CN103803888A - Method for preparing oil well cement test block by utilizing silicon oxynitride ceramic composite microspheres - Google Patents
Method for preparing oil well cement test block by utilizing silicon oxynitride ceramic composite microspheres Download PDFInfo
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- CN103803888A CN103803888A CN201410087529.1A CN201410087529A CN103803888A CN 103803888 A CN103803888 A CN 103803888A CN 201410087529 A CN201410087529 A CN 201410087529A CN 103803888 A CN103803888 A CN 103803888A
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Abstract
The invention provides a method for preparing an oil well cement test block by utilizing silicon oxynitride ceramic composite microspheres. The method comprises the following steps: preparing silicon oxynitride ceramic composite obturator hollow microspheres, compounding, mixing, performing stirring and size mixing, performing mold testing and performing strength testing; uniformly mixing and stirring 40 to 50 percent by weight of G-grade oil well cement, 10 to 15 percent by weight of 13-micrometer ultrafine cement, 25 to 35 percent by weight of silicon oxynitride ceramic composite obturator hollow microspheres with the granularity of 5 to 50 micrometers, 5 to 7 percent by weight of coal ash with the burning loss of 1.1 percent, 1.5 to 2 percent by weight of calcium oxide with the purity of 99.9 percent, 0.5 to 1.0 percent by weight of sodium sulfate and 1 to 3 percent by weight of silica fume, stirring and mixing the raw materials for 40 seconds inside a stirring machine with the water-ash ratio of 0.5 to 0.6 (W/C), then pouring the mixture into a test mold, conserving for 24-48 hours in a water-bath maintenance box at a constant temperature of 52 DEG C, immersing the demolded mixture in cold water for 1 hour, and finally performing the performance test on the mixture.
Description
Technical field
The present invention relates to a kind of silicon oxynitride Ceramic Composite microballon and prepare the method for oil well cementing cement briquette, belong to material technology field.
Background technology
Current domestic oil well cementing light-weight additive adopts the pearl that floats in flyash, comprises heavy pearl and floats pearl at flyash, and heavy pearl density is at 1.1～2.8g/cm
3between, content accounts for flyash 30～70%, and floating pearl is the glass microballon that is less than water-mass density in flyash, floats pearl and mainly comprises aluminosilicate glass microballon and porous carbon granule, the pearl that floats of removing after carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, surfaces externally and internally is smooth, and volume is large, is a kind of rounded, light weight, closed pore is hollow, wear-resisting, high temperature resistant, thermal conductivity is little, intensity is high, float pearl amount and account for 0.5～1% of flyash total amount, aluminosilicate glass microballon is hollow spherosome.
Wherein floating pearl it be that coal dust is in thermal power plant boiler during through 1100～1500 ° of C burning in flyash, clayey material is melt into micro-drop, spin at a high speed under the hot air acting of turbulent flow in stove, form perfectly round sial spheroid, the gases such as nitrogen, hydrogen and the carbonic acid gas that burning and scission reaction produce, in the high temperature aluminum silicon spheroid of melting, expand rapidly, under capillary effect, form the glass envelope of hollow, then enter flue cooling rapidly, after sclerosis, become the vitreous state cenosphere of high vacuum, i.e. fly ash float.
Flyash is put into water and stir, leave standstill for some time, be less than water-mass density owing to floating pearl density, will swim on the water surface and pull out and dry, be and float pearl, the pearl that floats 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 μ m, particle size range is mainly distributed in 147～84 μ m, but it is large to float the particle diameter of pearl, and ultimate compression strength is low.
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 and floating pearl in flyash, cause in short supply, only have medium and small thermal power plant and arcola do not adopt desulfurization technology supply a small amount of float pearl, that floats pearl in short supplyly causes price increase, and float the impure flyash that mixed of pearl, affect cementing quality, float pearl substantial appreciation of prices, 10,000 yuan of breakthroughs per ton, maximum compressive strength 20Mpa, in view of above-mentioned condition, adopt composite ceramic material to make the pearl that floats of the alternative flyash of closed pore cenosphere, performance is better than floating pearl, economic benefit is large, market outlook are good.
