CN104478418A - Method for manufacturing high temperature resisting and high pressure resisting oil well cementation briquette through silicon bauxite ceramic microbeads - Google Patents
Method for manufacturing high temperature resisting and high pressure resisting oil well cementation briquette through silicon bauxite ceramic microbeads Download PDFInfo
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Abstract
A method for manufacturing a high temperature resisting and high pressure resisting oil well cementation briquette through silicon bauxite ceramic microbeads comprises the steps that the silicon bauxite closed-hole hollow ceramic microbeads are manufactured, burdening, mixing, stirring and size mixing are carried out, 55-65wt percent of G-class oil well cement, 25-35wt percent of the silicon bauxite closed-hole hollow ceramic microbeads with the grain size of five microns to 50 microns, five to seven wt percent of pulverized fuel ash with the loss on ignition of 1.1 percent and the grain size of 20 microns to 50 microns, 1.5 to two wt percent of calcium oxide with the purity of 99.9 percent, 0.5-1.0wt percent of sodium sulfate and one to three wt percent of micro-silicon with the grain size of five microns to 20 microns are mixed, size mixing is carried out according to the water cement ratio of 0.5 to 0.7, the mixtures are poured into a set of two briquette molds with the length of 53 mm, the width of 53 mm and the height of 53 mm, are maintained in a water bath maintenance box for 24 hours and 48 hours respectively at the constant temperature of 52 DEG C, and are soaked in cold water for one hour after demolding, and a performance index test is carried out.
Description
Technical field
The present invention relates to the method that sial sinter(-)corundum microballon prepares the test block of high-temperature-resistant high-pressure-resistant oil well cementing, belong to material technology neck.
Background technology
Current domestic well cementation light-weight additive adopts the drift pearl in flyash, and comprise heavy pearl and drift pearl at flyash, heavy pearl density is at 1.1 ~ 2.8g/cm
3between, content accounts for flyash 30 ~ 70%, and drift pearl is the glass microballon being less than water-mass density in flyash, and drift pearl mainly comprises aluminosilicate glass microballon and porous carbon granule, drift pearl after removing carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, surfaces externally and internally is smooth, and volume is large, is that one is rounded, light weight, closed pore are hollow, wear-resisting, high temperature resistant, thermal conductivity is little, intensity is high, drift pearl amount accounts for 0.5 ~ 1% of flyash total amount, and aluminosilicate glass microballon is hollow spherosome.
Drift pearl wherein in flyash it be coal dust in thermal power plant boiler through 1100 ~ 1500 DEG C burning time, clayey material melts becomes microlayer model, in stove turbulent flow hot air acting under at a high speed spin, form perfectly round sial spheroid, the gases such as nitrogen, hydrogen and carbonic acid gas that burning and scission reaction produce, undergoes rapid expansion in the high temperature aluminum silicon spheroid of melting, under capillary effect, form the glass envelope of hollow, then enter flue to cool rapidly, after sclerosis, become the vitreous state cenosphere of high vacuum, i.e. fly ash float.
Flyash is put into water stir, leave standstill for some time, because drift pearl density is less than water-mass density, will swim in the water surface pulls out and dry, be and float pearl, the drift pearl in flyash is canescence, and main component is SiO
2account for 70% and AI
2o
3account for 13%, loss on ignition is 0.40% ~ 0.574%, density 0.475 ~ 0.574g/cm
3, wall thickness 1.44 ~ 5.41 μm, particle size range is mainly distributed in 147 ~ 84 μm.
In recent years, due to the impact of northern haze weather, the big-and-middle-sized thermal power generation of China adopts the desulfurization technology of environmental protection, not containing in flyash floats pearl, cause in short supply, only have the drift pearl that middle small coal power plants and arcola do not adopt desulfurization technology supply a small amount of, drift the in short supply of pearl causes price increase, and float that pearl is impure is mixed with flyash, affect cementing quality.
In reinforcing oil well field, hydrocarbon distribution is wide, and long shut-in well is more and more, and main use of long shut-in well is light weight cement well cementation, and long shut-in well mainly adopts low-density cement mortar, wants to make the density of grout at 0.72 g/cm
3~ 1.5 g/cm
3between, density must at 0.5 g/cm for the lightening material (inorganic mineral material and organic synthesis material composition) of non-drift pearl
3~ 0.85 g/cm
3between, just can make the well cementation test block of high-temperature-resistant high-pressure-resistant, the density of G level oil well watertight is at 3.1 g/cm
3, light-weight additive density must be less than 1 g/cm
3, just can configure density 0.72 g/cm
3~ 1.5 g/cm
3between grout, precondition is that light-weight additive addition can not exceed 40% of total amount, otherwise can affect the ultimate compression strength of cement briquette.
Summary of the invention
The object of the invention is to overcome prior art present situation, there is provided a kind of cost low, excellent property, the pearl of wafing in flyash can be replaced, excellent property, makes density determine velocity of variation and is less than 0.02, reach design density, sial alumina closed pore hollow ceramic microspheres is made, density range 0.50 g/cm by the method for synthesis
3~ 0.85g/cm
3, and then configuration low density 1.0 g/cm
3~ 1.5g/cm
3the preparation method of high-temperature-resistant high-pressure-resistant oil well cementing test block, meets the requirement of long shut-in well well cementing material.
its technical scheme is.
