CN104592963B - The method that aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block - Google Patents

The method that aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block Download PDF

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CN104592963B
CN104592963B CN201510004504.5A CN201510004504A CN104592963B CN 104592963 B CN104592963 B CN 104592963B CN 201510004504 A CN201510004504 A CN 201510004504A CN 104592963 B CN104592963 B CN 104592963B
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aluminium
diatomite
closed pore
hollow ceramic
ceramic microspheres
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CN104592963A (en
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郭志东
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Shandong University of Technology
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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
    • C09K8/473—Density reducing additives, e.g. for obtaining foamed cement compositions
    • 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
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
    • 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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium

Abstract

The method that aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block,Include the preparation of aluminium diatomite closed pore hollow ceramic microspheres,Dispensing,Mixing,Stirring is sized mixing,By the wt% of G levels oil-well cement 55~65,Particle diameter is 10~50 μm of the wt% of aluminium diatomite closed pore hollow ceramic microspheres 25~35,20~50 μm of wt% of flyash 5~7 of particle diameter of loss on ignition 1.1%,The wt% of 99.9% calcium oxide of purity 1.5~2,The wt% of sodium sulphate 0.5~1.0 and micro- wt% of silicon 1~3 of 5~20 μm of particle diameter,Compound is sized mixing with 0.5~0.7 ratio of mud,A part pours into one group two pieces of length,It is wide,Height is respectively in 53mm*53mm*53mm die trials,Conserved respectively 24 hours in the water-bath curing box of 52 DEG C of constant temperature,48 hours,Soaked 1 hour in cold water after the demoulding,Carry out testing performance index.

Description

The method that aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block
Technical field
The present invention relates to the method that aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block, belong to material Technology is led.
Background technology
Domestic well cementation palliative uses the floating bead in flyash at present, includes heavy pearl and floating bead in flyash, heavy pearl is close Degree is in 1.1~2.8g/cm3, between, content accounts for flyash 30~70%, and floating bead is micro- less than the glass of water density in flyash Pearl, floating bead mainly include aluminosilicate glass microballon and porous carbon granule, and it is mainly micro- including thin-walled aluminosilicate glass to remove the floating bead after carbon granule Pearl, surfaces externally and internally is smooth, and volume is big, be it is a kind of it is rounded, light, closed pore is hollow, wear-resisting, high temperature resistant, thermal conductivity factor are small, intensity Height, floating bead amount account for the 0.5~1% of flyash total amount, and aluminosilicate glass microballon is hollow spherosome.
Floating bead wherein in flyash it be coal dust in thermal power plant boiler by 1100~1500 DEG C of burnings when, clayey Material melts spin at a high speed under the hot air acting of turbulent flow in stove into microlayer model, form perfectly round sial spheroid, burn and split The gas such as nitrogen, hydrogen and carbon dioxide, expands rapidly in the high temperature aluminum silicon ball body of melting caused by solution reaction, on surface In the presence of power, hollow glass envelope is formed, is cooled down rapidly subsequently into flue, after hardening, the glassy state for turning into high vacuum is empty Heart microballon, i.e. fly ash float.
Flyash is put into water and stirred, a period of time is stood, because floating bead density is less than water density, the water surface will be swum in On pull out and dry, as floating bead, the floating bead in flyash is canescence, main component SiO2Account for 70% and AI2O313% is accounted for, is burnt Vector is 0.40%~0.574%, 0.475~0.574g/cm of density3, 1.44~5.41 μm of wall thickness, particle size range is mainly distributed At 147~84 μm.
In recent years, due to the influence of northern haze weather, the big-and-middle-sized thermal power generation in China uses the desulfurization technology of environmental protection, Floating bead is free of in flyash, causes in short supply, only middle small coal power plants and arcola do not use desulfurization technology supply A small amount of floating bead, the in short supply of floating bead cause rise in price, and floating bead is impure is mixed with flyash, influence cementing quality.
In reinforcing oil well field, hydrocarbon distribution is wide, and long shut-in well is more and more, and the long main use of shut-in well is light weight cement Well cementation, long shut-in well mainly use low-density cement mortar, and the density for wanting to make cement mortar is in 1.0 g/cm3~1.5 g/cm3Between, The lightening material of non-floating bead（Inorganic mineral material and organic synthesis material composition）Density must be in 0.5 g/cm3~0.85 g/ cm3Between, the well cementation test block of high-temperature-resistant high-pressure-resistant can be just made, the density of G level oil well watertights is in 3.1 g/cm3, palliative is close Degree is necessarily less than 0.5 g/cm3~0.85 g/cm3Density 1.0g/cm can just be configured3~1.5 g/cm3Between cement mortar, it is preceding The condition of carrying is 40% of palliative addition no more than total amount, otherwise can influence the compression strength of cement briquette.
The content of the invention
It is an object of the invention to overcome state of the art, the breach of new technology is found out, there is provided a kind of cost is low, property Can be excellent, the pearl of floaing in flyash can be replaced, function admirable, density is determined rate of change less than 0.02, passes through the method for synthesis Make aluminium diatomite closed pore hollow ceramic microspheres, the g/cm of density range 0.503~0.85g/cm3, and then configure low-density 1.0 g/cm3~1.5g/cm3The preparation method of high-temperature-resistant high-pressure-resistant oil well cementing test block, meet long shut-in well well cementing material requirement.
Its technical scheme is.