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 the main low-density cement mortar that adopts of long shut-in well, wants to make the density of grout at 1.0 g/cm
3～1.5 g/cm
3between, density must be at 0.5g/cm for the non-lightening material that floats pearl (inorganic mineral material and organic synthesis material composition)
3～0.85 g/cm
3between, (density of G level oil well watertight is at 3.1 g/cm just to make low-density grout
3, light-weight additive density must be less than 1 g/cm
3, just can configure density 1.0 g/cm
3～1.5 g/cm
3between grout, precondition be light-weight additive addition can not exceed total amount 40%, otherwise can affect the ultimate compression strength of cement briquette).
According to well cementation degree of depth difference, conventionally 2000 meters of following oil wells low hot-well, (temperature in oil well is between 70～90 ° of C, and cement slurry density is at 1.8 g/cm for highdensity grout for low temperature oil well cementing
3～1.9 g/cm
3); Between 2000～4000 meters, be middle hot-well, middle temperature oil well cementing with in the grout of density (temperature in oil well is between 90～150 ° of C, and cement slurry density is at 1.6 g/cm
3～1.7 g/cm
3); And be greater than 4000 meters for hot hole, with low-density grout, (temperature in oil well is between 150～240 ° of C, and cement slurry density is at 1.0 g/cm in high-temperature oil well well cementation
3～1.5 g/cm
3).
Because land low temperature oil well oil-gas resource is gradually reducing, progressively by land low temperature oil well, landwards deep layer and bathypelagic are developed in exploitation, traditional well cementing material floats pearl and can not meet the needs of deep layer high-temperature oil well, the requirement need to employ new technology, novel process, novel material meeting deep-level high pressure high-temperature oil well.
Summary of the invention
The object of the invention is to overcome the existing fly ash float state of the art, substitute the pearl that floats of flyash with Ceramic Composite cenosphere, provide a kind of cost low, excellent property, makes the rate of change of the density of cement briquette be less than 0.02, reach cementing design density, silicon oxynitride ceramic composite is prepared closed pore cenosphere, through high temperature sintering, makes the performance index such as resistance to compression, folding strength exceed fly ash float, produce and not affected by other conditions, composite ceramics closed pore cenosphere density range 0.5 g/cm
3～0.85g/cm
3controlled, and then configuration 1.0 g/cm
3～1.5g/cm
3the preparation method of oil well cementing light weight cement test block, meets the requirement of 4000～6000 meters of long shut-in well of dark oil well well cementing materials.
its technical scheme is.
Comprise a kind of silicon oxynitride Ceramic Composite closed pore cenosphere preparation, batching, mix, stirring is sized mixing, die trial, strength trial, by G level oil well cement 40～50 wt%, 13 μ m superfine cement 10～15 wt%, particle diameter is silicon oxynitride Ceramic Composite closed pore cenosphere 25～35 wt% of 5～50 μ m, , 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 SILICA FUME 1～3 wt% mix, with 0.5～0.6(W/C) water cement ratio in stirrer, stir and size mixing 40 seconds, get part sample and carry out cement slurry property test, comprise the mensuration of silicon oxynitride Ceramic Composite closed pore cenosphere resistance to hydrostatic pressure intensity, cement slurry density is measured, withstand voltage density test, sedimentation stability, the free liquid amount of separating out, fluid loss falls, thickening time, the liquidity scale, pours die trial (one group of two block length into, wide, high 53mm*53mm*53mm respectively), maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature, 48 hours, after the demoulding, in cold water, soak 1 hour, carry out compressive property test.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, by 5～50 μ m silicon-dioxide, particle diameter 1～60 μ m silicon carbide, particle diameter 5～50 μ m silicon nitrides, stir by weight 70～80 wt %:2～5, wt %:6～10, wt %:10～15 wt % mixed powders with particle diameter 10～60 μ m aluminum oxide, add again binding agent polyvinyl alcohol solution, lignin sulfonic acid sodium solution and dextrin stir at pressing machine briquetting than 1～1.5 wt%:0.2～0.8, wt%:2～4 wt% by powder mix gross weight, cryodrying moulding, heat preservation sintering 8～12 hours in 1120～1450 ° of C electric furnaces, silicon oxynitride sintered ceramic composite body is processed into 10～50 μ m microballons at balling machine.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, and the weight percent of silicon oxynitride Ceramic Composite microballon liquid slurry consists of: 10～50 μ m silicon oxynitride Ceramic Composite microballon 70～80 wt%: water 20～30 wt%.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, and in silicon oxynitride Ceramic Composite microballon liquid slurry, adding whipping agent is the one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1～3g/L.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, silicon oxynitride Ceramic Composite microballon liquid is starched to abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, 800～850 ° of C of the expansion temperature of dewatering on Si district electric furnace, oven dry sintering temperature, at 1400～1600 ° of C, 1700～1800 ° of C of melt surface temperature, 1400～1500 ° of C of one-tenth bulb temperature, obtain 10～50 μ m silicon oxynitride Ceramic Composite closed pore cenospheres through air classification.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, same batch of density range ± 0.01 g/cm with sampling spot silicon oxynitride Ceramic Composite closed pore cenosphere
3.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, and silicon oxynitride Ceramic Composite closed pore cenosphere its floatability is greater than 95%.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, and the 8 hours ultimate compression strength of cement briquette of preparation is greater than 15MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, and the fluid loss that falls of cement briquette is less than 50ml/30min.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, and cement briquette rate of change of the density is less than 0.02.
