process of petroleum, in order to increase production capacity, it is often necessary to be transformed to reservoir, acid fracturing is exactly it
The middle most effective also most common measure of one kind.Therefore require Behavior of Hardened Cement Paste and its composition material that there is the characteristic of acid corrosion-resistant, this
Invention uses one of potassium titanate crystal whisker, aluminium borate whisker, magnesium sulfate crystal whisker, silicon carbide whisker and magnesium borate crystal whisker or several
Kind combination, good acid resistance is all had, without using easily with the magnesium carbonate whisker etc. that chemically reacts of acid, being not necessarily to pair
Whisker carries out further cladding processing, that is, can reach the effect of acidproof corruption.
Crystal whisker materials cause it to disperse in the base since with ultra-fine size, surface can be bigger, and easy aggregation is agglomerating
Property is poor, and the dispersion of non-modified crystal whisker materials in water is shown in Fig. 1.The surfactant that the present invention uses can reduce
The surface energy of crystal whisker materials, disperses crystal whisker materials in the base more evenly；The defoaming agent of use is able to suppress because surface is added
Bubble problem caused by activating agent eliminates cement slurry because causing to make under cement strength due to accumulation is not close containing a large amount of bubbles
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. substances density it is relatively high, easily settled in cement slurry, lead to toughening material
Material disperses inhomogenous in cement slurry, to influence toughening effect, therefore uses stabilizer of the invention to solve the problems, such as this；Together
When, the part composition such as ultrafine slag, SILICA FUME etc. in stabilizer can also improve whisker-cement matrix interface performance, increase
Big matrix wraps up power to the bonding of whisker.The synergistic effect of fiber reinforced dose of each raw material, the fibre provided by through the invention
Dimension toughener is added in cementing slurry, can be homogeneously dispersed in cement slurry, to be effectively improved the power of hardened oilwell cement
Performance is learned, all has being greatly increased to the compression strength of hardened oilwell cement, tensile splitting strength, shock resistance, together
When reduce Behavior of Hardened Cement Paste Young's modulus, and do not influence construction safety.
On the other hand, the present invention also provides a kind of fiber reinforced dose of preparation method of above-mentioned cementing slurry,
The following steps are included:
(1) preparation of silane coupling agent dilution: in parts by weight, by 5~10 parts of silane coupling agents with 250~1000 parts
Dehydrated 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~
5 parts of defoaming agents and the prepared silane coupling agent dilution of step (1) successively pour into the container for filling 100 parts of water, stirring 20
~40min, then it is placed in 20~40min of dispersion in ultrasonic wave, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are in 100~150 DEG C of items
Dry 48~96h under part, then the modified crystal whiskers after drying are blended with 10~25 parts of stabilizers, obtain the well cementation water
Mud is with fiber reinforced dose.
In the above preparation method, it is preferable that step (2) further include: Reusability distilled water flushing changes during suction filtration
Property whisker crude product to remove extra surfactant, silane coupling agent and defoaming agent obtain the modified crystal whiskers.
Fiber reinforced dose of preparation process provided by the invention is simple, it is easy to accomplish industrialized production.This fiber reinforced dose
With preferably hydrophilicity, wettability in water is good, can be evenly dispersed in oil well cement paste, does not influence construction peace
Entirely.This fiber reinforced dose compression strength, tensile splitting strength, the shock resistance that can effectively improve hardened oilwell cement, simultaneously
Reduce Behavior of Hardened Cement Paste Young's modulus.
In conclusion fiber reinforced dose provided by the invention, there is preferably hydrophilicity, wettability in water
It is good, it can be evenly dispersed in oil well cement paste.By in fiber reinforced dose of addition cementing slurry of the invention, water will not influence
The working security of mud, and it can be effectively improved the mechanical property of hardened oilwell cement, compression strength, splitting to hardened oilwell cement
Tensile strength, shock resistance, which have, largely to be improved, while reducing Behavior of Hardened Cement Paste Young's modulus.Fiber provided by the invention
Toughener is suitable for oil gas well cementing operation operation, has broad application prospects.
