CN103880358B - A kind of composite ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette - Google Patents
A kind of composite ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette Download PDFInfo
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Abstract
The invention provides a kind of method that composite ceramics closed pore cenosphere prepares oil well cementing cement briquette, comprise the preparation of composite ceramics closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, by G level oil well cement 40 ~ 50wt%, particle diameter 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the composite ceramics closed pore cenosphere 25 ~ 35wt% of 5 ~ 50 μm, flyash 5 ~ the 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2wt%, the ratio mixing of sodium sulfate 0.5 ~ 1.0wt% and micro-silicon 1 ~ 3wt%, with 0.5 ~ 0.6(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, pour die trial into, maintenance 24 hours in the water-bath maintaining box of constant temperature 52 ° of C, 48 hours, soak 1 hour in cold water after the demoulding, carry out performance test.
Description
Technical field
The present invention relates to a kind of method that composite ceramics closed pore cenosphere prepares oil well cementing cement briquette, belong to field of material technology.
Background technology
Current domestic oil well cementing 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%, drift pearl is the glass microballon being less than water-mass density in flyash, drift pearl mainly comprises aluminosilicate glass microballon and porous carbon granule, and the drift pearl after removing carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, and surfaces externally and internally is smooth, volume is large, be 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 has 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, drift pearl price per ton at least 1 ten thousand yuan, maximum compressive strength 20MPa, so adopt composite ceramic material making cenosphere to substitute the drift pearl of flyash, environment is not had any impact, not by 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 long shut-in well mainly adopts low-density cement mortar, wants to make the density of grout at 1.0g/cm
3~ 1.5g/cm
3between, density must at 0.5g/cm for the lightening material (inorganic mineral material and organic synthesis material composition) of non-drift pearl
3~ 0.8g/cm
3between, (density of G level oil well watertight is at 3.1g/cm just to make low-density grout
3, light-weight additive density must be less than 1g/cm
3, just can configure density 1.0g/cm
3~ 1.5g/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).
Different according to the well cementation degree of depth, usually the oil well of less than 2000 meters low hot-well, low temperature oil-well is cemented the well, and with highdensity grout, (, between 70 ~ 90 DEG C, namely cement slurry density is at 1.8g/cm for the temperature in oil well
3~ 1.9g/cm
3); Be middle hot-well between 2000 ~ 4000 meters, (, between 90 ~ 150 DEG C, namely cement slurry density is at 1.6g/cm for the temperature in oil well for the grout of middle temperature oil well cementing Midst density
3~ 1.7g/cm
3); And be greater than 4000 meters for hot hole, with low-density grout, (, between 150 ~ 240 DEG C, namely cement slurry density is at 1.0g/cm for the temperature in oil well in high-temperature oil well well cementation
3~ 1.5g/cm
3).
Because land low temperature oil-well hydrocarbon resources is gradually reducing, progressively by land low temperature oil-well, landwards deep layer and bathypelagic are developed in exploitation, traditional well cementing material drift pearl can not meet the needs of deep layer high-temperature oil well, need employ new technology, novel process, novel material to meet the requirement of deep-level high pressure high-temperature oil well, cement slurry density is at 1.0g/cm
3~ 1.5g/cm
3between, composite ceramics microballon resistance to hydrostatic pressure intensity 200MPa ~ 300MPa.
Summary of the invention
The object of the invention is to overcome the existing drift pearl state of the art, the drift pearl of flyash is substituted with ceramic hollow microballon, there is provided a kind of cost low, excellent property, make 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 drift pearl of flyash, output very much not affects by other condition, density range 0.5g/cm
3~ 0.8g/cm
3controlled, and then configuration low density 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, mixing, stirring is sized mixing, die trial, strength trial, by G level oil well cement 40 ~ 50wt%, 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the composite ceramics closed pore cenosphere 25 ~ 35wt% of 5 ~ 50 μm, flyash 5 ~ the 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2wt%, the ratio mixing of sodium sulfate 0.5 ~ 1.0wt% and micro-silicon 1 ~ 3wt%, with 0.5 ~ 0.6(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, get aliquot and carry out cement slurry property test, comprise the mensuration of composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity, cement slurry density measures, withstand voltage density test, sedimentation stability, free liquid amount of precipitation, fluid loss falls, thickening time, the liquidity scale, pours die trial (one group of two block length into, wide, high 53mm*53mm*53mm respectively), 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 compressive property test.