Described a kind of silicon oxynitride Ceramic Composite microballon is prepared the method for oil well cementing cement briquette, silicon oxynitride Ceramic Composite closed pore cenosphere resistance to hydrostatic pressure intensity 60～80 MPa.
The present invention has the following advantages.
1, can change the dependence to flyash floating bead in long-term well cementation, adopt silicon oxynitride composite ceramic material to make the required lightening material of oil well cementing, the production technique such as the density of hollow ceramic microspheres, wall thickness, sintering temperature can be controlled.
2, this technical matters advanced person, technology maturation, product performance are stablized, and production cost is low, and output is high, and performance is good, having opened up the synthetic virgin material new way of well cementation.
3
,silicon oxynitride Ceramic Composite microballon density can be controlled in 0.5 g/cm
3～0.85g/cm
3add superfine cement can increase the early strength of Behavior of Hardened Cement Paste test block, according to piling up the theoretical space between SILICA FUME filler particles that adds, increase dioxide-containing silica and cement slurry suspension stability, G level oil well cement, superfine cement, ceramic fine bead have greater activity through the above high temperature sintering of 1000 degree, hydration reaction is fast, can form jelly, can improve early strength.
4
,utilize vertical four district high temperature Cheng Zhulu, adopt high pressure spraying high speed centrifugation rotary spraying technique, spraying sheet aperture is determining granular size, after the abundant atomization of liquid, enter body of heater, drop is at breathing space expanded by heating, and expanding volume is relevant with expansion temperature and density of foaming agent, then through sintering, melting, last balling-up, prevent from tying wall employing thermal cycling air-bleed system in order to improve output, blower fan adopts speed control by frequency variation blower fan.
5, because Ceramic Composite closed pore cenosphere particle diameter is little, and the avidity of grout is strong, and grout stability is strong.
6, spheronization techniques is that material is blown afloat by blower fan, and motion phase mutual friction between material and material forms circle or subcircular particle.
Embodiment.
Embodiment 1.
(1) preparation of silicon oxynitride Ceramic Composite closed pore cenosphere, 1. batching is fired: by 5～15 μ m silicon-dioxide, particle diameter 1～20 μ m silicon carbide, particle diameter 5～15 μ m silicon nitrides, stir by weight 75 wt %:10 wt %:10 wt %:5 wt % mixed powders with particle diameter 10～25 μ m aluminum oxide, add again binding agent polyvinyl alcohol solution, lignin sulfonic acid sodium solution and dextrin stir at pressing machine briquetting than 1 wt%:2 wt%:0.2 wt% by above-mentioned powder mix gross weight, cryodrying moulding, 1120 ° of C heat preservation sinterings 12 hours in stove, silicon oxynitride sintered ceramic composite body is processed into 10～20 μ m microballons at balling machine, 2. dosing: 10～20 μ m silicon oxynitride Ceramic Composite microballon 75 wt%: water 25 wt%, in liquid slurry, add light calcium carbonate whipping agent, concentration is 1g/L, 4. filter: by macrobead and Impurity removal, 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, on vertical four district's electric furnaces, expand through dehydration, dry sintering, melt surface, balling-up, 800 ° of C of the expansion temperature of dewatering on Si district electric furnace, dry sintering temperature at 1400 ° of C, 1700 ° of C of melt surface, become 1400 ° of C of bulb temperature, clean classification through wind-force and obtain 5～15 μ m silicon oxynitride Ceramic Composite closed pore cenospheres.