Sial sinter(-)corundum microballon prepares the method for high-temperature-resistant high-pressure-resistant oil well cementing test block, comprise the preparation of sial alumina closed pore hollow ceramic microspheres, batching, mixing, stirring sized mixing, die trial, performance test, sial alumina closed pore hollow ceramic microspheres performance test comprise its floatability mensuration, density measurement, resistance to hydrostatic pressure intensity mensuration, serum density mensuration, sedimentation stability, thickening time, fluid loss, withstand voltage density test, the liquidity scale, compressive property test are fallen;
Comprise the following steps:
The preparation of A, sial alumina closed pore hollow ceramic microspheres:
The first step, batching: get particle diameter 1 ~ 20 μm of silica flour, particle diameter 5 ~ 20 μm of bauxitic clays, weight percent is: 80 ~ 85wt%:15 ~ 20 wt%;
Second step, base: by particle diameter 1 ~ 20 μm of silica flour, particle diameter 5 ~ 20 μm of bauxitic clays are mixed to get powder mix by the weight percent sampling of the first step, stir, by particle diameter 1 ~ 20 μm of silica flour, resol is added in the powder mix of particle diameter 5 ~ 25 μm of bauxitic clays, ratio is: 1.0 wt%:0.5 ~ 0.8 wt%, by particle diameter 1 ~ 20 μm of silica flour, particle diameter 5 ~ 20 μm of bauxitic clays and resol mixing and stirring, solidification treatment at 50 ~ 100 DEG C of temperature, cured body is pulverized in powder-making machine, obtain particle diameter 10 ~ 20 μm of powder mixs, powder mix puts into mould, pressing machine applies 1 ~ 3 MPa pressure, extrusion molding obtains blank,
3rd step, high-temperature firing: second step is obtained blank and puts into high temperature sintering furnace, at 1500 ~ 1600 DEG C, are 5 ~ 8 hours in the time of nitrogen atmosphere stove heat preservation sintering, and 300 ~ 500 DEG C of carbonization treatment obtain sial alumina block;
4th step, the making of sial alumina solid microbeads: the 3rd step is obtained the solid ceramic microbeads that sial alumina block is processed into particle diameter 5 ~ 20 μm of sial alumina spherical shape on balling machine, balling machine is processed into the solid ceramic microbeads of particle diameter 5 ~ 10 μm of sial alumina spherical shape, balling machine is not jaw crusher, jaw crusher utilizes metal accelerating impact or knocks material, the material shapes formed is sheet, many prismatics etc. are irregularly shaped, nodularization processing is that material blows afloat by blower fan, rotary motion phase mutual friction between material is spherical shape microballon, the particle of spherical shape is even in each particle stress distribution, ultimate compression strength is large, sheet, many prismatics high-temperature expansion sintered shape is still original shape, irregular shape is through high-temperature expansion sintering in cuttlefish fish head shapes, and ultimate compression strength is low, grinds stranding one fragmentation with two fingers, the density of broken rear slurry can increase, water cement ratio also increases, and setting time is long, and test block contraction ratio is large, blind hole, flat impossible Cheng Yuan's, nodularization is different with attrition crushing principle, and the performance of microballon is also different,
5th step, sial alumina slurry make: the per-cent of sial alum liquor slurry consists of: particle diameter 5 ~ 20 μm of sial alumina solid microbeads 65 ~ 70 wt%: water 30 ~ 35 wt%, is mixed in proportion stirring and sizes mixing;
6th step, whipping agent add: in the sial alumina slurry that the 5th step makes, add whipping agent, the one in calcium carbonate, potassium sulfate or sodium sulfate, concentration is 1 ~ 3g/L;
7th step, prepared by sial alumina closed pore hollow ceramic microspheres: by the abundant agitation and filtration of the 6th step mixed serum, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, the oxygenation gas furnace of zonal control expands through dehydration, high temperature sintering, melt surface vitreous, balling-up, classification is selected to obtain 5 ~ 50 μm of sial alumina closed pore hollow ceramic microspheres through Feng Li Cheongju, sial alumina closed pore hollow ceramic microspheres wall thickness is at 10 ~ 20 μm, ultimate compression strength is at 100 ~ 200 MPa, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, through overexpansion on the oxygenation gas furnace of zonal control, high temperature sintering, melt surface vitreous, balling-up, the concentration of oxygen is 30 ~ 35%, the concentration of oxygen is higher, burning-point is lower, burn more abundant, the heat of release is more, temperature is higher, wherein expansion temperature 800 ~ 900 DEG C, dry sintering temperature at 1400 ~ 1600 DEG C, melt surface temperature 1700 ~ 1800 DEG C, become bulb temperature 1400 ~ 1500 DEG C, balling-up selects classification to obtain 5 ~ 50 μm of sial alumina closed pore hollow ceramic microspheres through Feng Li Cheongju, high-pressure pump is adopted to starch extracting liquid from mixed solution, through pressurization, mixed solution slurry is delivered to centrifugal rotation spraying machine, the rotating speed of high speed centrifugation motor is at 24000 revs/min, motor is high temperature resistant at 1800 DEG C, high speed rotating produces larger centrifugal force and forms microballon, the size of microballon and injection aperture, pressure is relevant with speed, the higher expanding volume of dehydration expansion temperature is larger, relevant with temperature height, melt surface temperature could form sial alumina closed pore hollow ceramic microspheres, mineral substance produces activity after the above high temperature sintering of 900 DEG C, easy generation hydration reaction, generate spawn, improve early strength, as unslaked lime, flyash, silica flour etc., in addition, particle diameter is less, specific surface is larger, activity is larger, speed of response is fast, and the composition floating pearl determined by the composition of coal, the size of particle diameter cannot manual control, therefore the drift pearl performance in flyash can not change, i.e. wall thickness, the size of particle diameter and ultimate compression strength can not change, high pressure spraying high speed centrifugation rotary spraying technique can control the size of the particle diameter of microballon, wall thickness and ultimate compression strength, and the drift pearl wall thickness in flyash is less than 6 μm, maximum compressive strength 20 Mpa performance index artificially cannot control, relevant with the performance of material own, prepare high temperature resistant, the raw material light-weight additive that high pressure well cementation test block uses, as the performance of closed pore hollow ceramic microspheres and various well cementation light-weight additive material, performance index are as wall thickness, density, sphericity, its floatability, ultimate compression strength, opening and closing hole, size, must be artificially controlled, meet These parameters, well cementation light-weight additive wide accommodation, in addition, ceramic material property exceedes alloy material, be widely used in space flight, military project, the fields such as machinery, prepared by the method for synthetic, cost is low, performance is high.
