CN103880358A - Method for preparing well-cementing cement briquette of oil well from composite ceramic closed-pore hollow microsphere - Google Patents
Method for preparing well-cementing cement briquette of oil well from composite ceramic closed-pore hollow microsphere Download PDFInfo
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- CN103880358A CN103880358A CN201410078285.0A CN201410078285A CN103880358A CN 103880358 A CN103880358 A CN 103880358A CN 201410078285 A CN201410078285 A CN 201410078285A CN 103880358 A CN103880358 A CN 103880358A
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Abstract
The invention provides a method for preparing a well-cementing cement briquette of an oil well from a composite ceramic closed-pore hollow microsphere. The method comprises the steps of carrying out preparation on the composite ceramic closed-pore hollow microsphere, dosing, mixing, stirring size-mixing, test mold pouring and strength test, namely in a proportion, mixing 40-50wt% of level-G oil well cement, 10-15wt% of ultra-fine cement, 25-35wt% of the composite ceramic closed-pore hollow microsphere, 5-7wt% of coal ash, 1.5-2wt% of calcium oxide, 0.5-1.0wt% of sodium sulfate and 1-3wt% of micro-silicon, carrying out stirring size-mixing for 40 seconds in a stirring machine in a water cement ratio of 0.5-0.6(W/C), pouring the slurry into a test mold, maintaining for 24 hours and 48 hours in a water bath maintaining tank at a constant temperature of 52 DEG C, demolding, and soaking the product for 1 hour in cold water, and carrying out performance test, wherein the particle size of the ultra-fine cement is 13 microns, the particle size of the composite ceramic closed-pore hollow microsphere is 5-50 microns, the ignition loss of the coal ash is 1.1%, and the purity of the calcium oxide is 9.9%.
Description
Technical field
The present invention relates to a kind of composite ceramics closed pore cenosphere 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.
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 per ton at least 1 ten thousand yuan of pearl price, maximum compressive strength 20Mpa, make the pearl that floats of the alternative flyash of cenosphere so adopt composite ceramic material, environment is not had any impact, be not subject to the restriction of envrionment conditions, 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 0.5 g/cm for the non-lightening material that floats pearl (inorganic mineral material and organic synthesis material composition)
3～0.8 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, cement slurry density is at 1.0 g/cm
3～1.5 g/cm
3between, composite ceramics microballon resistance to hydrostatic pressure intensity 200Mpa～300 Mpa.
Summary of the invention
The object of the invention is to overcome the existing pearl state of the art of floating, substitute the pearl that floats of flyash with ceramic hollow microballon, provide a kind of cost low, excellent property, makes rate of change of the density be less than 0.02, reach design density, prepare high resistance with zirconium diboride, silicon carbide and zirconia composite ceramics material and press off hole hollow ceramic microspheres, through high temperature sintering, make the performance index such as resistance to compression, folding strength exceed the pearl that floats of flyash, output is affected by other conditions very much not, density range 0.5 g/cm
3～0.8g/cm
3controlled, and then configuration 1.0g/cm
3～1.5g/cm
3the preparation method of oil well cementing light weight cement test block, meets the well cementing material requirement of long shut-in well 8000～ten thousand metres deep-sea oil well.
its technical scheme is.
Comprise the preparation of composite ceramics closed pore cenosphere, 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 composite ceramics 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%, the ratio of sodium sulfate 0.5～1.0 wt% and micro-silicon 1～3 wt% is mixed, 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 composite ceramics 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 composite ceramics closed pore cenosphere is prepared the method for oil well cementing cement briquette, 1～10 μ m zirconium diboride, particle diameter 5～20 μ m silicon carbide and particle diameter 1～10 μ m zirconium white stir by weight 55～70 wt%:5～25, wt%:20～25 wt% mixed powders, in vacuum oven, 1800～2000 ° of C heat preservation sinterings 60～70 minutes, are processed into 10～20 μ m microballons by zirconium diboride, silicon carbide and zirconia sintered body at balling machine.
Described a kind of composite ceramics closed pore cenosphere is prepared the method for oil well cementing cement briquette, and the weight percent of zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid slurry consists of: 10～20 μ m zirconium diborides, silicon carbide and zirconia composite ceramics closed pore cenosphere 70～80 wt%: water 20～30 wt%.
Described a kind of composite ceramics closed pore cenosphere is prepared the method for oil well cementing cement briquette, and in zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid slurry, adding whipping agent is light calcium carbonate, and the concentration of use is 1～3g/L.