(2) get 5～15 μ m silicon oxynitride Ceramic Composite closed pore hollow ceramic microspheres 50g, put into the beaker that fills water, with glass stick stirring 1 minute, leave standstill 5 minutes, observe the suspended state of Ceramic Composite closed pore cenosphere grain in beaker, float pearl and heavy pearl in beaker are taken out respectively to dry and weighed, calculate its floatability.
(3) get 5～15 μ m silicon oxynitride Ceramic Composite closed pore cenosphere grain 100g, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage that floats pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure value, off-test, take out pressure chamber, the compound sample that floats pearl is poured in the beaker that fills water, to float pearl floating in beaker by intact, breaks and float pearl and sink to the bottom of beaker, and float pearl and heavy pearl in beaker are taken out respectively to dry and weighed, calculate percentage of damage and static-pressure-resisting, can repeat 2～3 times.
(4) analyze 5～15 μ m silicon oxynitride Ceramic Composite closed pore cenosphere size distribution with laser particle size analyzer, wind-force is cleaned to classification to be obtained Ceramic Composite closed pore cenosphere and takes 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough observed and recorded sample size distribution into.
(5) low density oil well cementing cement briquette batching: be Ceramic Composite closed pore cenosphere 35 wt% of 5～15 μ m, flyash 5 wt%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5wt% and micro-silicon 3 wt% of loss on ignition 1.1% by G level oil well cement 40 wt%, 13 μ m superfine cement 15 wt%, particle diameter.
(6) mix: it is even that flyash 5 wt%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5wt% and micro-silicon 3 wt% that get G level oil well cement 40 wt%, 13 μ m superfine cement 15 wt%, particle diameter and be Ceramic Composite closed pore cenosphere 35 wt%, the loss on ignition 1.1% of 5～15 μ m put into stirrer for mixing.
(7) get in (6), mix sample a little, pour in beaker, by 0.5(W/C) water cement ratio modulation grout, stir with glass stick, pour into and in mud scale, weigh density.
(8) under 28 ° of C ± 1 ° C of temperature, with 0.5(W/C) water cement ratio pour corrugation agitator into, under even low speed, in 20 seconds, all mix, then build the lid of agitator, continue under the speed of 4000r/min, to stir 40 seconds, leave standstill 5 minutes and observe grout homogeneity.
(9) grout being stirred is poured in the die trial of a group two, the specification of die trial is long 53mm, the high 53mm of wide 53mm.
(10) observe weigh and record the free liquid amount of separating out, fall fluid loss, thickening time, the liquidity scale.
(11) maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked after the demoulding 1 hour in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(12) maintenance 48 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked after the demoulding 1 hour in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Embodiment 2.
(1) 1. the preparation of silicon oxynitride Ceramic Composite closed pore cenosphere is prepared burden and is fired: by particle diameter 20～35 μ m silicon-dioxide, particle diameter 25～40 μ m silicon carbide, particle diameter 20～35 μ m silicon nitrides, stir by weight 78 wt %:12 wt %:8 wt %:2 wt % mixed powders with particle diameter 30～45 μ m aluminum oxide, to add again binding agent polyvinyl alcohol solution, lignin sulfonic acid sodium solution and dextrin stir at pressing machine briquetting than 1.2 wt%:3 wt%:0.5 wt% by above-mentioned powder mix gross weight, cryodrying moulding, 1300 ° of C heat preservation sinterings 11 hours in stove, silicon oxynitride sintered ceramic composite body is processed into 20～30 μ m microballons at balling machine, 2. dosing: 20～30 μ m silicon oxynitride Ceramic Composite heart microballon 72 wt%: water 28wt%, in liquid slurry, add lightweight potassium sulfate whipping agent, concentration is 1.5g/L, 4. filter: by macrobead and Impurity removal, 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, on vertical four district's electric furnaces, expand through dehydration, dry sintering, melt surface, balling-up, 820 ° of C of the expansion temperature of dewatering on Si district electric furnace, dry sintering temperature at 1500 ° of C, 1750 ° of C of melt surface temperature, become 1450 ° of C of bulb temperature, clean classification through wind-force and obtain 20～30 μ m Ceramic Composite closed pore cenospheres.