8th step, testing performance index:
A, its floatability measures: take particle diameter 5 ~ 50 μm of sial alumina closed pore hollow ceramic microspheres 100 grams and pour in the beaker of 1000 milliliters, pour 500 ml tap waters again into fall in beaker, stir with glass stick, leave standstill 1 hour, sial alumina closed pore hollow ceramic microspheres floating in beaker is drift pearl, heavy pearl is precipitated as in beaker bottom, take out respectively and dry weigh floating pearl and heavy pearl in beaker, calculate its floatability, the its floatability of sial alumina closed pore hollow ceramic microspheres in water is greater than 98%, the density domination of sial alumina light-weight additive is in rational density range, i.e. 0.5g/cm
3~ 0.85 g/cm
3between, if the sial alumina closed pore hollow ceramic microspheres precipitation that sintering time is short, proportion is greater than water, broken sial alumina closed pore hollow ceramic microspheres water suction precipitation,
B, measure the density of sial alumina closed pore hollow ceramic microspheres: the volumetric flask getting 100 milliliters is weighed to obtain G
1, then sial alumina closed pore hollow ceramic microspheres is poured in 100 milliliters of volumetric flasks, the scale marks of sial alumina closed pore hollow ceramic microspheres concave surface and 100 milliliters of volumetric flasks is tangent, weighs sial alumina closed pore hollow ceramic microspheres and bottle recuperation G
2, 100 milliliters of sial alumina closed pore hollow ceramic microspheres nt wt net weights are G
2-G
1, obtain m=ρ V by quality, density and volume, density p=(G
2-G
1)/V, according to the cementing requirements of high temperature high voltage resistant test block, the density of test block is at 1.0 ~ 1.5g/cm
3, and sial alumina closed pore hollow ceramic microspheres density is at 0.5g/cm
3~ 0.85 g/cm
3between in scope;
C, the mensuration of resistance to hydrostatic pressure intensity: weigh sial alumina closed pore hollow ceramic microspheres 100 grams and pour in hydrostaticpressure intensity test tube, hydrostaticpressure intensity test tube is connected with pressure pump, water in pressure pump is stressed in hydrostaticpressure intensity test tube, record force value, the sial alumina closed pore hollow ceramic microspheres stopping pressurization taking out in test tube measures its floatability, after pressurization 110MPa, take out sial alumina closed pore hollow ceramic microspheres and measure its floatability, if the sial alumina closed pore hollow ceramic microspheres its floatability after pressurization is consistent with uninflated sial alumina closed pore hollow ceramic microspheres its floatability, show that the intensity of sial alumina closed pore hollow ceramic microspheres resistance to hydrostatic pressure is greater than 100 MPa, use the same method and measure 150MPa, 180 MPa, the numerical value such as 200 MPa, resistance to hydrostatic pressure intensity and sial alumina closed pore hollow ceramic microspheres ultimate compression strength, the intensity of sial alumina closed pore hollow ceramic microspheres resistance to hydrostatic pressure is at 100 ~ 200 MPa, and the maximum hydrostaticpressure intensity that fly ash float detects is 20 MPa, wall thickness is less than 6 μm, particle diameter is greater than 80 μm, the ultimate compression strength of test block depends on the ultimate compression strength of drift pearl, drift pearl in flyash is not suitable for the well cementation of High Temperature High Pressure oil well, namely less than 4000 meters are not suitable for, temperature is greater than the well cementation of the oil well of 150 DEG C, be suitable only for more than 2000 meters, temperature is less than the well cementation of the oil well of 90 DEG C, as everyone knows, stupalith is widely used in space flight, chemical industry, the fields such as machinery, the performance index such as stupalith ultimate compression strength are considerably beyond synthetic metals material, therefore sial alumina closed pore hollow ceramic microspheres can be used for the well cementation of High Temperature High Pressure oil well, stupalith is ultimate compression strength in making processes, wall thickness, the human controllable such as particle diameter, other materials is incomparable,
The variable density value of d, detection sial alumina closed pore hollow ceramic microspheres: the variable density scope of the sial alumina closed pore hollow ceramic microspheres of the sampling spot of same batch of different positions is at ± 0.01 g/cm
3, then the density of sampling spot sample should control at 0.69 g/cm
3~ 0.71g/cm
3between, high-temperature-resistant high-pressure-resistant oil well refers to oil well operation surface temperature at 150 ~ 240 DEG C, the oil well of the degree of depth below 4000 meters of oil well, ultimate compression strength is at 60 ~ 100MPa, the ultimate compression strength of well cementation test block depends on the ultimate compression strength of sial alumina closed pore hollow ceramic microspheres, low pressure oil well refers to that ultimate compression strength is less than 20 MPa, temperature is at 70 ~ 90 DEG C, middle force feed well refers to that ultimate compression strength is at 20 ~ 60MPa, at 90 ~ 150 DEG C of high pressure oil wells, temperature refers to that ultimate compression strength is greater than 60 ~ 100 MPa, temperature in oil well be surface temperature add oil well often decline 100 meters of temperature increase by 3 DEG C of values and,
B, sial alumina closed pore hollow ceramic microspheres prepare the test block of high-temperature-resistant high-pressure-resistant oil well cementing:
The first step, batching: be sial alumina closed pore hollow ceramic microspheres 25 ~ 35 wt% of 5 ~ 50 μm, particle diameter 20 ~ 50 μm of flyash 5 ~ 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2 wt%, sodium sulfate 0.5 ~ 1.0 wt% and micro-silicon 1 ~ 3 wt% of particle diameter 5 ~ 20 μm by G level oil well cement 55 ~ 65 wt%, particle diameter, the pH value of configuration slurries is between 8.0 ~ 10.5, G oil well cement particle diameter and sial alumina closed pore hollow ceramic microspheres size variant, adopt the flyash of loss on ignition 1.1%, according to accumulation principle, space between the bi-material particle diameter that flyash mainly fills up G oil well cement and sial alumina closed pore hollow ceramic microspheres, when the different particle of particle diameter is tangent between two, gap between tangent circles is filled by flyash, G oil well cement and glass microballon grain are combined closely, but usage quantity should control within the specific limits, namely control within the scope of 5 ~ 7 % of gross weight, otherwise, affect the intensity of high temperature high voltage resistant test block, next is through the flyash that high temperature sintering generates, there is activity, significantly improve the hydration rate of slurries, the flyash that loss on ignition is low needs water cement ratio little, the morning contributing to well cementation test block is strong, purity 99.9% calcium oxide, calcium oxide purity is higher, activity is stronger, hydration rate