The method that aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block, including aluminium diatomite closed pore are empty Preparation, dispensing, mixing, the stirring of heart ceramic fine bead are sized mixing, die trial, performance test, sial diatomite closed pore hollow ceramic microspheres Performance test includes its floatability measure, density measurement, the measure of resistance to hydrostatic pressure intensity, serum density measure, sedimentation stability, thick Change time, drop fluid loss, pressure-resistant density test, the liquidity scale, compressive property test；
Comprise the following steps：
A, the preparation of aluminium diatomite closed pore hollow ceramic microspheres：
The first step, dispensing：10~20 μm of diatomite of particle diameter, 10~30 μm of aluminium powders are taken, percentage by weight is：85~90wt%： 10~15 wt%；
Second step, base：10~20 μm of diatomite of particle diameter, 10~30 μm of aluminium powders are taken, percentage by weight is：85~90wt%： 10~15 wt%；Mixed powder is mixed to get by the percentage by weight sampling of the first step, stirs, takes 10~20 μm of diatoms of particle diameter Soil, 10~30 μm of aluminium powders mixed powder in add phenolic resin, ratio is：1.0 wt%：0.5~0.8wt%, take particle diameter 10~20 μm diatomite, 10~30 μm of aluminium powders and phenolic resin are mixed evenly, and the curing process at a temperature of 50~100 DEG C, will solidify Body is crushed in flour mill, obtains 10~30 μm of mixed powders of particle diameter, and mixed powder is put into mould, on forcing press apply 3~ 5MPa pressure, extrusion forming obtain blank；
3rd step, fire：Second step is obtained into blank to be put into sintering furnace, in the time of 1500~1600 DEG C of heat preservation sinterings For 6~8 hours, aluminium diatomite block is obtained；Aluminium diatomite block is obtained, because diatomite contains up to 78% silica, Add aluminium powder increase composite in aluminium content, enhancing well cementation palliative performance, as well cementation mitigate agent material, its into Point it must is fulfilled for silica and more than 75%, aluminum oxide is more than 12%, calcium oxide and is more than 1.0%, iron oxide to be more than 1.0%, magnesia More than 0.5%, the compression strength for palliative of cementing the well depends primarily on the content of vitreous content, i.e. silica；
The making of 4th step, aluminium diatomite solid ceramic microbeads：3rd step is obtained into aluminium diatomite block on balling machine The solid ceramic microbeads of 5~20 μm of aluminium diatomite spherical shapes of particle diameter are processed into, 5~20 μm of particle diameter is processed on balling machine The solid microbeads of aluminium diatomite spherical shape, balling machine are not jaw crushers, jaw crusher be using metal accelerating impact or Material is tapped, the material shapes of formation are the irregular shapes such as sheet, more prismatics, and nodularization processing is that blower fan blows afloat material, thing Rotary motion phase mutual friction between material is in spherical shape microballon, and the microballon of spherical shape is uniform in each particle stress distribution, resistance to compression Intensity is big；Sheet, more prismatic high-temperature expansion sintered shapes are still original shape, and irregular shape is in through high-temperature expansion sintering Cuttlefish fish head shape, compression strength is low, and grinding stranding one with two fingers crushes, and the density of broken rear slurry can increase, and the ratio of mud also increases Adding, setting time length, test block shrinkage ratio is big, causes blind hole, flat impossible Cheng Yuan's, and nodularization is different with attrition crushing principle, The performance of microballon is also different；
5th step, aluminium diatomite slurries make：The percentage of aluminium diatomite slurry forms：5~20 μm of aluminium diatoms of particle diameter The native wt% of solid ceramic microbeads 65~70：The wt% of water 30~35, mix size mixing in proportion；
6th step, foaming agent add：Foaming agent, calcium carbonate, sulfuric acid are added in the aluminium diatomite slurries made to the 5th step One kind in potassium or sodium sulphate, concentration are 1~3g/L；
It is prepared by the 7th step, aluminium diatomite closed pore hollow ceramic microspheres：6th step mixed serum is sufficiently stirred filtering, used High-pressure injection high speed centrifugation rotary spraying technique, microballoon is formed, by dehydration expansion, high temperature on the oxygenation gas furnace of zonal control Sintering, melt surface vitreous, balling-up, classification is selected to obtain 10~50 μm of aluminium diatomite closed pore hollow ceramic microspheres by Feng Li Cheongju, Aluminium diatomite closed pore hollow ceramic microspheres wall thickness is at 10~20 μm, and compression strength is in 100~180MPa, using high-pressure injection at a high speed Centrifugal rotation spray-on process, microballoon is formed, melted on the oxygenation gas furnace of vertical zonal control by expansion, high temperature sintering, surface Melt vitreous, balling-up, the concentration of oxygen is 30~35%, and the concentration of oxygen is higher, and burning-point is lower, and burn more abundant, the heat of release More, temperature is higher, and wherein 800~900 DEG C of expansion temperature, drying sintering temperature are in 1200~1250 DEG C, melt surface temperature 1300~1350 DEG C, 1100~1200 DEG C of balling-up temperature, classification is selected to obtain 10~50 μm of aluminium diatomite closed pores by Feng Li Cheongju empty Heart ceramic fine bead, using high-pressure pump from slurry extract body is mixed, centrifugal rotation spraying machine is delivered to by slurry is mixed through over pressurizeed, The rotating speed of high speed centrifugation motor is at 24000 revs/min, and for motor high temperature resistant at 1800 DEG C, rotation at a high speed produces larger centrifugal force Microballon is formed, the size of microballon is relevant with injection aperture, pressure and speed, and dehydration expansion temperature more highly expanded volume is bigger, with Temperature height is relevant, and melt surface temperature could form aluminium diatomite closed pore hollow ceramic microspheres, mineral matter by 900 DEG C with On high temperature sintering after produce activity, be also easy to produce hydration reaction, generate spawn, early strength is improved, such as quick lime, powder Coal ash, silica flour etc., in addition, particle diameter is smaller, bigger than surface, activity is bigger, and reaction speed is fast, and the composition of floating bead is by coal Composition determined, the size of particle diameter can not manual control, therefore the floating bead performance in flyash can not change, i.e. wall thickness, particle diameter Size and compression strength can not change, high-pressure injection high speed centrifugation rotary spraying technique can control the big of the particle diameter of microballon Small, wall thickness and compression strength, and the floating bead wall thickness in flyash is less than 6 μm, the MPa of maximum compressive strength 20, performance indications people It is relevant with material performance itself for that cannot control, raw material palliative used in preparation high temperature resistant, high pressure well cementation test block, such as Closed pore hollow ceramic microspheres and various well cementation mitigate the performance of agent material, performance indications such as wall thickness, density, sphericity, floating Rate, compression strength, opening and closing hole, particle size, it is necessary to it is artificial controllable, meet These parameters, palliative wide adaptation range of cementing the well, separately Outside, ceramic material property exceedes alloy material, is widely used in the fields such as space flight, military project, machinery, passes through artificial synthesized method Prepare, cost is low, and performance is high；