Described a kind of composite ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette, 1 ~ 10 μm of zirconium diboride, particle diameter 5 ~ 20 μm of silicon carbide and particle diameter 1 ~ 10 μm of zirconium white stir by weight 55 ~ 70wt%:20 ~ 25wt%:5 ~ 25wt% mixed powder, 1800 ~ 2000 DEG C of heat preservation sinterings 60 ~ 70 minutes, are processed into 10 ~ 20 μm of microballons by zirconium diboride, silicon carbide and zirconia sintered body at balling machine in a vacuum furnace.
Described a kind of composite ceramics closed pore cenosphere prepares 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 μm of zirconium diboride, silicon carbide and zirconia composite ceramics closed pore cenospheres 70 ~ 80wt%: water 20 ~ 30wt%.
Described a kind of composite ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette, and in zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid slurry, add whipping agent is light calcium carbonate, and the concentration of use is 1 ~ 3g/L.
Described a kind of composite ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette, 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, expansion temperature that four district's electric furnaces dewater 800 ~ 850 DEG C, dry sintering temperature 1400 ~ 1600 DEG C, melt surface temperature 1700 ~ 1800 DEG C, become bulb temperature 1400 ~ 1500 DEG C, obtain 5 ~ 50 μm of zirconium diborides, silicon carbide and zirconia composite ceramics closed pore cenosphere through classification.
Described a kind of composite ceramics closed pore cenosphere prepares 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 prepares the method for oil well cementing cement briquette, and the cement briquette 8 hours ultimate compression strength 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 prepares 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 prepares 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 prepares 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 the lightening material of composite ceramic material making needed for oil well cementing, the production technique such as density, wall thickness, sintering temperature of ceramic fine bead 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
,zirconium diboride, silicon carbide and zirconia composite ceramics bead density can be controlled in 0.5g/cm
3~ 0.8g/cm
3add the early strength that 13 μm of superfine cements can increase Behavior of Hardened Cement Paste test block, according to piling up the theoretical space added between SILICA FUME filler particles, 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 more than 1000 DEG C high temperature sinterings, 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 decides granular size, body of heater is entered after liquid is fully atomized, 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 knot wall from adopting thermal cycling air-bleed system 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, and the avidity of cement is strong, and 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 μm of zirconium diboride, particle diameter 5 ~ 10 μm of silicon carbide and particle diameter 1 ~ 3 μm of zirconium white stir in 55wt%:25wt%:20wt% mixed powder stirrer, 1800 DEG C of heat preservation sinterings 60 minutes in a vacuum furnace, by zirconium diboride, silicon carbide and zirconia sintered body are processed into 10 μm of microballons at balling machine, 2. dosing: 10 μm of zirconium diborides, silicon carbide and zirconia composite ceramics microballon 70wt%: water 30wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 1g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, expansion temperature that four district's electric furnaces dewater 800 DEG C, dry sintering temperature at 1400 DEG C, melt surface 1700 DEG C, become bulb temperature 1400 DEG C, clean classification through wind-force and obtain 5 ~ 15 μm of composite ceramics closed pore cenospheres.
(2) 5 ~ 15 μm of composite ceramics closed pore cenosphere grain 50g are got, put into the beaker filling water, 1 minute is stirred with glass stick, leave standstill 5 minutes, observe the suspended state of composite ceramics closed pore cenosphere grain in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the composite ceramics closed pore cenosphere grain 100g of 5 ~ 15 μm is got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, sample compound being floated pearl is poured into and is filled in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, calculate percentage of damage and static-pressure-resisting and compressive strength, repeat 2 ~ 3 times.
(4) low density oil well cementing cement briquette batching: be the composite ceramics closed pore cenosphere 35wt% of 5 ~ 15 μm, the flyash 5wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5wt%, sodium sulfate 0.5wt% and micro-silicon 3wt% by G level oil well cement 40wt%, 13 μm of superfine cement 15wt%, particle diameter.