Compared with the prior art with fiber reinforced dose, main advantage is cementing slurry provided by the invention:
(1) surface modification technology of whisker and fiber reinforced dose of preparation process are simple, it is easy to accomplish industrialized production；
(2) there is preferably hydrophilicity this fiber reinforced dose, wettability in water is good, can be evenly dispersed in oil
In cementing slurry for well, construction safety is not influenced；
(3) this fiber reinforced dose can effectively improve hardened oilwell cement compression strength, tensile splitting strength, shock resistance
Performance；
(4) after this fiber reinforced dose being added in cement, the characteristic for making cement have impact resistance strong, perforation is to water
The destruction of mud ring is small, fundamentally solves the problems, such as " secondary channelling ".
Detailed description of the invention
Fig. 1 is the dispersion figure of non-modified crystal whisker materials in water.
Fig. 2 is the fiber reinforced dose of dispersion figure in water that embodiment 1 provides.
Fig. 3 is the dispersion figure of traditional polymer fiber toughener in water.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
A kind of cementing slurry is present embodiments provided with fiber reinforced dose, through the following steps that being prepared:
(1) preparation of silane coupling agent dilution: in parts by weight, 5 parts of silane resin acceptor kh-550s are anhydrous with 500 parts
Ethyl alcohol 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, diameter is 0.1-1 μm, carbonization
Silicon wafer must length be 50-100 μm, diameter is 0.1-0.6 μm, the length of magnesium borate crystal whisker is 10-100 μm, diameter 0.1-
2.0 μm), 5 parts of surfactant styrylphenol polyoxyethylene ethers, 1 part of defoaming agent tributyl phosphate and step (1) prepare
Silane coupling agent dilution successively pour into the beaker for filling 100 parts of distilled water, stir 20min, then be placed in ultrasonic wave point
20min is dissipated, is then filtered, and the Reusability distilled water flushing modified crystal whiskers crude product during suction filtration, it is extra to remove
Surfactant, silane coupling agent and defoaming agent, obtain modified crystal whiskers；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are done under the conditions of 150 DEG C
Dry 48h, then by after drying modified crystal whiskers and 10 parts of stabilizers (it is made of 9 parts of wollastonites in powder, 1 part of xanthan gum) be total to
It is mixed, the cementing slurry is obtained with fiber reinforced dose, is denoted as XWZR-1.
Fiber reinforced dose of XWZR-1 provided in this embodiment is added to the water, dispersion 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, dispersion is as shown in Figure 3.It can be seen by the comparison of Fig. 2-3
Out, there is preferably hydrophilicity fiber reinforced dose provided in this embodiment, 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, through the following steps that preparation:
(1) preparation of silane coupling agent dilution: in parts by weight, 5 parts of silane resin acceptor kh-550s are anhydrous with 250 parts
Ethyl alcohol 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, diameter is 0.1-1.0 μm, carbon
The length of SiClx whisker is 50-100 μm, diameter is 0.1-0.6 μm, and the length of magnesium borate crystal whisker is 10-100 μm, diameter is
0.1-2.0 μm), 10 parts of surfactant sodium dodecyl base sodium sulfonates, 5 parts of defoaming agent tributyl phosphates and step (1) it is prepared
Silane coupling agent dilution successively pours into the beaker for filling 100 parts of distilled water, stirs 20min, then be placed in ultrasonic wave and disperse
Then 20min is filtered, and the Reusability distilled water flushing modified crystal whiskers crude product during suction filtration, extra to remove
Surfactant, silane coupling agent and defoaming agent, obtain modified crystal whiskers；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are done under the conditions of 120 DEG C
Dry 72h, then by after drying modified crystal whiskers and 25 parts of stabilizers (it is by 10 parts of ultrafine slags, 5 parts of white carbon blacks, 5 parts of SILICA FUMEs, 3
Part wollastonite in powder, 1 part of nano silica, 1 part of xanthan gum composition) it is blended, obtain the cementing slurry fiber
Toughener is denoted as XWZR-2.