8th step, testing performance index：
A, its floatability determines：10~50 μm of aluminium diatomite closed pore hollow ceramic microspheres of particle diameter are weighed, 100 grams are poured into 1000 millis In the beaker risen, then pour into 500 milliliters of running water and fall in beaker, stirred with glass bar, stand 1 hour, floated in beaker Aluminium diatomite closed pore hollow ceramic microspheres be floating bead, be precipitated as heavy pearl in beaker bottom, floating bead in beaker and heavy pearl distinguished Take out and dry and weigh, calculate its floatability, its floatability of the aluminium diatomite closed pore hollow ceramic microspheres in water is more than 98%, aluminium silicon The density domination of diatomaceous earth palliative is in rational density range, i.e. 0.5g/cm3~0.85 g/cm3Between, if sintering time The aluminium diatomite closed pore hollow ceramic microspheres that short, proportion is more than water precipitate, and broken aluminium diatomite closed pore hollow ceramic microspheres are inhaled Water sedimentation；
B, the density of aluminium diatomite closed pore hollow ceramic microspheres is measured：100 milliliters of volumetric flask is taken to weigh to obtain G1, then by aluminium Diatomite closed pore hollow ceramic microspheres are poured into 100 milliliters of volumetric flasks, aluminium diatomite closed pore hollow ceramic microspheres concave surface and 100 millis It is tangent to rise the graduation mark of volumetric flask, weighs aluminium diatomite closed pore hollow ceramic microspheres and restores G with bottle2, 100 milliliters of aluminium diatomite close Hole hollow ceramic microspheres nt wt net weight is G2- G1, m=ρ V are obtained by quality, density and volume, density p=（G2- G1）/ V, according to resistance to The cementing requirements of HTHP test block, the density of test block is in 1.0~1.5g/cm3, and aluminium diatomite closed pore hollow ceramic microspheres are close Degree is in 0.5g/cm3~0.85 g/cm3In the range between；
C, the measure of resistance to hydrostatic pressure intensity：Weigh 100 grams of aluminium diatomite closed pore hollow ceramic microspheres and pour into hydrostatic pressing intensity In test tube, hydrostatic pressing intensity test tube is connected with compression pump, and the water in compression pump is stressed in hydrostatic pressing intensity test tube, record pressure Force value, stop the aluminium diatomite closed pore hollow ceramic microspheres that pressurization is taken out in test tube and measure its floatability, after the 100MPa that pressurizes, take out Aluminium diatomite closed pore hollow ceramic microspheres measure its floatability, if the aluminium diatomite closed pore hollow ceramic microspheres its floatability after pressurization It is consistent with uninflated aluminium diatomite closed pore hollow ceramic microspheres its floatability, show that aluminium diatomite closed pore hollow ceramic microspheres are resistance to quiet The intensity of hydraulic pressure is more than 120 MPa, and it is strong to measure numerical value, the resistance to hydrostatic pressure such as 150MPa, 160 MPa, 180 MPa with same method Degree is aluminium diatomite closed pore hollow ceramic microspheres compression strength, and the intensity of aluminium diatomite closed pore hollow ceramic microspheres resistance to hydrostatic pressure exists 120~200 MPa；And the maximum hydrostatic pressing intensity of fly ash float detection is 20 MPa, wall thickness is less than 6 μm, and particle diameter is more than 80 μ M, the compression strength of test block depend on the compression strength of floating bead, and the floating bead in flyash is not suitable for consolidating for HTHP oil well Well, that is, it is not suitable for less than 4000 meters, the well cementation of oil well of the temperature more than 150 DEG C, is suitable only for more than 2000 meters, temperature is less than The well cementation of 90 DEG C of oil well, it is well known that ceramic material is widely used in the fields such as space flight, chemical industry, machinery, ceramic material resistance to compression The performance indications such as intensity are considerably beyond synthesis metal material, therefore aluminium diatomite closed pore hollow ceramic microspheres can be used for high temperature high pressure oil Human controllable, the other materials such as the well cementation of well, ceramic material compression strength in manufacturing process, wall thickness, particle diameter are incomparable；
D, the variable density value of aluminium diatomite closed pore hollow ceramic microspheres is detected：The sample point of same batch diverse location The variable density scope of aluminium diatomite closed pore hollow ceramic microspheres is in ± 0.01 g/cm3, then the density of sample point sample should control In 0.69 g/cm3~0.71g/cm3Between, high-temperature-resistant high-pressure-resistant oil well refers to oil well operation face temperature at 150~240 DEG C, Oil well of the depth of oil well below 4000 meters, compression strength depend on aluminium in 60~100MPa, the compression strength for test block of cementing the well The compression strength of diatomite closed pore hollow ceramic microspheres, low pressure oil well refer to compression strength and are less than 20 MPa, temperature at 70~90 DEG C, Middle force feed well refers to compression strength and refers to compression strength more than 60~100 in 90~150 DEG C of high pressure oil wells in 20~60MPa, temperature MPa, the temperature in oil well be surface temperature plus oil well often decline 100 meters of temperature increase by 3 DEG C of values with；
B, aluminium diatomite closed pore hollow ceramic microspheres prepare high-temperature-resistant high-pressure-resistant oil well cementing test block：
The first step, dispensing：The wt% of G levels oil-well cement 55~65, particle diameter is hollow for 10~50 μm of aluminium diatomite closed pore The wt% of ceramic fine bead 25~35,20~50 μm of wt% of flyash 5~7 of particle diameter of loss on ignition 1.1%, the calcium oxide 1.5 of purity 99.9% ~2 wt%, the wt% of sodium sulphate 0.5~1.0 and the micro- wt% of silicon 1~3 of 5~20 μm of particle diameter, configure the pH value of slurries 8.0~ Between 10.5；G oil-well cements particle diameter and aluminium diatomite closed pore hollow ceramic microspheres particle size are variant, using loss on ignition 1.1% Flyash, according to accumulation principle, flyash mainly fills up two kinds of G oil-well cements and aluminium diatomite closed pore hollow ceramic microspheres Space between material particle size, when the different particle of particle diameter is tangent two-by-two, the gap between tangent circle is filled by flyash, makes G oil wells Cement and glass microballoon grain are combined closely, but 5~7 % within the specific limits, that is, controlled in gross weight should be controlled in usage amount In the range of, otherwise, the intensity of high temperature high voltage resistant test block is influenceed, next to that the flyash generated by high temperature