Described a kind of composite ceramics closed pore cenosphere is prepared the method for oil well cementing cement briquette, zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid are 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 5～50 μ m zirconium diborides, silicon carbide and zirconia composite ceramics closed pore cenosphere through classification.
Described a kind of composite ceramics closed pore cenosphere is prepared the method for oil well cementing cement briquette, and composite ceramics closed pore cenosphere its floatability is greater than 98%.
Described a kind of composite ceramics closed pore cenosphere 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 40MPa.
Described a kind of composite ceramics closed pore cenosphere is prepared the method for oil well cementing cement briquette, and the fluid loss that falls of cement stone is less than 50ml/30min.
Described a kind of composite ceramics closed pore cenosphere 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 composite ceramics closed pore cenosphere is prepared the method for oil well cementing cement briquette, composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity 200～300 MPa.
The present invention has the following advantages.
1, can change the dependence to flyash floating bead in long-term well cementation, adopt composite ceramic material to make oil well cementing required lightening material, the production technique such as the density of ceramic fine bead, 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
,zirconium diboride, silicon carbide and zirconia composite ceramics microballon density can be controlled in 0.5 g/cm
3～0.8g/cm
3add 13 μ m superfine cements 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 machine Behavior of Hardened Cement Paste high temperature resistance, G level oil well cement, superfine cement, ceramic fine bead have greater activity through 1000 ° of above high temperature sinterings of C, 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 zirconium diboride, silicon carbide and zirconia composite ceramics microballon particle diameter are little, strong with the avidity of cement, grout stability is strong.
Embodiment.
Embodiment 1.
(1) zirconium diboride, 1. the preparation of silicon carbide and zirconia composite ceramics closed pore cenosphere grain is prepared burden and is fired: by particle diameter 1～3 μ m zirconium diboride, particle diameter 5～10 μ m silicon carbide and particle diameter 1～3 μ m zirconium white stir in 55 wt%:25 wt%:20 wt% mixed powder stirrers, 1800 ° of C heat preservation sinterings 60 minutes in vacuum oven, by zirconium diboride, silicon carbide and zirconia sintered body are processed into 10 μ m microballons at balling machine, 2. dosing: 10 μ m zirconium diborides, silicon carbide and zirconia composite ceramics microballon 70 wt%: water 30 wt%, in liquid slurry, add lightweight potassium sulfate 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, 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 composite ceramics closed pore cenospheres.
(2) get 5～15 μ m composite ceramics closed pore cenosphere grain 50g, put into the beaker that fills water, with glass stick stirring 1 minute, leave standstill 5 minutes, observe the suspended state of composite ceramics 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 the composite ceramics closed pore cenosphere grain 100g of 5～15 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 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, calculating percentage of damage and static-pressure-resisting is compressive strength, repeats 2～3 times.
(4) low density oil well cementing cement briquette batching: be composite ceramics 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.
(5) 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 composite ceramics closed pore cenosphere 35 wt%, the loss on ignition 1.1% of 5～15 μ m put into stirrer for mixing.
(6) get in (5), 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, recording density value g/cm
3.
(7) 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.
(8) 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.
(9) observe weigh and record the free liquid amount of separating out, fall fluid loss, thickening time, the liquidity scale.
(10) 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.
(11) 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) zirconium diboride, 1. the preparation of silicon carbide and zirconia composite ceramics closed pore cenosphere grain is prepared burden and is fired: by 4～6 μ m zirconium diborides, particle diameter 11～15 μ m silicon carbide and particle diameter 7～10 μ m zirconium whites stir in 60 wt%:25 wt%:15 wt% mixed powder stirrers, 1900 ° of C heat preservation sinterings 65 minutes in vacuum oven, by zirconium diboride, silicon carbide and zirconia sintered body are processed into 15 μ m microballons at balling machine, 2. dosing: 15 μ m zirconium diborides, silicon carbide and zirconia composite ceramics microballon 75 wt%: water 25wt%, in liquid slurry, add lightweight potassium 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, 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 composite ceramics closed pore cenospheres.
(2) get 20～30 μ m composite ceramics 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 composite ceramics 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 the composite ceramics closed pore cenosphere 100g of 20～30 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, 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, calculating percentage of damage and static-pressure-resisting is compressive strength, repeats 2～3 times.
(4) 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 composite ceramics 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%.