(5) mix: get G level oil well cement 40wt%, 13 μm of superfine cement 15wt%, particle diameter is composite ceramics closed pore cenosphere 35wt%, the flyash 5wt% of loss on ignition 1.1% of 5 ~ 15 μm, that purity 99.9% calcium oxide 1.5wt%, sodium sulfate 0.5wt% and micro-silicon 3wt% put into stirrer for mixing is even.
(6) get in (5) that to mix sample a little, pour in beaker, by 0.5(W/C) water cement ratio modulation grout, stir with glass stick, pour in mud scale and weigh density, recording density value g/cm
3.
(7) at temperature 28 DEG C ± 1 DEG C, with 0.5(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(8) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(9) observe weigh and record free liquid amount of precipitation, fall fluid loss, the thickening time, the liquidity scale.
(10) 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 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 constant temperature 52 DEG C, soaks 1 hour after the demoulding 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 μm of zirconium diborides, particle diameter 11 ~ 15 μm of silicon carbide and particle diameter 7 ~ 10 μm of zirconium whites stir in 60wt%:25wt%:15 wt% mixed powder stirrer, 1900 DEG C of heat preservation sinterings 65 minutes in a vacuum furnace, by zirconium diboride, silicon carbide and zirconia sintered body are processed into 15 μm of microballons at balling machine, 2. dosing: 15 μm of zirconium diborides, silicon carbide and zirconia composite ceramics microballon 75wt%: water 25wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 2g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, expansion temperature that four district's electric furnaces dewater 820 DEG C, dry sintering temperature at 1500 DEG C, melt surface temperature 1750 DEG C, become bulb temperature 1450 DEG C, clean classification through wind-force and obtain 20 ~ 30 μm of composite ceramics closed pore cenospheres.
(2) 20 ~ 30 μm of composite ceramics closed pore cenosphere 50g are got, put into the beaker filling water, 1 minute is stirred with glass stick, leave standstill 5 minutes, observe the suspended state of composite ceramics closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the composite ceramics closed pore cenosphere 100g of 20 ~ 30 μm is got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, being poured into by the sample of drift pearl fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, calculate percentage of damage and static-pressure-resisting and compressive strength, repeat 2 ~ 3 times.
(4) low density oil well cementing cement briquette batching: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter is composite ceramics closed pore cenosphere 30wt%, the flyash 6wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 2wt%, sodium sulfate 1wt% and micro-silicon 1wt% of 20 ~ 30 μm.
(5) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter is composite ceramics closed pore cenosphere 30wt%, the flyash 6wt% of loss on ignition 1.1% of 20 ~ 30 μm, that purity 99.9% calcium oxide 2wt%, sodium sulfate 1wt% and micro-silicon 1wt% put into stirrer for mixing is even.
(6) get in (5) that to mix sample a little, pour in beaker, by 0.6(W/C) water cement ratio modulation grout, stir with glass stick, pour in mud scale and weigh density, recording density value g/cm
3.
(7) at temperature 28 DEG C ± 1 DEG C, with 0.6(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(8) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(9) observe record free liquid amount of precipitation of weighing, fall fluid loss, thickening time, the liquidity scale.
(10) 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 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 constant temperature 52 DEG C, soaks 1 hour after the demoulding 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 μm of zirconium diborides, particle diameter 16 ~ 20 μm of silicon carbide and particle diameter 4 ~ 6 μm of zirconium whites stir in 70wt%:22wt%:8wt% mixed powder stirrer, 2000 DEG C of heat preservation sinterings 70 minutes in a vacuum furnace, by zirconium diboride, silicon carbide and zirconia sintered body are processed into 20 μm of microballons at balling machine, 2. dosing: 20 μm of zirconium diborides, silicon carbide and zirconia composite ceramics microballon 80wt%: water 20wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 3g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, four district's electric furnaces to dewater expansion 850 DEG C, dry sintering temperature at 1600 DEG C, melt surface temperature 1800 DEG C, become bulb temperature 1500 DEG C, clean classification through wind-force and obtain 35 ~ 50 μm of composite ceramics closed pore cenospheres.