sintering, active, The hydration rate of slurries is significantly improved, the low flyash of loss on ignition needs the ratio of mud small, contributes to the early strong of test block of cementing the well, purity 99.9% calcium oxide, calcium oxide purity is higher, and activity is stronger, and hydration rate is fast, discharges during calcium oxide hydration reaction substantial amounts of Heat, and gelatinous material calcium hydroxide is generated, beneficial to the early strong of high temperature high voltage resistant slurries, temperature rises by force important to the morning of test block Effect, the calcium hydroxide secondly generated after aquation can adjust the pH value of high temperature high voltage resistant slurries, in alkalescent bar in alkalescence Under part, the early strength of high-temperature-resistant high-pressure-resistant oil-well cement can be improved, sodium sulphate is a kind of fluid loss agent, and drop dehydration effect is bright It is aobvious, the sodium ion in sodium sulphate, there is counter-infiltration function, diffusion velocity is fast, slurries is separated out part water, sodium sulphate in solidification How much is dosage, and the drop dehydration to slurries plays an important role, and rationally drops dehydration and is advantageous to the early strong of high temperature high voltage resistant Behavior of Hardened Cement Paste, if resistance to It is excessive that dehydration drops in HTHP slurries in solidification, and high temperature high voltage resistant well cementation test block amount of contraction is big, causes blind hole, influences matter of cementing the well Amount, for sodium sulphate compared with other fluid loss agents, sodium ion diffusivity is strong, spreads uniformity, and cost is low, significant effect, according to Accumulation principle, the gap that SILICA FUME is mainly filled up between G oil-well cements and aluminium diatomite closed pore hollow ceramic microspheres and flyash, With greater activity, spawn is formed, improves the intensity of high temperature high voltage resistant slurries, increases dioxide-containing silica and slurries Suspension stability and Behavior of Hardened Cement Paste high temperature resistance are indispensable technical conditions, above-mentioned several additions and must control dosage；
Second step, make high-temperature-resistant high-pressure-resistant oil well cementing test block：It is mixed to get by the percentage by weight sampling of the first step Mixed powder, stir, sized mixing with 0.5~0.7 ratio of mud, slurries are aspirated by liquid pump, are sprayed to high speed revolving drum Outer surface, produce centrifugal force in outer surface of cylinder and shed slurries, Stirring is shed in realization, pours into one group of two pieces of length Respectively in 53mm*53mm*53mm die trials, conserve 24 hours, 48 hours, take off respectively in the water-bath curing box of 52 DEG C of constant temperature Soaked 1 hour in cold water after mould, carry out testing performance index, if water usage amount more than 0.5~0.7 scope, during grout cures Between it is long, early strength is low, drop dehydration it is excessive, test block drop dehydration be more than 50ml/30min, test block amount of contraction is big, causes blind hole, shadow Ring cementing quality；
3rd step, testing performance index：
A, serum density determines：Take second step to make slurries, pour into and density g/cm is weighed in fluid densitometer3, high temperature resistant, The density of high pressure slurries is in 1.0~1.5g/cm3Between；High temperature resistant, the density of high pressure resistant slurries are in 1.0~1.5g/cm3Between, Test block rate of change of the density is less than 0.02 g/cm3, according to ρ=m/V formula, weigh up the weight G of test block1, according to volume V1, calculate close Spend ρ1, test block is put on forcing press and pressurizeed, weighs up the weight G of test block2, according to volume V2,Calculate density p2, rate of change of the density is （ρ2-ρ1）/ρ1, rate of change of the density, which is less than, illustrates that well cementation test block anti-pressure ability is strong, V after pressurization2Volume Changes are small, density p2Change It is small；
B, the pH value measure of slurries：Take second step to make slurries, pour into pH value tester, show pH value, the pH of slurries Value is between 8.0~10.5；
C, sedimentation stability：Take second step to make slurries and pour into settlement barrel, observe homogeneity after 0.5 hour, stability, One property is that aluminium diatomite closed pore hollow ceramic microspheres mutually merge with slurries, and no longer floating fluctuation, microballon are evenly distributed on up and down In slurries；
D, the test of the performance and dosage of well cementing material：Base-material, i.e. G levels oil well superfine cement, palliative are floating bead or closed Hole hollow ceramic microspheres, additive, additive refer to the material beyond base-material and palliative, measurement density, wall thickness, sphericity, close Hole, particle size, hydration reaction speed, particle diameter is measured with particle instrument；
E, the thickening time：Vary with temperature obvious, also relevant with additive addition quantity species, the record thickening time；
F, intensity test：Conserved respectively 24 hours, 48 hours in the water-bath curing box of 52 DEG C of constant temperature, well cementation examination Clotting is consolidated, and one piece of well cementation test block therein is taken out after 24 hours, is put on forcing press and carries out applied voltage test, calculate variable density Rate, another piece of cement briquette is taken out after 48 hours and carries out pressure test, with the extension of time, the compression strength of well cementation test block increases Add, calculate the rate of change of density, high temperature resistant, the density of high pressure slurries are in 1.0~1.5g/cm3Between, test block rate of change of the density is small In 0.02 g/cm3, according to ρ=m/V formula, weigh up the weight G of test block1, according to volume V1, calculate density p1, test block is put into Pressurizeed on forcing press, weigh up the weight G of test block2, according to volume V2,Calculate density p2, rate of change of the density is（ρ2-ρ1）/ρ1, density Rate of change, which is less than, illustrates that well cementation test block anti-pressure ability is strong, V after pressurization2Volume Changes are small, density p2Change is also small；
The restriction of 4th step, other performance index：
A, high-temperature-resistant high-pressure-resistant oil well refers to oil well operation face temperature at 150~240 DEG C, and the depth of oil well is at 4000 meters Following oil well, the compression strength for test block of cementing the well is in 60~100MPa；
B, because high-temperature-resistant high-pressure-resistant oil well operation face temperature is at 150~240 DEG C, conventional additive is early strength agent, divided Powder, fluid loss agent, coagulant, defoamer must mark use range, and temperature rise additive decomposition is ineffective, if do not had There is special instruction, conventional additive is all low form, and the temperature used will fail below 90 DEG C more than 90 DEG C；