Embodiment 3
A kind of cementing slurry is present embodiments provided with fiber reinforced dose, through the following steps that preparation:
(1) preparation of silane coupling agent dilution: in parts by weight, by 10 parts of silane coupling agent KH-560,1000 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
It is 0.1-1.0 μm, the length of aluminium borate whisker is 10-100 μm, diameter is 0.1-2.0 μm, and the length of silicon carbide whisker is 50-
100 μm, diameter be 0.1-0.6 μm, the length of magnesium sulfate crystal whisker is 10-60 μm, diameter is 0.1-1 μm), 5 parts of surfactants
Aliphatic acid polyethenoxy ether, 3 parts of defoaming agent tributyl phosphates and the prepared silane coupling agent dilution of step (1) successively pour into
In the beaker for filling 100 parts of distilled water, 20min is stirred, then be placed in ultrasonic wave and disperse 20min, then filtered, and taking out
Reusability distilled water flushing modified crystal whiskers crude product during filter, to remove extra surfactant, silane coupling agent and disappear
Infusion obtains modified crystal whiskers；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are done under the conditions of 130 DEG C
Dry 72h, then by after drying modified crystal whiskers and 20 parts of stabilizers (it is by 10 parts of SILICA FUMEs, 8 parts of wollastonites in powder, 1 part of nano-silica
SiClx, 1 part of xanthan gum composition) it is blended, the cementing slurry is obtained with fiber reinforced dose, is denoted as XWZR-3.
Embodiment 4
A kind of cementing slurry is present embodiments provided with fiber reinforced dose, through the following steps that preparation:
(1) preparation of silane coupling agent dilution: in parts by weight, by 10 parts of silane coupling agent KH-560,500 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
It is 0.1-1.0 μm for 10-100 μm, diameter, the length of aluminium borate whisker is 10-100 μm, diameter is 0.1-2.0 μm, magnesium sulfate
The length of whisker is 10-60 μm, diameter is 0.1-1.0 μm, and the length of silicon carbide whisker is 50-100 μm, diameter is 0.1-0.6 μ
M, the length of magnesium borate crystal whisker is 10-100 μm, diameter is 0.1-2.0 μm), 10 parts of surfactant fatty acid polyoxyethylene ether,
5 parts of defoaming agent tributyl phosphates and the prepared silane coupling agent dilution of step (1) successively pour into and fill 100 parts of distilled water
In beaker, 20min is stirred, then be placed in ultrasonic wave and disperse 20min, then filtered, and Reusability steams during suction filtration
Distilled water rinses modified crystal whiskers crude product, to remove extra surfactant, silane coupling agent and defoaming agent, obtains modified crystalline substance
Palpus；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are done under the conditions of 100 DEG C
Dry 96h, then by after drying modified crystal whiskers and 25 parts of stabilizers (its by 1 part of ultrafine slag, 1 part of white carbon black, 10 parts of SILICA FUMEs,
10 parts of wollastonites in powder, 2 parts of nano silicas, 1 part of xanthan gum composition) it is blended, it is fine to obtain the cementing slurry
Toughener is tieed up, XWZR-4 is denoted as.