(2) get 20～30 μ m silicon oxynitride Ceramic Composite closed pore cenosphere 50g, put into the beaker that fills water, with glass stick stirring 1 minute, leave standstill 5 minutes, observe the suspended state of silicon oxynitride Ceramic Composite closed pore cenosphere in beaker, float pearl and heavy pearl in beaker are taken out respectively to dry and weighed, calculate its floatability.
(3) get 20～30 μ m silicon oxynitride Ceramic Composite closed pore cenosphere 100g, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage that floats pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure value, off-test, take out pressure chamber, the sample that floats pearl is poured in the beaker that fills water, to float pearl floating in beaker by intact, breaks and float pearl and sink to the bottom of beaker, and float pearl and heavy pearl in beaker are taken out respectively to dry and weighed, calculate percentage of damage and static-pressure-resisting, can repeat 2～3 times.
(4) analyze 20～30 μ m silicon oxynitride Ceramic Composite closed pore cenosphere size distribution with laser particle size analyzer, wind-force is cleaned to classification to be obtained silicon oxynitride Ceramic Composite closed pore cenosphere and takes 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough observed and recorded sample size distribution into.
(5) low density oil well cementing cement briquette batching: get G level oil well cement 45 wt%, 13 μ m superfine cement 15 wt%, particle diameter is silicon oxynitride Ceramic Composite closed pore cenosphere 30 wt% of 20～30 μ m, flyash 6 wt%, purity 99.9% calcium oxide 2 wt%, sodium sulfate 1wt% and micro-silicon 1 wt% of loss on ignition 1.1%.
(6) mix: it is even that flyash 6 wt%, purity 99.9% calcium oxide 2 wt%, sodium sulfate 1wt% and micro-silicon 1 wt% that gets G level oil well cement 45 wt%, 13 μ m superfine cement 15 wt%, particle diameter and be silicon oxynitride closed pore Hollow Compound ceramic fine bead 30 wt%, the loss on ignition 1.1% of 20～30 μ m puts into stirrer for mixing.
(7) get in (6), mix sample a little, pour in beaker, by 0.6(W/C) water cement ratio modulation grout, stir with glass stick, pour into and in mud scale, weigh density.
(8) under 28 ° of C ± 1 ° C of temperature, with 0.6(W/C) water cement ratio pour corrugation agitator into, under even low speed, in 20 seconds, all mix, then build the lid of agitator, continue under the speed of 4000r/min, to stir 40 seconds, leave standstill 5 minutes and observe grout homogeneity.
(9) grout being stirred is poured in the die trial of a group two, the specification of die trial is long 53mm, the high 53mm of wide 53mm.
(10) the observed and recorded free liquid amount of separating out, fluid loss, thickening time, the liquidity scale fall.
(11) maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked after the demoulding 1 hour in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(12) maintenance 48 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked after the demoulding 1 hour in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Embodiment 3.
(1) 1. the preparation of silicon oxynitride Ceramic Composite closed pore cenosphere is prepared burden and is fired: by particle diameter 40～50 μ m silicon-dioxide, particle diameter 45～60 μ m silicon carbide, particle diameter 40～50 μ m silicon nitrides, stir by weight 80 wt %:10wt %:7wt %:3 wt % mixed powders with particle diameter 50～60 μ m aluminum oxide, to add again binding agent polyvinyl alcohol solution, lignin sulfonic acid sodium solution and dextrin stir at pressing machine briquetting than 1.5 wt%:4 wt%:0.8 wt% by above-mentioned powder mix gross weight, cryodrying moulding, 1450 ° of C heat preservation sinterings 10 hours in stove, silicon oxynitride sintered ceramic composite body is processed into 40～50 μ m microballons at balling machine, 2. dosing: 40～50 μ m silicon oxynitride Ceramic Composite microballons are pressed 80 wt%: water 20wt%, in liquid slurry, add lightweight sodium sulfate whipping agent, concentration is 2g/L, 4. filter: by macrobead and Impurity removal, 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, on vertical four district's electric furnaces, expand through dehydration, dry sintering, melt surface, balling-up, 850 ° of C of dehydration expansion on Si district electric furnace, dry sintering temperature at 1600 ° of C, 1800 ° of C of melt surface temperature, become 1500 ° of C of bulb temperature, clean classification through wind-force and obtain 35～50 μ m silicon oxynitride Ceramic Composite closed pore cenospheres.