C, the restriction of palliative and additional agent content：Palliative refers to the addition of aluminium diatomite closed pore hollow ceramic microspheres Amount should be less than 35%, and the necessary heatproof of additive is more than 300 DEG C, and addition controls within the specific limits, i.e. the fine coal of loss on ignition 1.1% 5~7wt% of ash, the 1.5~2wt% of calcium oxide of purity 99.9%, 0.5~1.0wt% of sodium sulphate and micro- 1~3wt% of silicon, well cementing material can It is divided into：Base-material is that G level oil wells superfine cement, palliative i.e. floating bead and closed pore hollow ceramic microspheres, additive, additive refer to base-material With the material beyond palliative, G level oil wells superfine cement, aluminium diatomite hole hollow ceramic microspheres particle diameter, the burning of flyash The index such as vector and activity, the pH value of slurries, G level oil wells superfine cement, aluminium diatomite hole hollow ceramic microspheres, loss on ignition 1.1% flyash, the calcium oxide of purity 99.9%, micro- silicon are all by the material of more than 900 °C of high-temperature firing, salt sodium sulphate 884 DEG C of fusing point, it is not easily decomposed in HTHP oil well, stability is strong, using the flyash of loss on ignition 1.1%, loss on ignition Low, phosphorus content is low, and sintering is abundant, and activity is high, and hydration reaction speed is fast, and it is fast to form gelatinous material speed, former according to accumulation Reason, flyash mainly fill up space between two kinds of material particle sizes of G oil-well cements and closed pore hollow glass micropearl, different of particle diameter When grain is tangent two-by-two, the gap between tangent circle is filled by flyash, makes G oil-well cements and the hollow glass of aluminium diatomite closed pore Microballon grain is combined closely, but should be controlled and within the specific limits, that is, be controlled in the range of 5~7 % of gross weight in usage amount, no Then, the intensity of test block is influenceed, next to that the flyash generated by high temperature sintering, active, the hydration rate of slurries is accelerated, Contribute to the early strong of test block of cementing the well, the calcium oxide of purity 99.9%, calcium oxide purity is higher, and activity is stronger, and hydration rate is fast, oxidation Substantial amounts of heat is discharged during calcium hydration reaction, raises the temperature of slurries, and generates gelatinous material calcium hydroxide, beneficial to examination Block it is early strong, the calcium hydroxide secondly generated after aquation can adjust the pH value of slurries, under weak basic condition, i.e., in alkalescence PH value can improve the early strength of oil well test block between 8~10.5, and sodium sulphate is a kind of fluid loss agent, and drop dehydration effect is bright It is aobvious, the sodium ion in sodium sulphate, there is counter-infiltration function, diffusion velocity is fast, slurries is separated out part water, sodium sulphate in solidification How much is dosage, and the drop dehydration to slurries plays an important role, and rationally drops dehydration and is advantageous to the early strong of Behavior of Hardened Cement Paste, if slurries are in solidification It is excessive that dehydration drops, and well cementation test block amount of contraction is big, causes blind hole, influences cementing quality, sodium sulphate is compared with other fluid loss agents, sodium Ionic diffusion is strong, spreads uniformity, cost is low, significant effect, and additive must control usage amount, flyash dosage mistake Greatly, cement the well test block compression strength reduce, density increase, the ratio of mud increase, i.e., water consumption increase, drop dehydration increase, it is impossible to use Additive replaces palliative, and base-material oil-well cement can not be replaced with additive, loses the intensity of test block, can increase the close of slurries Degree, compression strength reduce, or even well cementation test block does not have compression strength and rupture strength, and palliative and additive must control use Amount, need to particularly indicate that use range and condition, although some additives have similar function to the above-mentioned additive used, make Environment is different, and use environment, which changes additive, will lose function, conventional additive such as early strength agent, fluid loss agent, promote to coagulate Agent is low form, used below at 90 DEG C, is otherwise failed, and other additives such as flyash, calcium oxide, micro- silicon etc. must limit The indexs such as purity, composition, color, addition, the scope that uses, carry out parametrization demarcation, i.e., cement the well and try for high temperature high voltage resistant Block, more than 4000 meters, temperature in use at 150~240 DEG C, test block pressure resistance intensity prepares high temperature resistant in 60~100MPa for well cementation The aluminium diatomite bead density of high pressure well cementation test block is in 0.5g/cm3~0.85 g/cm3Between, and flyash, silica flour, bentonite, Zirconium oxide, diatomite, sepiolite antisaline soil isodensity are all in 2.0 g/cm3More than, it is impossible to density is prepared in 1.0~1.5g/cm3 Between slurries, generally by 1.0~1.5g/cm3Between be high temperature high voltage resistant slurries, 1.6 g/cm3~1.7 g/cm3For resistance to medium temperature Middle mud jacking liquid, 1.8 g/cm3~1.9 g/cm3For low-temperature low pressure resistance slurries, and G levels oil well superfine cement density 3.0~ 3.3g/cm3, density uses weighted average calculation.
The method that described aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block, the high temperature of preparation are high Pressure well cementation test block drop fluid loss is less than 50mL/30min.
The microballon of closed pore must be used, the hollow glass micropearl of perforate mitigates agent material as oil well cementing, with G levels oil A certain proportion of water is added after well cement mixing, hydrone is entered in hollow glass microballoon by micropore, makes unit volume The increase of perforate hollow glass micropearl quality, causes hollow glass micropearl density to increase, and ratio of mud increase, the density of cement mortar also becomes Greatly, i.e. water consumption increase, in process of setting, the thickening time increases, Behavior of Hardened Cement Paste tries fast early strength reduces, drops dehydration cement mortar Increase, excessive, anti-pressure ability reduction is shunk in Behavior of Hardened Cement Paste examination soon, easily causes the blind hole accident of oil well, in addition, closed pore hollow ceramic is micro- The compression strength of pearl is much larger than the compression strength of perforate hollow ceramic microspheres, in addition, its performance of material difference is also different, difference is matched somebody with somebody It is also more different than its effect, it is impossible to the material of certain single component compared with composite, without comparativity, even identical material Material, proportioning is the same, and the succession of mixing changes, and its performance is still more the ratio of different materials there is also a world of difference Compared with without comparativity.
The present invention has advantages below.
1st, the dependence to flyash floating bead in long-term well cementation, density, wall thickness, the sintering temperature of ceramic fine bead can be changed Degree can control.
2nd, the technical matters is advanced, and technology maturation, properties of product are stable, and production cost is low, and yield is high, and performance is good, opens up Well cementation synthesis virgin material new way.