(defoaming agent is not added, compare with embodiment 2) in comparative example 1
This comparative example provides a kind of cementing slurry with fiber reinforced dose, through the following steps that preparation:
(1) preparation of silane coupling agent dilution: in parts by weight, 5 parts of silane resin acceptor kh-550s are anhydrous with 250 parts
Ethyl alcohol 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, diameter is 0.1-1.0 μm, carbon
The length of SiClx whisker is 50-100 μm, diameter is 0.1-0.6 μm, and the length of magnesium borate crystal whisker is 10-100 μm, diameter is
0.1-2.0 μm), 10 parts of surfactant sodium dodecyl base sodium sulfonates and the prepared silane coupling agent dilution of step (1) successively
It pours into the beaker for filling 100 parts of distilled water, stirs 20min, then be placed in ultrasonic wave and disperse 20min, then filtered, and
The Reusability distilled water flushing modified crystal whiskers crude product during suction filtration, to remove extra surfactant and silane coupled
Agent obtains modified crystal whiskers；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are done under the conditions of 120 DEG C
Dry 72h, then by after drying modified crystal whiskers and 25 parts of stabilizers (it is by 10 parts of ultrafine slags, 5 parts of white carbon blacks, 5 parts of SILICA FUMEs, 3
Part wollastonite in powder, 1 part of nano silica, 1 part of xanthan gum composition) it is blended, obtain cementing slurry with fiber reinforced dose,
It is denoted as XWZR-5.
(stabilizer is not added, compare with embodiment 3) in comparative example 2
This comparative example provides a kind of cementing slurry with fiber reinforced dose, through the following steps that being prepared:
(1) preparation of silane coupling agent dilution: in parts by weight, by 10 parts of silane coupling agent KH-560,1000 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
It is 0.1-1.0 μm, the length of aluminium borate whisker is 10-100 μm, diameter is 0.1-2.0 μm, and the length of silicon carbide whisker is 50-
100 μm, diameter be 0.1-0.6 μm, the length of magnesium sulfate crystal whisker is 10-60 μm, diameter is 0.1-1 μm), 5 parts of surfactants
Aliphatic acid polyethenoxy ether, 3 parts of defoaming agent tributyl phosphates and the prepared silane coupling agent dilution of step (1) successively pour into
In the beaker for filling 100 parts of distilled water, 20min is stirred, then be placed in ultrasonic wave and disperse 20min, then filtered, and taking out
Reusability distilled water flushing modified crystal whiskers crude product during filter, to remove extra surfactant, silane coupling agent and disappear
Infusion obtains modified crystal whiskers；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are done under the conditions of 130 DEG C
Dry 72h obtains cementing slurry with fiber reinforced dose, is denoted as XWZR-6.
1 cement-slurry method of table and performance
Remarks: [1] is prepared according to API10A specification and measurement cement slurry；[2] tensile splitting strength is real by Brazil's splitting
Test obtains；[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 defoaming agent, XWZR-1, XWZR-2, XWZR-3, XWZR-4, XWZR-5, XWZR-6 are respectively embodiment 1-4 and comparative example 1-
Fiber reinforced dose of 2 preparations.
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 will not influence the workability of cement slurry, therefore the present invention mentions
For fiber reinforced dose of the cementing slurry brittleness that can effectively reduce Behavior of Hardened Cement Paste, so that it is guaranteed that the long term seal of cement sheath is complete
Property.
Claims (5)
1. a kind of cementing slurry is with fiber reinforced dose, in parts by weight, raw material composition includes: 20~60 parts of crystal whisker materials, 5
~10 parts of surfactants, 5~10 parts of silane coupling agents, 1~5 part of defoaming agent, 10~25 parts of stabilizers, 100 parts of water and 250
~1000 parts of dehydrated alcohols；
Wherein, the crystal whisker materials include potassium titanate crystal whisker, aluminium borate whisker, magnesium sulfate crystal whisker, silicon carbide whisker and boric acid
The combination of one or more of magnesium whisker；
The surfactant includes styrylphenol polyoxyethylene ether, dodecyl sodium sulfate and aliphatic acid polyethenoxy
The combination of one or more of ether；The defoaming agent includes tributyl phosphate；The stabilizer includes ultrafine slag, hard charcoal
The combination of one or more of black, SILICA FUME, wollastonite in powder, nano silica and xanthan gum；
Above-mentioned cementing slurry with fiber reinforced dose through the following steps that preparation:
(1) preparation of silane coupling agent dilution: in parts by weight, 5~10 parts of silane coupling agents are anhydrous with 250~1000 parts
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, 1~5 part
Defoaming agent and the prepared silane coupling agent dilution of step (1) successively pour into the container for filling 100 parts of water, and stirring 20~
40min, then it is placed in 20~40min of dispersion in ultrasonic wave, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are under the conditions of 100~150 DEG C
Dry 48~96h, then the modified crystal whiskers after drying are blended with 10~25 parts of stabilizers, obtain the cementing slurry
With fiber reinforced dose.