is fast, a large amount of heat is discharged during calcium oxide hydration reaction, and generate gelatinous material calcium hydroxide, the morning being beneficial to high temperature high voltage resistant slurries is strong, temperature plays an important role by force the morning to test block, secondly the calcium hydroxide generated after aquation is in alkalescence, the pH value of high temperature high voltage resistant slurries can be regulated, under weak basic condition, the early strength of high temperature high voltage resistant oil well cement can be improved, sodium sulfate is a kind of water retaining, it is obvious that dehydration effect falls, sodium ion in sodium sulfate, there is reverse osmosis function, velocity of diffusion is fast, make slurries in solidifying, separate out part water, sodium sulfate consumption is how many, the dehydration of falling of slurries is played an important role, rationally falling dehydration, to be conducive to morning of high temperature high voltage resistant Behavior of Hardened Cement Paste strong, if it is too much that dehydration falls in high temperature high voltage resistant slurries in solidifying, high temperature high voltage resistant well cementation test block shrinkage is large, cause blind hole, affect cementing quality, sodium sulfate is compared with other water retainings, sodium ion diffustivity is strong, diffusion uniformity, cost is low, Be very effective, according to accumulation principle, SILICA FUME mainly fills up G oil well cement and the gap between sial alumina closed pore hollow ceramic microspheres and flyash, there is greater activity, form spawn, improve the intensity of high temperature high voltage resistant slurries, increasing dioxide-containing silica and slurries suspension stability and Behavior of Hardened Cement Paste high temperature resistance is indispensable technical qualification, above-mentioned several interpolation and must consumption be controlled,
Second step, make the test block of high-temperature-resistant high-pressure-resistant oil well cementing: be mixed to get powder mix by the weight percent sampling of the first step, stir, with 0.5 ~ 0.7(W/C) water cement ratio size mixing, slurries are aspirated by liquid pump, spray the outside surface of high speed rotating rotating cylinder, produce centrifugal force at outer surface of cylinder slurries are shed, Stirring is shed in realization, pour one group of two block length into, wide, height is respectively in 53mm*53mm*53mm die trial, difference maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, 48 hours, soak 1 hour in cold water after the demoulding, carry out testing performance index, if water usage quantity is more than 0.5 ~ 0.7 scope, the grout cures time is long, early strength is low, it is too much that dehydration is fallen, test block is fallen dehydration and is greater than 50ml/30min, test block shrinkage is large, cause blind hole, affect cementing quality,
3rd step, testing performance index:
A, serum density measure: get second step and make slurries, pour in fluid densitometer and weigh density g/cm
3, the density of high temperature resistant, high pressure slurries is at 1.0 ~ 1.5g/cm
3between; The density of high temperature resistant, high pressure slurries is at 1.0 ~ 1.5g/cm
3between, test block rate of change of the density is less than 0.015 g/cm
3, according to ρ=m/V formula, weigh up the weight G of test block
1, according to volume V
1, bulk density ρ
1, test block is put on pressing machine and pressurizes, weigh up the weight G of test block
2, according to volume V
2,bulk density ρ
2, rate of change of the density is (ρ
2-ρ
1)/ρ
1, it is strong that rate of change of the density is less than explanation well cementation test block anti-pressure ability, V after pressurization
2volume change is little, density p
2change also little;
The pH value of b, slurries measures: get second step and make slurries, pour in pH value tester, display pH value, and the pH value of slurries is between 8.0 ~ 10.5;
C, sedimentation stability: get second step making slurries and pour settlement barrel into, observe homogeneity after 0.5 hour, stability, homogeneity is that sial alumina closed pore hollow ceramic microspheres and slurries merge mutually, no longer upper and lower floating fluctuation, and microballon is evenly distributed in slurries;
The performance of d, well cementing material and the test of consumption: base-material, namely namely G level oil well superfine cement, light-weight additive float pearl or closed pore hollow ceramic microspheres, admixture, admixture refers to the material beyond base-material and light-weight additive, measuring density, wall thickness, sphericity, closed pore, size, hydration reaction speed, measure particle diameter with particle instrument;
E, thickening time: vary with temperature obviously, also adds quantity kind with admixture relevant, records the thickening time;
F, intensity test: difference maintenance 24 hours, 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, well cementation test block is solidified, one piece of well cementation test block is wherein taken out after 24 hours, put on pressing machine and carry out applied voltage test, bulk density velocity of variation, take out another block cement briquette after 48 hours and carry out pressure test, along with the prolongation of time, the ultimate compression strength of well cementation test block increases, the velocity of variation of bulk density, and the density of high temperature resistant, high pressure slurries is at 1.0 ~ 1.5g/cm
3between, test block rate of change of the density is less than 0.015 g/cm
3, according to ρ=m/V formula, weigh up the weight G of test block
1, according to volume V
1, bulk density ρ
1, test block is put on pressing machine and pressurizes, weigh up the weight G of test block
2, according to volume V
2,bulk density ρ
2, rate of change of the density is (ρ
2-ρ
1)/ρ
1, it is strong that rate of change of the density is less than explanation well cementation test block anti-pressure ability, V after pressurization
2volume change is little, density p
2change also little;
The restriction of the 4th step, other performance index:
A, high-temperature-resistant high-pressure-resistant oil well refer to oil well operation surface temperature at 150 ~ 240 DEG C, the oil well of the degree of depth below 4000 meters of oil well, and the ultimate compression strength of well cementation test block is at 60 ~ 100MPa;
B, because High Temperature High Pressure oil well operation surface temperature is at 150 ~ 240 DEG C, conventional admixture such as hardening accelerator, dispersion agent, water retaining, setting accelerator, defoamer etc. must mark use range, temperature raises admixture and decomposes ineffective, if not otherwise specified, conventional admixture is all low temperature modification, the temperature used, below 90 DEG C, will lose efficacy more than 90 DEG C;