3rd, aluminium diatomite ceramic fine bead density is in 0.50 g/cm3~0.85g/cm3, filled out according to the theoretical SILICA FUME that adds of accumulation Void among particles are filled, dioxide-containing silica is high, increases Behavior of Hardened Cement Paste high temperature resistance, and G levels oil-well cement, ceramic fine bead pass through 1000 DEG C high temperature above sintering has greater activity, and hydration reaction is fast, can form jelly, can improve early strength.
4th, expansion, high temperature sintering, melt surface vitreous, balling-up are passed through on the oxygenation gas furnace of zonal control, oxygen Concentration is 30~35%, and the concentration of oxygen is higher, and burning-point is lower, and burning is more abundant, and the heat of release is more, and temperature is higher, adopt With high-pressure injection high speed centrifugation rotary spraying technique, liquid enters body of heater after being fully atomized, drop is in breathing space expanded by heating, expansion Volume is relevant with expansion temperature and density of foaming agent, then sintered, melting, last balling-up, prevents that tying wall adopts to improve yield With thermal cycle extract system, blower fan uses frequency controlling fan.
Embodiment
Embodiment.
Preparation, dispensing, mixing, stirring including aluminium diatomite closed pore hollow ceramic microspheres are sized mixing, die trial, performance test, Aluminium diatomite closed pore hollow ceramic microspheres performance test includes its floatability measure, density measurement, the measure of resistance to hydrostatic pressure intensity, slurry Liquid density measurement, sedimentation stability, thickening time, drop fluid loss, pressure-resistant density test, the liquidity scale, compressive property test.
Comprise the following steps.
A, the preparation of aluminium diatomite closed pore hollow ceramic microspheres.
The first step, dispensing：10 μm of diatomite of particle diameter, 15 μm of aluminium powders are taken, percentage by weight is：85~90wt%：10~15 wt%；
Second step, base：10 μm of diatomite of particle diameter, 15 μm of aluminium powders are mixed to get by the percentage by weight sampling of the first step Mixed powder, stir, by 10 μm of diatomite of particle diameter, 15 μm of aluminium powders mixed powder in add phenolic resin, ratio is：1.0 wt%：0.5 wt%, 10 μm of diatomite of particle diameter, 15 μm of aluminium powders and phenolic resin will be taken to be mixed evenly, it is solid at a temperature of 60 DEG C Change is handled, and firming body is crushed in flour mill, obtains 10 μm of mixed powders of particle diameter, compound is put into mould, on forcing press Apply 1.5MPa pressure, extrusion forming obtains blank.
3rd step, high-temperature firing：Second step is obtained into blank to be put into high temperature sintering furnace, at 1500 DEG C,
The time of heat preservation sintering is 8 hours, obtains aluminium diatomite block.
The making of 4th step, aluminium diatomite solid microbeads：3rd step is obtained into aluminium diatomite block to process on balling machine The full particle of 10 μm of aluminium diatomite spherical shapes of particle diameter is made.
5th step, aluminium diatomite slurries make：The percentage of aluminium diatomite slurry forms：10 μm of aluminium diatomite 70 of particle diameter wt%：The wt% of water 30..
6th step, foaming agent add：Foaming agent calcium carbonate is added in the aluminium diatomite slurries made to the 5th step, concentration is 2.5g/L。
It is prepared by the 7th step, aluminium diatomite closed pore hollow ceramic microspheres：6th step mixed serum is sufficiently stirred filtering, used High-pressure injection high speed centrifugation rotary spraying technique, microballoon is formed, by dehydration expansion, high temperature on the oxygenation gas furnace of zonal control Sintering, melt surface vitreous, balling-up, classification is selected to obtain 30 μm of aluminium diatomite closed pore hollow ceramic microspheres, aluminium silicon by Feng Li Cheongju Diatomaceous earth closed pore hollow ceramic microspheres wall thickness is at 30 μm, and compression strength is in 150MPa.
8th step, testing performance index.
A, its floatability determines：Weigh 30 μm of 100 grams of aluminium diatomite closed pore hollow ceramic microspheres of particle diameter and pour into 1000 milliliters In beaker, then pour into 500 milliliters of running water and fall in beaker, stirred with glass bar, stand 1 hour, the aluminium floated in beaker Diatomite closed pore hollow ceramic microspheres are floating bead, and heavy pearl is precipitated as in beaker bottom, and floating bead in beaker and heavy pearl are taken out respectively And dry and weigh, its floatability is calculated, its floatability of the aluminium diatomite closed pore hollow ceramic microspheres in water is more than 98%.
B, the density of aluminium diatomite closed pore hollow ceramic microspheres is measured：100 milliliters of volumetric flask is taken to weigh to obtain G1, then by aluminium Diatomite closed pore hollow ceramic microspheres are poured into 100 milliliters of volumetric flasks, aluminium diatomite closed pore hollow ceramic microspheres concave surface and 100 millis It is tangent to rise the graduation mark of volumetric flask, weighs aluminium diatomite closed pore hollow ceramic microspheres and restores G with bottle2, 100 milliliters of aluminium diatomite close Hole hollow ceramic microspheres nt wt net weight is G2- G1, and aluminium diatomite closed pore hollow ceramic microspheres density is in 0.75 g/cm3Between.
C, the measure of resistance to hydrostatic pressure intensity：Weigh 100 grams of aluminium diatomite closed pore hollow ceramic microspheres and pour into hydrostatic pressing intensity In test tube, hydrostatic pressing intensity test tube is connected with compression pump, and the water in compression pump is stressed in hydrostatic pressing intensity test tube, record pressure Force value, stop the aluminium diatomite closed pore hollow ceramic microspheres that pressurization is taken out in test tube and measure its floatability, aluminium diatomite closed pore is hollow The intensity of ceramic fine bead resistance to hydrostatic pressure is in 150 MPa.
D, the variable density value of aluminium diatomite closed pore hollow ceramic microspheres is detected：The sample point of same batch diverse location The variable density scope of aluminium diatomite closed pore hollow ceramic microspheres is in ± 0.01 g/cm3。
B, aluminium diatomite closed pore hollow ceramic microspheres prepare high temperature high voltage resistant oil well cementing test block.