2. cementing slurry according to claim 1 is with fiber reinforced dose, wherein the length of the crystal whisker materials is 10-
500 μm, diameter is 0.1-10 μm, draw ratio 1-5000.
3. cementing slurry according to claim 1 is with fiber reinforced dose, wherein the silane coupling agent includes KH-550
And/or KH-560.
4. a kind of fiber reinforced dose of preparation method of described in any item cementing slurries of claim 1-3 comprising following
Step:
(1) preparation of silane coupling agent dilution: in parts by weight, 5~10 parts of silane coupling agents are anhydrous with 250~1000 parts
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, 1~5 part
Defoaming agent and the prepared silane coupling agent dilution of step (1) successively pour into the container for filling 100 parts of water, and stirring 20~
40min, then it is placed in 20~40min of dispersion in ultrasonic wave, modified crystal whiskers are obtained after suction filtration；
(3) fiber reinforced dose of preparation: in parts by weight, the modified crystal whiskers that step (2) is obtained are under the conditions of 100~150 DEG C
Dry 48~96h, then the modified crystal whiskers after drying are blended with 10~25 parts of stabilizers, obtain the cementing slurry
With fiber reinforced dose.
5. the preparation method according to claim 4, wherein step (2) further include: the Reusability distilled water during suction filtration
Modified crystal whiskers crude product is rinsed, to remove extra surfactant, silane coupling agent and defoaming agent, obtains the modified crystalline substance
Palpus.
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| CN110734753A (en) * | 2018-07-20 | 2020-01-31 | 中国石油化工股份有限公司 | wet mixing fiber for well cementation and preparation method thereof |
| CN109913186B (en) * | 2019-04-10 | 2019-12-17 | 陕西延长石油（集团）有限责任公司 | Petroleum drilling auxiliary and preparation method thereof |
| CN111574992B (en) * | 2020-05-27 | 2022-09-06 | 中国石油大学(华东) | Nano-phase permeability improver for acidizing and fracturing as well as preparation method and application of nano-phase permeability improver |
| CN112174568B (en) * | 2020-09-27 | 2022-03-04 | 嘉华特种水泥股份有限公司 | Modified toughening material for well cementation |
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| CN113429163B (en) * | 2021-06-17 | 2022-10-18 | 中国石油化工股份有限公司 | Cement composition for well cementation operation, cement slurry system and preparation method thereof |
| CN114525119A (en) * | 2022-02-21 | 2022-05-24 | 中国石油化工集团有限公司 | Preparation method of inorganic fiber toughening agent for oil-gas well cementing cement slurry |
| CN114854301B (en) * | 2022-03-25 | 2023-04-28 | 广东川奥高新科技有限公司 | Solvent-free polyurethane three-dimensional line pattern modeling runway surface layer and preparation method thereof |
| CN115925341B (en) * | 2022-12-20 | 2024-03-08 | 中国石油天然气集团有限公司 | Flexible self-healing cement slurry for well cementation of salt cavern gas storage and preparation method thereof |
| CN116218491B (en) * | 2023-05-09 | 2023-07-21 | 山东省地质矿产勘查开发局第二水文地质工程地质大队(山东省鲁北地质工程勘察院) | Hydrogel plugging agent, preparation method of hydrogel plugging agent and water-based drilling fluid |
| CN117659971B (en) * | 2024-01-31 | 2024-04-16 | 山东省地质矿产勘查开发局第二水文地质工程地质大队(山东省鲁北地质工程勘察院) | High-temperature-resistant cement slurry system for dry-hot rock cementing |
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