C, the restriction of light-weight additive and admixture content: the add-on that light-weight additive refers to sial alumina closed pore hollow ceramic microspheres should be less than 35%, admixture heatproof must be greater than 300 DEG C, addition controls within the specific limits, i.e. flyash 5 ~ 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2 wt%, sodium sulfate 0.5 ~ 1.0 wt% and micro-silicon 1 ~ 3 wt%, well cementing material can be divided into: base-material and G level oil well superfine cement, namely light-weight additive floats pearl and closed pore hollow ceramic microspheres, admixture, admixture refers to the material beyond base-material and light-weight additive, G level oil well superfine cement, sial alumina hole hollow ceramic microspheres particle diameter, the loss on ignition of flyash and activity, the indexs such as the pH value of slurries, G level oil well superfine cement, sial alumina hole hollow ceramic microspheres, the flyash of loss on ignition 1.1%, purity 99.9% calcium oxide, micro-silicon is all through the material of the high-temperature firing of 900 ° of more than C, the fusing point that salt sodium sulfate is 884 DEG C, not easily decompose in High Temperature High Pressure oil well, stability is strong, adopt the flyash of loss on ignition 1.1%, loss on ignition is low, carbon content is low, sintering fully, active high, hydration reaction speed is fast, form gelatinous material speed fast, according to accumulation principle, space between the bi-material particle diameter that flyash mainly fills up G oil well cement and closed pore hollow glass micropearl, when the different particle of particle diameter is tangent between two, gap between tangent circles is filled by flyash, G oil well cement and the hollow glass microballon grain of sial alumina closed pore are combined closely, but usage quantity should control within the specific limits, namely control within the scope of 5 ~ 7 % of gross weight, otherwise, affect the intensity of test block, next is through the flyash that high temperature sintering generates, there is activity, the hydration rate of slurries is accelerated, the morning contributing to well cementation test block is strong, purity 99.9% calcium oxide, calcium oxide purity is higher, activity is stronger, hydration rate is fast, a large amount of heat is discharged during calcium oxide hydration reaction, the temperature of slurries is raised, and generate gelatinous material calcium hydroxide, the morning being beneficial to test block is strong, secondly the calcium hydroxide generated after aquation is in alkalescence, the pH value of slurries can be regulated, under weak basic condition, namely pH value is between 8 ~ 10.5, the early strength of oil well test block can be improved, sodium sulfate is a kind of water retaining, it is obvious that dehydration effect falls, sodium ion in sodium sulfate, there is reverse osmosis function, velocity of diffusion is fast, make slurries in solidifying, separate out part water, sodium sulfate consumption is how many, the dehydration of falling of slurries is played an important role, rationally falling dehydration, to be conducive to morning of Behavior of Hardened Cement Paste strong, if it is too much that dehydration falls in slurries in solidifying, well cementation test block shrinkage is large, cause blind hole, affect cementing quality, sodium sulfate is compared with other water retainings, sodium ion diffustivity is strong, diffusion uniformity, cost is low, Be very effective, admixture must control usage quantity, flyash consumption is excessive, the ultimate compression strength of well cementation test block reduces, density increases, water cement ratio increases, namely water consumption increases, fall dehydration to increase, light-weight additive can not be replaced with admixture, more can not replace basic oil well cement with admixture, the intensity of loss test block, the density of slurries can be increased, ultimate compression strength reduces, test block of even cementing the well does not have ultimate compression strength and folding strength, light-weight additive and admixture must control consumption, use range and condition need be shown especially, although some admixture has similar function to the admixture of above-mentioned use, but the environment used is different, environment for use changes admixture will lose function, conventional admixture is as hardening accelerator, water retaining, setting accelerator is low temperature modification, use below 90 DEG C, otherwise lost efficacy, other admixture is as flyash, calcium oxide, micro-silicon etc. must limit purity, composition, color, addition, the indexs such as the scope used, carry out parametrization demarcation, namely for high temperature high voltage resistant well cementation test block, well cementation is greater than 4000 meters, use temperature is at 150 ~ 240 DEG C of C, test block pressure resistance intensity is at 60 ~ 100MPa, namely the sial alumina bead density of high temperature high voltage resistant well cementation test block is prepared at 0.5g/cm
3~ 0.85 g/cm
3between, and flyash, silica flour, wilkinite, kaolin, diatomite, sepiolite, antisaline soil isodensity are all at 2.0 g/cm
3above, density can not be prepared at 1.0 ~ 1.5g/cm
3between slurries, usually by 1.0 ~ 1.5g/cm
3between be high temperature high voltage resistant slurries, 1.6 g/cm
3~ 1.7 g/cm
3for the slurries of resistance to medium temperature and medium pressure, 1.8 g/cm
3~ 1.9 g/cm
3for low-temperature low pressure resistance slurries, and G level oil well superfine cement density is at 3.0 ~ 3.3g/cm
3, density adopts weighted average calculation.
Described sial sinter(-)corundum microballon prepares the method for high-temperature-resistant high-pressure-resistant oil well cementing test block, and the High Temperature High Pressure well cementation test block of preparation is fallen fluid loss and is less than 50ml/30min.
The microballon of closed pore must be used, the hollow glass micropearl of perforate is as oil well cementing light-weight additive material, a certain proportion of water is added after mixing with G level oil well cement, water molecules enters in hollow glass microballon by micropore, the perforate hollow glass micropearl quality of unit volume is increased, hollow glass micropearl density is caused to increase, water cement ratio increases, the density of grout also becomes large, namely water consumption increases, grout is in process of setting, thickening time increases, Behavior of Hardened Cement Paste tries fast early strength to be reduced, fall dehydration to increase, the fast contraction of Behavior of Hardened Cement Paste examination is excessive, anti-pressure ability reduces, easily cause the blind hole accident of oil well, in addition, the ultimate compression strength of closed pore hollow ceramic microspheres is much larger than the ultimate compression strength of closed pore hollow ceramic microspheres, in addition, material its performance different is also different, its effect of different ratio is also different, can not with the material of certain single component compared with matrix material, there is no comparability, even identical material, proportioning is the same, the succession of mixing changes, also there is a world of difference in its performance, the comparison of differing materials still more, there is no comparability.
The present invention has the following advantages.