(2) get 35～50 μ m silicon oxynitride Ceramic Composite closed pore cenosphere 50g, put into the beaker that fills water, with glass stick stirring 1 minute, leave standstill 5 minutes, observe the suspended state of silicon oxynitride Ceramic Composite closed pore cenosphere pearl in beaker, float pearl and heavy pearl in beaker are taken out respectively to dry and weighed, calculate its floatability.
(3) get the silicon oxynitride Ceramic Composite closed pore cenosphere 100g of 35～50 μ m, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage that floats pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure value, off-test, take out pressure chamber, the sample that floats pearl is poured in the beaker that fills water, to float pearl floating in beaker by intact, break and float pearl and sink to the bottom of beaker, float pearl and heavy pearl in beaker are taken out respectively to dry and weighed, calculate percentage of damage and static-pressure-resisting.
(4) analyze 35～50 μ m silicon oxynitride Ceramic Composite closed pore cenosphere size distribution with laser particle size analyzer, wind-force is cleaned to classification to be obtained silicon oxynitride Ceramic Composite closed pore cenosphere and takes 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough observed and recorded sample size distribution into.
(5) low density oil well cementing cement briquette batching: by getting G level oil well cement 45 wt%, 13 μ m superfine cement 12 wt%, particle diameter is silicon oxynitride Ceramic Composite microballon 33 wt% of 35～50 μ m, flyash 7 wt%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5wt% and micro-silicon 1 wt% of loss on ignition 1.1%.
(6) mix: it is even that flyash 7 wt%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5wt% and micro-silicon 1 wt% that gets G level oil well cement 45 wt%, 13 μ m superfine cement 12 wt%, particle diameter and be silicon oxynitride Ceramic Composite microballon 33 wt%, the loss on ignition 1.1% of 35～50 μ m puts into stirrer for mixing.
(7) get in (6), mix sample a little, pour in beaker, by 0.55(W/C) water cement ratio modulation grout, stir with glass stick, pour into and in mud scale, weigh density.
(8) under 28 ° of C ± 1 ° C of temperature, with 0.55(W/C) water cement ratio pour corrugation agitator into, under even low speed, in 20 seconds, all mix, then build the lid of agitator, continue under the speed of 4000r/min, to stir 40 seconds, leave standstill 5 minutes and observe grout homogeneity.
(9) grout being stirred is poured in the die trial of a group two, the specification of die trial is long 53mm, the high 53mm of wide 53mm.
(10) the observed and recorded free liquid amount of separating out, fluid loss, thickening time, the liquidity scale fall.
(11) maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked after the demoulding 1 hour in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(12) maintenance 48 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked after the demoulding 1 hour in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Note: G level oil well cement is Qi Yin cement mill, Shandong, purity 99.9% calcium oxide is the prosperous sub-calcium industry of Shandong Zibo, the flyash Huaneng Group Xin Dian power plant of loss on ignition 1.1%.
Claims (11)
1. silicon oxynitride Ceramic Composite microballon is prepared a method for oil well cementing cement briquette, comprises the preparation of silicon oxynitride Ceramic Composite closed pore cenosphere, batching, mix, stirring is sized mixing, die trial, strength trial, is characterized in that: by G level oil well cement 40～50 wt%, 13 μ m superfine cement 10～15 wt%, particle diameter is silicon oxynitride Ceramic Composite microballon 25～35 wt% of 5～50 μ m, , 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 SILICA FUME 1～3 wt% mix, with 0.5～0.6(W/C) water cement ratio in stirrer, stir and size mixing 40 seconds, get part sample and carry out cement slurry property test, comprise the mensuration of silicon oxynitride Ceramic Composite closed pore cenosphere resistance to hydrostatic pressure intensity, cement slurry density is measured, withstand voltage density test, sedimentation stability, the free liquid amount of separating out, fluid loss falls, thickening time, the liquidity scale, pours die trial (one group of two block length into, wide, high 53mm*53mm*53mm respectively), maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature, 48 hours, after the demoulding, in cold water, soak 1 hour, carry out compressive property test.
2. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: by 5～50 μ m silicon-dioxide, particle diameter 1～60 μ m silicon carbide, particle diameter 5～50 μ m silicon nitrides and particle diameter 10～60 μ m aluminum oxide stir by weight 70～80 wt %:2～5, wt %:6～10, wt %:10～15 wt % mixed powders, add again binding agent polyvinyl alcohol solution, lignin sulfonic acid sodium solution and dextrin stir at pressing machine briquetting than 1～1.5 wt%:0.2～0.8, wt%:2～4 wt% by powder mix gross weight, cryodrying moulding, heat preservation sintering 8～12 hours in 1120～1450 ° of C electric furnaces, silicon oxynitride sintered ceramic composite body is processed into 10～50 μ m microballons at balling machine.
3. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: the weight percent of silicon oxynitride Ceramic Composite microballon liquid slurry consists of: 10～50 μ m silicon oxynitride Ceramic Composite microballon 70～80 wt%: water 20～30 wt%.
4. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: in silicon oxynitride Ceramic Composite microballon liquid slurry, adding whipping agent is the one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1～3g/L.
5. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: silicon oxynitride Ceramic Composite microballon liquid is starched to abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, 800～850 ° of C of the expansion temperature of dewatering on Si district electric furnace, oven dry sintering temperature, at 1400～1600 ° of C, 1700～1800 ° of C of melt surface temperature, 1400～1500 ° of C of one-tenth bulb temperature, obtain 10～50 μ m silicon oxynitride Ceramic Composite closed pore cenospheres through air classification.
6. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: density range ± 0.01 g/cm of same batch of different sampling spot silicon oxynitride Ceramic Composite closed pore cenospheres
3.
7. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: silicon oxynitride Ceramic Composite closed pore cenosphere its floatability is greater than 95%.
8. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: the 8 hours ultimate compression strength of cement briquette of preparation is greater than 15MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
9. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: the fluid loss that falls of cement briquette is less than 50ml/30min.
10. a kind of silicon oxynitride Ceramic Composite microballon according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: cement briquette rate of change of the density is less than 0.02.
11. a kind of silicon oxynitride Ceramic Composite microballons according to claim 1 are prepared the method for oil well cementing cement briquette, it is characterized in that: silicon oxynitride composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity 60～80 MPa.
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| CN107807230A (en) * | 2017-11-21 | 2018-03-16 | 淄博职业学院 | Carborundum kaolin ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak |
| CN107860900A (en) * | 2017-11-21 | 2018-03-30 | 淄博职业学院 | Mica kaolin ceramic fine bead prepares oil well anti-gas-leak well cementation test block performance test methods |
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| CN107884554A (en) * | 2017-11-21 | 2018-04-06 | 淄博职业学院 | Silicon kaolin ceramic fine bead prepares oil well anti-gas-leak well cementation test block performance test methods |
| CN108008121A (en) * | 2017-11-21 | 2018-05-08 | 淄博职业学院 | Silicon vanadine ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block |
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| CN108037271A (en) * | 2017-11-21 | 2018-05-15 | 淄博职业学院 | Sial brunisolic soil ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak |
| CN108051571A (en) * | 2017-11-21 | 2018-05-18 | 淄博职业学院 | Zirconium kaolin ceramic fine bead prepares oil well anti-gas-leak well cementation test block performance test methods |
| CN108046636A (en) * | 2017-12-20 | 2018-05-18 | 潜江市联瑞石油机械有限公司 | A kind of well cementation 4D extra materials |
| CN110922114A (en) * | 2019-11-26 | 2020-03-27 | 济南大学 | Method for preparing porous cement-based material by using activated carbon material |
| CN110922114B (en) * | 2019-11-26 | 2022-03-08 | 济南大学 | Method for preparing porous cement-based material by using activated carbon material |
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