(5) 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 composite ceramics closed pore cenosphere 30 wt%, the loss on ignition 1.1% of 20～30 μ m puts into stirrer for mixing.
(6) get in (5), 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, recording density value g/cm
3.
(7) 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.
(8) 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.
(9) observe weigh record the free liquid amount of separating out, fall fluid loss, thickening time, the liquidity scale.
(10) 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.
(11) 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) zirconium diboride, 1. the preparation of silicon carbide and zirconia composite ceramics closed pore cenosphere grain is prepared burden and is fired: by 7～10 μ m zirconium diborides, particle diameter 16～20 μ m silicon carbide and particle diameter 4～6 μ m zirconium whites stir in 70 wt%:22 wt%:8wt% mixed powder stirrers, 2000 ° of C heat preservation sinterings 70 minutes in vacuum oven, by zirconium diboride, silicon carbide and zirconia sintered body are processed into 20 μ m microballons at balling machine, 2. dosing: 20 μ m zirconium diborides, silicon carbide and zirconia composite ceramics microballon 80 wt%: water 20wt%, in liquid slurry, add lightweight potassium sulfate whipping agent, concentration is 3g/L, 4. filter: by macrobead and Impurity removal, 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, 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 composite ceramics closed pore cenospheres.
(2) get 35～50 μ m composite ceramics 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 composite ceramics 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 the compound closed pore hollow ceramic microspheres 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, calculating percentage of damage and static-pressure-resisting is that compressive strength repeats 2～3 times.
(4) 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 composite ceramics closed pore cenosphere 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%.
(5) 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 composite ceramics closed pore cenosphere 33 wt%, the loss on ignition 1.1% of 35～50 μ m puts into stirrer for mixing.
(6) get in (5), 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, recording density value g/cm
3.
(7) 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.
(8) 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.
(9) the observed and recorded free liquid amount of separating out, fluid loss, thickening time, the liquidity scale fall.
(10) 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.
(11) 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, the prosperous sub-calcium industry of purity 99.9% calcium oxide Shandong Zibo, the flyash Huaneng Group Xin Dian power plant of loss on ignition 1.1%.
Claims (10)
1. composite ceramics closed pore cenosphere is prepared a method for oil well cementing cement briquette, comprises the preparation of composite ceramics 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 composite ceramics 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%, the ratio of sodium sulfate 0.5～1.0 wt% and SILICA FUME 1～3 wt% is mixed, 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, the mensuration of composite ceramics 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 composite ceramics closed pore cenosphere according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: particle diameter 1～10 μ m zirconium diboride, particle diameter 5～20 μ m silicon carbide and particle diameter 1～10 μ m zirconium white are stirred by weight 55～70 wt%:5～25, wt%:20～25 wt% mixed powders, in vacuum oven, 1800～2000 ° of C heat preservation sinterings 60～70 minutes, are processed into 10～20 μ m microballons by zirconium diboride, silicon carbide and zirconia sintered body at balling machine.
3. a kind of composite ceramics closed pore cenosphere according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: the weight percent of zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid slurry consists of: 10～20 μ m zirconium diborides, silicon carbide and zirconia composite ceramics microballon 70～80 wt%: water 20～30 wt%.
4. a kind of composite ceramics closed pore cenosphere according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: in zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid slurry, adding whipping agent is light calcium carbonate, and the concentration of use is 1～3g/L.
5. a kind of composite ceramics closed pore cenosphere according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: by zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid are starched 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, dry sintering temperature at 1400～1600 ° of C, 1700～1800 ° of C of melt surface temperature, become 1400～1500 ° of C of bulb temperature, obtain 5～50 μ m zirconium diborides through classification, silicon carbide and zirconia composite ceramics closed pore cenosphere.
6. a kind of composite ceramics closed pore cenosphere according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: composite ceramics closed pore cenosphere its floatability is greater than 98%.
7. a kind of composite ceramics closed pore cenosphere 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 40MPa.
8. a kind of composite ceramics closed pore cenosphere 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.
9. a kind of composite ceramics closed pore cenosphere 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.
10. a kind of composite ceramics closed pore cenosphere according to claim 1 is prepared the method for oil well cementing cement briquette, it is characterized in that: composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity 200～300 MPa.
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| CN104531111A (en) * | 2015-01-07 | 2015-04-22 | 山东理工大学 | Method for manufacturing high temperature and high pressure resisting oil well cementing test block through silicon kaolin ceramic microbeads |
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