1, can change the dependence to flyash floating bead in long-term well cementation, the density of ceramic fine bead, wall thickness, sintering temperature can control.
2, this technical matters is advanced, and technology maturation, product performance are stable, and production cost is low, and output is high, and performance is good, opens well cementation synthesis virgin material new way.
3
,sial sinter(-)corundum bead density is at 0.50 g/cm
3~ 0.85g/cm
3, according to piling up the theoretical space added between SILICA FUME filler particles, dioxide-containing silica is high, increase Behavior of Hardened Cement Paste high temperature resistance, G level oil well cement, ceramic fine bead have greater activity through more than 1000 DEG C high temperature sinterings, and hydration reaction is fast, can jelly be formed, can early strength be improved.
4
,through overexpansion on the oxygenation gas furnace of zonal control, high temperature sintering, melt surface vitreous, balling-up, the concentration of oxygen is 30 ~ 35%, the concentration of oxygen is higher, burning-point is lower, burn more abundant, the heat of release is more, temperature is higher, , adopt high pressure spraying high speed centrifugation rotary spraying technique, body of heater is entered after liquid is fully atomized, drop is at breathing space expanded by heating, expanding volume is relevant with expansion temperature and density of foaming agent, again through sintering, melting, last balling-up, prevent knot wall from adopting thermal cycling air-bleed system to improve output, blower fan adopts speed control by frequency variation blower fan.
Embodiment
Embodiment.
Comprise the preparation of sial alumina closed pore hollow ceramic microspheres, batching, mixing, stirring sized mixing, die trial, performance test, silica flour bauxitic clay closed pore hollow ceramic microspheres performance test comprise its floatability mensuration, density measurement, resistance to hydrostatic pressure intensity mensuration, serum density mensuration, sedimentation stability, thickening time, fluid loss, withstand voltage density test, the liquidity scale, compressive property test are fallen.
Comprise the following steps.
The preparation of A, sial alumina closed pore hollow ceramic microspheres.
The first step, batching: get particle diameter 10 μm of silica flours, particle diameter 15 μm of bauxitic clays, weight percent is: 80wt%:20 wt%;
Second step, base: by particle diameter 10 μm of silica flours, particle diameter 15 μm of bauxitic clays are mixed to get powder mix by the weight percent sampling of the first step, stir, by particle diameter 10 μm of silica flours, resol is added in the powder mix of particle diameter 15 μm of bauxitic clays, ratio is: 1.0 wt%:0.5 wt%, by particle diameter 10 μm of silica flours, particle diameter 15 μm of bauxitic clays and resol mixing and stirring, solidification treatment at 60 DEG C of temperature, cured body is pulverized in powder-making machine, obtain particle diameter 20 μm of powder mixs, powder mix puts into mould, pressing machine applies 1.5 MPa pressure, extrusion molding obtains blank.
3rd step, high-temperature firing: second step is obtained blank and puts into high temperature sintering furnace, at 1500 DEG C,
Be 8 hours in the time of nitrogen atmosphere stove heat preservation sintering, 500 DEG C of carbonization treatment obtain sial alumina block.
The making of the 4th step, sial alumina solid microbeads: the 3rd step is obtained the full particle that sial alumina block is processed into particle diameter 10 μm of sial alumina spherical shape on balling machine.
5th step, sial alumina slurry make: the per-cent of sial alum liquor slurry consists of: particle diameter 10 μm of sial alumina 70 wt%: water 30 wt%.。
6th step, whipping agent add: in the sial alumina slurry that the 5th step makes, add whipping agent calcium carbonate, concentration is 2g/L.
Prepared by the 7th step, sial alumina closed pore hollow ceramic microspheres: by the abundant agitation and filtration of the 6th step mixed serum; adopt high pressure spraying high speed centrifugation rotary spraying technique; form microballoon; through dehydration expansion, high temperature sintering, melt surface vitreous, balling-up on the oxygenation gas furnace of zonal control; classification is selected to obtain 20 μm of sial alumina closed pore hollow ceramic microspheres through Feng Li Cheongju; sial alumina closed pore hollow ceramic microspheres wall thickness is at 20 μm, and ultimate compression strength is at 200 MPa.
8th step, testing performance index.
A, its floatability measure: take particle diameter 20 μm of sial alumina closed pore hollow ceramic microspheres 100 grams and pour in the beaker of 1000 milliliters, pour 500 ml tap waters again into fall in beaker, stir with glass stick, leave standstill 1 hour, sial alumina closed pore hollow ceramic microspheres floating in beaker is drift pearl, is precipitated as heavy pearl in beaker bottom, takes out respectively and dries weigh floating pearl and heavy pearl in beaker, calculate its floatability, its floatability of sial alumina closed pore hollow ceramic microspheres in water is greater than 98%.
B, measure the density of sial alumina closed pore hollow ceramic microspheres: the volumetric flask getting 100 milliliters is weighed to obtain G
1, then sial alumina closed pore hollow ceramic microspheres is poured in 100 milliliters of volumetric flasks, the scale marks of sial alumina closed pore hollow ceramic microspheres concave surface and 100 milliliters of volumetric flasks is tangent, weighs sial alumina closed pore hollow ceramic microspheres and bottle recuperation G
2, 100 milliliters of sial alumina closed pore hollow ceramic microspheres nt wt net weights are G
2-G
1, and sial alumina closed pore hollow ceramic microspheres density is at 0.75 g/cm
3between.
The mensuration of c, resistance to hydrostatic pressure intensity: weigh sial alumina closed pore hollow ceramic microspheres 100 grams and pour in hydrostaticpressure intensity test tube, hydrostaticpressure intensity test tube is connected with pressure pump, water in pressure pump is stressed in hydrostaticpressure intensity test tube, record force value, the sial alumina closed pore hollow ceramic microspheres stopping pressurization taking out in test tube measures its floatability, and the intensity of sial alumina closed pore hollow ceramic microspheres resistance to hydrostatic pressure is at 200 MPa.
The variable density value of d, detection sial alumina closed pore hollow ceramic microspheres: the variable density scope of the sial alumina closed pore hollow ceramic microspheres of the sampling spot of same batch of different positions is at ± 0.01 g/cm
3.