(2) 35 ~ 50 μm of composite ceramics closed pore cenosphere 50g are got, put into the beaker filling water, 1 minute is stirred with glass stick, leave standstill 5 minutes, observe the suspended state of composite ceramics closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the compound closed pore hollow ceramic microspheres 100g of 35 ~ 50 μm is got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, being poured into by the sample of drift pearl fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, and calculates percentage of damage and static-pressure-resisting and compressive strength and repeats 2 ~ 3 times.
(4) low density oil well cementing cement briquette batching: by getting G level oil well cement 45wt%, 13 μm of superfine cement 12wt%, particle diameter is composite ceramics closed pore cenosphere 33wt%, the flyash 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5wt%, sodium sulfate 0.5wt% and micro-silicon 1wt% of 35 ~ 50 μm.
(5) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 12wt%, particle diameter is composite ceramics closed pore cenosphere 33wt%, the flyash 7wt% of loss on ignition 1.1% of 35 ~ 50 μm, that purity 99.9% calcium oxide 1.5wt%, sodium sulfate 0.5wt% and micro-silicon 1wt% put into stirrer for mixing is even.
(6) get in (5) that to mix sample a little, pour in beaker, by 0.55(W/C) water cement ratio modulation grout, stir with glass stick, pour in mud scale and weigh density, recording density value g/cm
3.
(7) at temperature 28 DEG C ± 1 DEG C, with 0.55(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(8) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(9) observed and recorded free liquid amount of precipitation, fluid loss, thickening time, the liquidity scale fall.
(10) 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 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 constant temperature 52 DEG C, soaks 1 hour after the demoulding 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 (6)
1. a composite ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette, comprise the preparation of composite ceramics closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, it is characterized in that: by particle diameter 1 ~ 10 μm of zirconium diboride, particle diameter 5 ~ 20 μm of silicon carbide and particle diameter 1 ~ 10 μm of zirconium white stir by weight 55 ~ 70wt%:20 ~ 25wt%:5 ~ 25wt% mixed powder, 1800 ~ 2000 DEG C of heat preservation sinterings 60 ~ 70 minutes in a vacuum furnace, by zirconium diboride, silicon carbide and zirconia sintered body are processed into 10 ~ 20 μm of microballons at balling machine, the weight percent of zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid slurry consists of: 10 ~ 20 μm of zirconium diborides, silicon carbide and zirconia composite ceramics microballon 70 ~ 80wt%: water 20 ~ 30wt%, in zirconium diboride, silicon carbide and zirconia composite ceramics microballon liquid slurry, add whipping agent is light calcium carbonate, and the concentration of use is 1 ~ 3g/L, 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, expansion temperature that four district's electric furnaces dewater 800 ~ 850 DEG C, dry sintering temperature 1400 ~ 1600 DEG C, melt surface temperature 1700 ~ 1800 DEG C, become bulb temperature 1400 ~ 1500 DEG C, obtain 5 ~ 50 μm of zirconium diborides, silicon carbide and zirconia composite ceramics closed pore cenosphere through classification, by G level oil well cement 40 ~ 50wt%, 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the composite ceramics closed pore cenosphere 25 ~ 35wt% of 5 ~ 50 μm, flyash 5 ~ the 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2wt%, the ratio mixing of sodium sulfate 0.5 ~ 1.0wt% and SILICA FUME 1 ~ 3wt%, water cement ratio with 0.5 ~ 0.6 stirs in stirrer sizes mixing 40 seconds, get aliquot and carry out cement slurry property test, the mensuration of composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity, cement slurry density measures, withstand voltage density test, sedimentation stability, free liquid amount of precipitation, fluid loss falls, thickening time, the liquidity scale, pour one group of two block length into, wide, height is respectively in the die trial of 53mm*53mm*53mm, 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 compressive property test.
2. a kind of composite ceramics closed pore cenosphere according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: composite ceramics closed pore cenosphere its floatability is greater than 98%.
3. a kind of composite ceramics closed pore cenosphere according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: the cement briquette 8 hours ultimate compression strength of preparation is greater than 15MPa, and within 24 hours, ultimate compression strength is greater than 40MPa.
4. a kind of composite ceramics closed pore cenosphere according to claim 1 prepares 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.
5. a kind of composite ceramics closed pore cenosphere according to claim 1 prepares 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.
6. a kind of composite ceramics closed pore cenosphere according to claim 1 prepares 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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