The first step, dispensing：By the wt% of G levels oil-well cement 60, the aluminium diatomite closed pore hollow ceramic microspheres that particle diameter is 30 μm 30 wt%, 20 μm of wt% of flyash 5 of particle diameter of loss on ignition 1.1%, the calcium oxide 1.5wt% of purity 99.9%, the wt% of sodium sulphate 1.0 and The micro- wt% of silicon 2.5 of 10 μm of particle diameter.
Second step, make high-temperature-resistant high-pressure-resistant oil well cementing test block：It is mixed to get by the percentage by weight sampling of the first step Mixed powder, stir, with 0.6（W/C）The ratio of mud size mixing, slurries are aspirated by liquid pump, are sprayed to high speed revolving drum Outer surface, outer surface of cylinder produce centrifugal force slurries are shed, realization shed Stirring, pour into one group two pieces length and width, Height is respectively in 53mm*53mm*53mm die trials, is conserved respectively 24 hours, 48 hours in the water-bath curing box of 52 DEG C of constant temperature, Soaked 1 hour in cold water after the demoulding, carry out testing performance index.
3rd step, testing performance index.
A, serum density determines：Take second step to make slurries, pour into and density g/cm is weighed in fluid densitometer3, high temperature resistant, The density of high pressure slurries is in 1.3g/cm3Between.
B, the pH value measure of slurries：Take second step to make slurries, be put into pH value tester, show pH value, the pH of slurries Value is between 10.0.
C, sedimentation stability：Take second step to make slurries and pour into settlement barrel, observe homogeneity after 0.5 hour, stability, One property is that aluminium diatomite closed pore hollow ceramic microspheres mutually merge with slurries, and no longer floating fluctuation, microballon are evenly distributed on up and down In slurries.
D, the test of the performance and dosage of well cementing material：Base-material, i.e. G levels oil well superfine cement, palliative are floating bead or closed Hole hollow ceramic microspheres, additive, additive refer to the material beyond base-material and palliative, test hydration reaction speed, heatproof, resistance to Pressure.
E, the thickening time：Vary with temperature obvious, also relevant with additive addition quantity species, the record thickening time.
F, intensity test：Conserved respectively 24 hours, 48 hours in the water-bath curing box of 52 DEG C of constant temperature, well cementation examination Clotting is consolidated, and one piece of well cementation test block therein is taken out after 24 hours, is put on forcing press and carries out applied voltage test, calculate variable density Rate, another piece of cement briquette is taken out after 48 hours and carries out pressure test, with the extension of time, the compression strength of well cementation test block increases Add, calculate the rate of change of density.
The measure of well cementation test block rate of change of the density, 24 and 48 hours well cementation test block density is determined, well cementation test block is put into pressure Power machine pressurizes（100 MPa、150 MPa、180 MPa）Well cementation test block density after measure pressurization, rate of change of the density are equal to：（Add Density subtracts 24 and 48 hours well cementation test block density after pressure）/ 24 and 48 hours well cementation test block density, if rate of change of the density is more than 0.02, illustrate that aluminium zirconium oxide closed pore hollow ceramic microspheres wall unevenness is even, percentage of damage is high, and density increases after pressurization, does not reach and sets Meter standard, rate of change of the density are the degree of off-design density, and the density for test block of cementing the well is equal to the quality and volume of well cementation test block The ratio between.
Conserve 24 hours, soaked 1 hour in cold water after the demoulding, by national standard GB/T in the water-bath curing box of 52 DEG C of constant temperature 177 regulation carries out compression strength and rupture strength experiment on forcing press.
Conserve 48 hours, soaked 1 hour in cold water after the demoulding, by national standard GB/T in the water-bath curing box of 52 DEG C of constant temperature 177 regulation carries out compression strength and rupture strength experiment on forcing press.

Claims (2)

1. the method that aluminium diatomite closed pore hollow ceramic microspheres prepare high-temperature-resistant high-pressure-resistant oil well cementing test block, including aluminium diatomite Preparation, dispensing, mixing, the stirring of closed pore hollow ceramic microspheres are sized mixing, die trial, performance test, aluminium diatomite closed pore hollow ceramic Microballon performance test includes its floatability measure, density measurement, the measure of resistance to hydrostatic pressure intensity, and the performance test for test block of cementing the well includes Serum density measure, sedimentation stability, thickening time, drop fluid loss, the intensity test of test block, the liquidity scale；
Comprise the following steps：
A, the preparation of aluminium diatomite closed pore hollow ceramic microspheres：
The first step, dispensing：10~20 μm of diatomite of particle diameter, 10~30 μm of aluminium powders are taken, percentage by weight is：85~90wt%：10~ 15 wt%；
Second step, base：10~20 μm of diatomite of particle diameter, 10~30 μm of aluminium powders are taken, percentage by weight is：85~90wt%：10~ 15 wt%；By the first step percentage by weight sampling be mixed to get mixed powder, stir, take 10~20 μm of diatomite of particle diameter, Phenolic resin is added in the mixed powder of 10~30 μm of aluminium powders, mixed powder and phenolic resin ratio are：1.0 wt%：0.5~0.8 Wt%, 10~20 μm of diatomite of particle diameter, 10~30 μm of aluminium powders and phenolic resin is taken to be mixed evenly, at a temperature of 50~100 DEG C Curing process, firming body is crushed in flour mill, obtain 10~30 μm of mixed powders of particle diameter, mixed powder is put into mould, pressed Apply 3~5 MPa pressure on power machine, extrusion forming obtains blank；
3rd step, fire：Second step is obtained into blank to be put into sintering furnace, is 6 in the time of 1500~1600 DEG C of heat preservation sinterings ~8 hours, obtain aluminium diatomite block；
The making of 4th step, aluminium diatomite solid ceramic microbeads：3rd step is obtained into aluminium diatomite block to process on balling machine The solid ceramic microbeads of 5~20 μm of aluminium diatomite spherical shapes of particle diameter are made；
5th step, aluminium diatomite slurries make：The percentage of aluminium diatomite slurry forms：5~20 μm of aluminium diatomite of particle diameter are real 65~70wt% of heart ceramic fine bead：30~35wt% of water；
6th step, add foaming agent：To the 5th step make aluminium diatomite slurries in add foaming agent calcium carbonate, concentration be 1~ 3g/L；