B, sial alumina closed pore hollow ceramic microspheres prepare the test block of high-temperature-resistant high-pressure-resistant oil well cementing.
The first step, batching: be sial alumina closed pore hollow ceramic microspheres 30 wt% of 20 μm, particle diameter 20 μm of flyash 5 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 1.0 wt% and micro-silicon 2.5 wt% of particle diameter 10 μm by G level oil well cement 60 wt%, particle diameter.
Second step, make the test block of high-temperature-resistant high-pressure-resistant oil well cementing: be mixed to get powder mix by the weight percent sampling of the first step, stir, with 0.6(W/C) water cement ratio size mixing, slurries are aspirated by liquid pump, spray the outside surface of high speed rotating rotating cylinder, produce centrifugal force at outer surface of cylinder slurries are shed, Stirring is shed in realization, pour one group of two block length into, wide, height is respectively in 53mm*53mm*53mm die trial, difference maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, 48 hours, soak 1 hour in cold water after the demoulding, carry out testing performance index.
3rd step, testing performance index.
A, serum density measure: get second step and make slurries, pour in fluid densitometer and weigh density g/cm
3, the density of high temperature resistant, high pressure slurries is at 1.3g/cm
3between.
The pH value of b, slurries measures: get second step and make slurries, put into pH value tester, and display pH value, the pH value of slurries is between 9.5.
C, sedimentation stability: get second step making slurries and pour settlement barrel into, observe homogeneity after 0.5 hour, stability, homogeneity is that sial alumina closed pore hollow ceramic microspheres and slurries merge mutually, no longer upper and lower floating fluctuation, and microballon is evenly distributed in slurries;
The performance of d, well cementing material and the test of consumption: base-material, namely namely G level oil well superfine cement, light-weight additive float pearl or closed pore hollow ceramic microspheres, admixture, and admixture refers to the material beyond base-material and light-weight additive, test aquation speed of response, heatproof, withstand voltage;
E, thickening time: vary with temperature obviously, also adds quantity kind with admixture relevant, records the thickening time.
F, intensity test: difference maintenance 24 hours, 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, well cementation test block is solidified, one piece of well cementation test block is wherein taken out after 24 hours, put on pressing machine and carry out applied voltage test, bulk density velocity of variation, takes out another block cement briquette and carries out pressure test, along with the prolongation of time after 48 hours, the ultimate compression strength of well cementation test block increases, the velocity of variation of bulk density.
The mensuration of well cementation test block rate of change of the density, measure 24 and 48 hours well cementation test block density, well cementation test block is put into pressing machine pressurization (60MPa, 75MPa, 100 MPa, 150 MPa, 200 MPa) measure the well cementation test block density after pressurizeing, rate of change of the density equals: (after pressurization, density deducts 24 and 48 hours well cementation test block density)/24 and 48 hours well cementation test block density, if rate of change of the density is greater than 0.02, illustrate that sial alumina closed pore hollow ceramic microspheres inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density, the density of well cementation test block equals the well cementation quality of test block and the ratio of volume, ultimate compression strength 150 MPa.
Maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
Maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
Claims (2)
1. sial sinter(-)corundum microballon prepares the method for high-temperature-resistant high-pressure-resistant oil well cementing test block, comprise the preparation of sial alumina closed pore hollow ceramic microspheres, batching, mixing, stirring sized mixing, die trial, performance test, silica flour bauxitic clay closed pore hollow ceramic microspheres performance test comprise its floatability mensuration, density measurement, resistance to hydrostatic pressure intensity mensuration, serum density mensuration, sedimentation stability, thickening time, fluid loss, the intensity test of test block, the liquidity scale fall;
Comprise the following steps:
The preparation of A, sial alumina closed pore hollow ceramic microspheres:
The first step, batching: get particle diameter 1 ~ 20 μm of silica flour, particle diameter 5 ~ 20 μm of bauxitic clays, weight percent is: 80 ~ 85wt%:15 ~ 20 wt%;
Second step, base: by particle diameter 1 ~ 20 μm of silica flour, particle diameter 5 ~ 20 μm of bauxitic clays are mixed to get powder mix by the weight percent sampling of the first step, stir, by particle diameter 1 ~ 20 μm of silica flour, resol is added in the powder mix of particle diameter 5 ~ 25 μm of bauxitic clays, ratio is: 1.0 wt%:0.5 ~ 0.8 wt%, by particle diameter 1 ~ 20 μm of silica flour, particle diameter 5 ~ 20 μm of bauxitic clays and resol mixing and stirring, solidification treatment at 50 ~ 100 DEG C of temperature, cured body is pulverized in powder-making machine, obtain particle diameter 10 ~ 20 μm of powder mixs, powder mix puts into mould, pressing machine applies 1 ~ 3 MPa pressure, extrusion molding obtains blank,
3rd step, high-temperature firing: second step is obtained blank and puts into high temperature sintering furnace, at 1500 ~ 1600 DEG C, be 5 ~ 8 hours in the time of nitrogen atmosphere stove heat preservation sintering, 300 ~ 500 DEG C of carbonization treatment obtain sial alumina block, form the sial combination of high silicon;
The making of the 4th step, sial alumina solid ceramic microbeads: the 3rd step is obtained the solid ceramic microbeads that sial alumina block is processed into particle diameter 5 ~ 20 μm of sial alumina spherical shape on balling machine;
5th step, sial alumina slurry make: the per-cent of sial alum liquor slurry consists of: particle diameter 5 ~ 20 μm sial alumina solid ceramic microbeads 65 ~ 70 wt%: water 30 ~ 35 wt%;
6th step, whipping agent add: in the sial alumina slurry that the 5th step makes, add whipping agent, the one in calcium carbonate, potassium sulfate or sodium sulfate, concentration is 1 ~ 3g/L;
Prepared by the 7th step, sial alumina closed pore hollow ceramic microspheres: by the abundant agitation and filtration of the 6th step mixed serum, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, through dehydration expansion, high temperature sintering, melt surface vitreous, balling-up on the oxygenation gas furnace of zonal control, classification is selected to obtain 5 ~ 50 μm of sial alumina closed pore hollow ceramic microspheres through Feng Li Cheongju, sial alumina closed pore hollow ceramic microspheres wall thickness is at 10 ~ 20 μm, and ultimate compression strength is at 100 ~ 200 MPa;