It is prepared by the 7th step, aluminium diatomite closed pore hollow ceramic microspheres：6th step mixed serum is sufficiently stirred filtering, using high pressure High speed centrifugation rotary spraying technique is sprayed, forms microballoon, by dehydration expansion, high temperature on the oxygenation gas furnace of vertical zonal control Sintering, melt surface vitreous, balling-up, classification is selected to obtain 10~50 μm of aluminium diatomite closed pore hollow ceramic microspheres by wind-force Chilly, Aluminium diatomite closed pore hollow ceramic microspheres wall thickness is at 10~20 μm, and compression strength is in 100~180 MPa；
8th step, testing performance index：
A, its floatability determines：Weigh 10~50 μm of 100 grams of aluminium diatomite closed pore hollow ceramic microspheres of particle diameter and pour into 1000 milliliters In beaker, then pour into 500 milliliters of running water and fall in beaker, stirred with glass bar, stand 1 hour, the aluminium floated in beaker Diatomite closed pore hollow ceramic microspheres are floating bead, and heavy pearl is precipitated as in beaker bottom, and floating bead in beaker and heavy pearl are taken out respectively And dry and weigh, its floatability is calculated, its floatability of the aluminium diatomite closed pore hollow ceramic microspheres in water is more than 98%；
B, the density of aluminium diatomite closed pore hollow ceramic microspheres is measured：100 milliliters of volumetric flask is taken to weigh to obtain G1, by particle diameter 10~ 50 μm of aluminium diatomite closed pore hollow ceramic microspheres are poured into 100 milliliters of volumetric flasks, aluminium diatomite closed pore hollow ceramic microspheres concave surface It is tangent with the graduation mark of 100 milliliters of volumetric flasks, weigh aluminium diatomite closed pore hollow ceramic microspheres and restore G with bottle2, 100 milliliters of aluminium Diatomite closed pore hollow ceramic microspheres nt wt net weight is G2-G1, aluminium diatomite closed pore hollow ceramic microspheres density is measured in 0.5g/cm3 ~0.85 g/cm3Between；
C, the measure of resistance to hydrostatic pressure intensity：Weighing 10~50 μm of 100 grams of aluminium diatomite closed pore hollow ceramic microspheres of particle diameter pour into quiet In hydraulic pressure intensity test tube, hydrostatic pressing intensity test tube is connected with compression pump, and the water in compression pump is stressed on into hydrostatic pressing intensity test tube In, pressure value is recorded, stops the aluminium diatomite closed pore hollow ceramic microspheres that pressurization is taken out in test tube and measures its floatability, aluminium diatomite The intensity of closed pore hollow ceramic microspheres resistance to hydrostatic pressure is in 100~180 MPa；
D, the variable density value of aluminium diatomite closed pore hollow ceramic microspheres is detected：The aluminium silicon of the sample point of same batch diverse location The variable density scope of diatomaceous earth closed pore hollow ceramic microspheres is in ± 0.01 g/cm3；
B, aluminium diatomite closed pore hollow ceramic microspheres prepare high-temperature-resistant high-pressure-resistant oil well cementing test block：
The first step, dispensing：The wt% of G levels oil-well cement 55~65, the aluminium diatomite closed pore hollow ceramic that particle diameter is 10~50 μm are micro- The wt% of pearl 25~35,20~50 μm of 5~7wt% of flyash of particle diameter of loss on ignition 1.1%, the wt% of 99.9% calcium oxide of purity 1.5~2, The wt% of sodium sulphate 0.5~1.0 and micro- 1~3wt% of silicon of 5~20 μm of particle diameter,
Second step, the slurries for making high-temperature-resistant high-pressure-resistant oil well cementing test block：Mixed by the percentage by weight sampling of the first step To mixed powder, stir, sized mixing with 0.5~0.7 ratio of mud, slurries are aspirated by liquid pump, and high speed revolving drum is arrived in spraying Outer surface, outer surface of cylinder produce centrifugal force slurries are shed, realization shed Stirring, pour into one group of two pieces of length and width, Height is respectively in 53mm*53mm*53mm die trials, is conserved respectively 24 hours, 48 hours in the water-bath curing box of 52 DEG C of constant temperature, Soaked 1 hour in cold water after the demoulding, carry out testing performance index,
3rd step, testing performance index：
A, serum density determines：Take second step to make slurries, pour into and density is weighed in fluid densitometer, high temperature resistant, high pressure slurries Density in 1.0~1.5g/cm3Between；
B, the pH value measure of slurries：Take second step to make slurries, pour into pH value tester, show pH value, the pH value of slurries exists Between 8.0~10.5；
C, sedimentation stability：Take second step to make slurries and pour into settlement barrel, homogeneity, stability, homogeneity are observed after 0.5 hour It is that aluminium diatomite closed pore hollow ceramic microspheres mutually merge with slurries, no longer floating fluctuation, microballon are evenly distributed on slurries up and down In；
D, the test of the performance and dosage of well cementing material：Base-material, i.e. G levels oil well superfine cement, palliative are aluminium diatomite closed pore Hollow ceramic microspheres, additive, additive refer to the material beyond base-material and palliative, wall-thickness measurement, sphericity, closed pore, particle diameter Size, activity, hydration reaction speed；
E, the thickening time：Vary with temperature obvious, the record thickening time；
F, intensity test：Conserved respectively 24 hours, 48 hours in the water-bath curing box of 52 DEG C of constant temperature, well cementation test block is coagulated Gu taking out one piece of well cementation test block therein after 24 hours, it is put on forcing press and carries out applied voltage test, calculating rate of change of the density, 48 Another piece of well cementation test block is taken out after hour and carries out pressure test, with the extension of time, the compression strength increase of well cementation test block, meter The rate of change of density is calculated, rate of change of the density is less than 0.02%；
The restriction of 4th step, other performance index：
A, high-temperature-resistant high-pressure-resistant oil well refers to oil well operation face temperature at 150~240 DEG C, and the depth of oil well is below 4000 meters Oil well, the compression strength for test block of cementing the well is in 60~100MPa；
2. the method that aluminium diatomite ceramic fine bead according to claim 1 prepares high-temperature-resistant high-pressure-resistant oil well cementing test block, It is characterized in that：The high-temperature-resistant high-pressure-resistant well cementation test block drop fluid loss of preparation is less than 50mL/30min.
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