8th step, testing performance index:
A, its floatability measure: take particle diameter 5 ~ 50 μm of sial alumina closed pore hollow ceramic microspheres 100 grams and pour in the beaker of 1000 milliliters, pour 500 ml tap waters again into fall in beaker, stir with glass stick, leave standstill 1 hour, sial alumina closed pore hollow ceramic microspheres floating in beaker is drift pearl, is precipitated as heavy pearl in beaker bottom, takes out respectively and dries weigh floating pearl and heavy pearl in beaker, calculate its floatability, its floatability of sial alumina closed pore hollow ceramic microspheres in water is greater than 98%;
B, measure the density of sial alumina closed pore hollow ceramic microspheres: the volumetric flask getting 100 milliliters is weighed to obtain G
1, then sial alumina closed pore hollow ceramic microspheres is poured in 100 milliliters of volumetric flasks, the scale marks of sial alumina closed pore hollow ceramic microspheres concave surface and 100 milliliters of volumetric flasks is tangent, weighs sial alumina closed pore hollow ceramic microspheres and bottle recuperation G
2, 100 milliliters of sial alumina closed pore hollow ceramic microspheres nt wt net weights are G
2-G
1, record sial alumina closed pore hollow ceramic microspheres density at 0.5g/cm
3~ 0.85 g/cm
3between;
The mensuration of c, resistance to hydrostatic pressure intensity: weigh sial alumina closed pore hollow ceramic microspheres 100 grams and pour in hydrostaticpressure intensity test tube, hydrostaticpressure intensity test tube is connected with pressure pump, water in pressure pump is stressed in hydrostaticpressure intensity test tube, record force value, the sial alumina closed pore hollow ceramic microspheres stopping pressurization taking out in test tube measures its floatability, and the intensity of sial alumina closed pore hollow ceramic microspheres resistance to hydrostatic pressure is at 100 ~ 200 MPa;
The variable density value of d, detection sial alumina closed pore hollow ceramic microspheres: the variable density scope of the sial alumina closed pore hollow ceramic microspheres of the sampling spot of same batch of different positions is at ± 0.01 g/cm
3;
B, sial alumina closed pore hollow ceramic microspheres prepare the test block of high-temperature-resistant high-pressure-resistant oil well cementing:
The first step, batching: G level oil well cement 55 ~ 65 wt%, particle diameter are sial alumina closed pore hollow ceramic microspheres 25 ~ 35 wt%, particle diameter 20 ~ 50 μm of flyash 5 ~ 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2 wt%, sodium sulfate 0.5 ~ 1.0 wt% and micro-silicon 1 ~ 3 wt% of particle diameter 5 ~ 20 μm of 5 ~ 50 μm
Second step, make the slurries of high-temperature-resistant high-pressure-resistant oil well cementing test block: be mixed to get powder mix by the weight percent sampling of the first step, stir, size mixing with the water cement ratio of 0.5 ~ 0.7, slurries are aspirated by liquid pump, spray the outside surface of high speed rotating rotating cylinder, produce centrifugal force at outer surface of cylinder slurries are shed, Stirring is shed in realization, pour one group of two block length into, wide, height is respectively in 53mm*53mm*53mm die trial, difference maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, 48 hours, soak 1 hour in cold water after the demoulding, carry out testing performance index,
3rd step, testing performance index:
A, serum density measure: get second step and make slurries, pour in fluid densitometer and weigh density, the density of high temperature resistant, high pressure slurries is at 1.0 ~ 1.5g/cm
3between;
The pH value of b, slurries measures: get second step and make slurries, pour in pH value tester, display pH value, and the pH value of slurries is between 8.0 ~ 10.5;
C, sedimentation stability: get second step making slurries and pour settlement barrel into, observe homogeneity after 0.5 hour, stability, homogeneity is that sial alumina closed pore hollow ceramic microspheres and slurries merge mutually, no longer upper and lower floating fluctuation, and microballon is evenly distributed in slurries;
The performance of d, well cementing material and the test of consumption: base-material, i.e. G level oil well superfine cement, light-weight additive and sial alumina closed pore hollow ceramic microspheres, admixture, admixture refers to the material beyond base-material and light-weight additive, wall-thickness measurement, sphericity, closed pore, size, activity, hydration reaction speed;
E, thickening time: record thickening time;
F, intensity test: difference maintenance 24 hours, 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, well cementation test block is solidified, one piece of well cementation test block is wherein taken out after 24 hours, put on pressing machine and carry out applied voltage test, bulk density velocity of variation, take out another block well cementation test block after 48 hours and carry out pressure test, along with the prolongation of time, the ultimate compression strength of well cementation test block increases, the velocity of variation of bulk density, and density transform rate is less than 0.02%;
The restriction of the 4th step, other performance index:
A, high-temperature-resistant high-pressure-resistant oil well refer to oil well operation surface temperature at 150 ~ 240 DEG C, the oil well of the degree of depth below 4000 meters of oil well, and the ultimate compression strength of well cementation test block is at 60 ~ 100MPa;
B, because high-temperature-resistant high-pressure-resistant oil well operation surface temperature is at 150 ~ 240 DEG C, conventional admixture must mark use range as hardening accelerator, dispersion agent, water retaining, setting accelerator, defoamer etc., and the temperature admixture exceeding regulation decomposes ineffective;
The restriction of c, light-weight additive and admixture usage quantity: the add-on of sial alumina closed pore hollow ceramic microspheres should be less than 40%, admixture heatproof must be greater than 300 DEG C, addition controls in certain scope, loss on ignition 1.1% flyash usage quantity is less than 10 wt%, purity 99.9% calcium oxide usage quantity is less than 3wt%, sodium sulfate usage quantity is less than 1.0 wt% and micro-silicon usage quantity is less than 3 wt%.
2. sial sinter(-)corundum microballon according to claim 1 prepares the method for 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 of preparation is fallen fluid loss and is less than 50ml/30min.
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