CN103803889B - High resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette - Google Patents
High resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette Download PDFInfo
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Abstract
The invention provides the method that high resistance to compression quartz-ceramics compounded microbeads prepares oil well cementing cement briquette, comprise the preparation of high resistance to compression quartz-ceramics compound closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, it is characterized in that: by G level oil well cement 40 ~ 50wt%, 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the high resistance to compression quartz-ceramics compound 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%, sodium sulfate 0.5 ~ 1.0? wt% and micro-silicon 1 ~ 3wt% mixing and stirring, 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 DEG C, 48 hours, soak 1 hour in cold water after the demoulding, carry out performance test.
Description
Technical field
The present invention relates to the method that high resistance to compression quartz-ceramics compounded microbeads 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, flyash floating bead is canescence, and main component is SiO
2account for 70% and AL
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, but the particle diameter of drift pearl is large, 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 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, and maximum compressive strength 20MPa, so adopt composite ceramic material making cenosphere to substitute the drift pearl of flyash, 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~ 0.85g/cm
3between, (density of G level oil well cement 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 controlled.
Summary of the invention
The object of the invention is to overcome the existing drift pearl state of the art, high resistance to compression quartz-ceramics cenosphere is utilized to substitute the drift pearl of flyash, 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 closed pore hollow ceramic microspheres by Quartz ceramic material, 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 conditions, density range 0.5g/cm
3~ 0.85g/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 requirement of long shut-in well well cementing material.
its technical scheme is.
High resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, comprises the preparation of high resistance to compression quartz-ceramics compound 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 high resistance to compression quartz-ceramics compound 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%, with 0.5 ~ 0.6(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, get aliquot and pour 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 constant temperature 52 DEG C, 48 hours, soak in cold water after the demoulding and carry out cement slurry property test in 1 hour, comprise the mensuration of quartz-ceramics compound 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, carries out compressive property test.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, by particle diameter 1 ~ 60 μm of silica powder, particle diameter 5 ~ 50 μm of zirconium whites, particle diameter 5 ~ 60 μm of silicon nitrides are by weight: 70 ~ 85wt%:5 ~ 20wt%:10 ~ 30wt%, first by silica powder, after zirconia powder and silicon nitride powder mixing and stirring, 2 ~ 5wt% the binding agent adding powder mix gross weight again stirs in stirrer, be pressed into blank, 100 ~ 300 DEG C of dryings 6 ~ 12 hours, 2 ~ 4 hours are fired 1200 ~ 1650 DEG C of insulations, obtain containing zirconium white silicon nitride height resistance to compression quartz-ceramics Composite Sintering body, 10 ~ 35 μm of microballons are processed at balling machine containing zirconium white silicon nitride height resistance to compression quartz-ceramics Composite Sintering body.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and the weight percent of zirconium white silicon nitride height resistance to compression quartz-ceramics compounded microbeads liquid slurry consists of: 10 ~ 35 μm containing zirconium white silicon nitride height resistance to compression quartz-ceramics compounded microbeads 70 ~ 80wt%: water 20 ~ 30wt%.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, adding whipping agent in zirconium white silicon nitride height resistance to compression quartz-ceramics compounded microbeads liquid slurry is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, abundant agitation and filtration is starched containing zirconium white silicon nitride height resistance to compression quartz-ceramics compounded microbeads liquid, 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 containing zirconium white silicon nitride height resistance to compression quartz-ceramics compound closed pore cenosphere through classification.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, is greater than 95% containing zirconium white silicon nitride height resistance to compression quartz-ceramics compound closed pore cenosphere its floatability.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and the cement briquette 8 hours ultimate compression strength of preparation is greater than 20MPa, and within 24 hours, ultimate compression strength is greater than 30MPa.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, the density range ± 0.01g/cm of same batch of different sampling spot height resistance to compression quartz-ceramics compound closed pore cenosphere
3.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and the fluid loss that falls of cement briquette is less than 50mL/30min.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and cement briquette rate of change of the density is less than 0.02.
Described high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, quartz-ceramics compound closed pore cenosphere resistance to hydrostatic pressure intensity 120 ~ 280MPa.
The present invention has the following advantages.
1, the dependence to flyash floating bead in long-term well cementation can be changed, it is high that ceramic composite has ultimate compression strength, and fold resistance is good, high through high temperature sintering activity, size is controlled, selects meet cementing requirements containing zirconium white silicon nitride height resistance to compression quartz-ceramics matrix material.
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
,quartz-ceramics compounded microbeads density can be controlled in 0.5g/cm
3~ 0.85g/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, G level oil well cement, superfine cement, ceramic fine bead have greater activity through more than 1000 DEG C high temperature sinterings, and hydration reaction is fast, jelly can be formed, can improve early strength, ceramic fine bead performance is better than fly ash float, at military project space industry widespread use.
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, quartz-ceramics microballon particle diameter is little, and strong with the avidity of cement, grout stability is strong.
6, adopt purity 99.9% calcium oxide, react with water and generate calcium hydroxide, release amount of heat, improve cement briquette early strength.
Embodiment.
Embodiment 1.
(1) 1. the preparation of high resistance to compression quartz-ceramics compound closed pore cenosphere is prepared burden and is fired: by particle diameter 1 ~ 20 μm of silica powder, particle diameter 5 ~ 20 μm of zirconia powders, particle diameter 5 ~ 25 μm of silicon nitride powders are by weight: after 70wt%:10wt%:20wt% mixing and stirring, add powder mix gross weight 3wt% binding agent again to stir in stirrer, be pressed into blank, 100 DEG C of dryings 12 hours, fire 1650 DEG C of insulations and within 3 hours, obtain high resistance to compression quartz-ceramics composite sintered material, 10 ~ 15 μm of microballons will be processed at balling machine containing zirconium white silicon nitride height resistance to compression quartz-ceramics Composite Sintering body, 2. dosing: 10 ~ 15 μm containing zirconium white silicon nitride height resistance to compression quartz-ceramics compounded microbeads 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, vertical four district's electric furnaces dewater expansion temperature 800 DEG C, dry sintering temperature 1400 DEG C, melt surface 1700 DEG C, become bulb temperature 1400 DEG C, clean classification through wind-force and obtain 5 ~ 15 μm high resistance to compression quartz-ceramics compound closed pore cenospheres.
(2) 5 ~ 15 μm high resistance to compression quartz-ceramics compound 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 high resistance to compression quartz-ceramics compound 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 high resistance to compression quartz-ceramics compound 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, being poured into by the sample of high resistance to compression quartz-ceramics compounded microbeads fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate percentage of damage and record static-pressure-resisting value and compressive strength.
(4) 5 ~ 15 μm high resistance to compression quartz-ceramics compound closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain high resistance to compression quartz-ceramics compound closed pore cenosphere and take 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 particle diameter distributes.
(5) low density oil well cementing cement briquette batching: be the high resistance to compression quartz-ceramics compound 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.
(6) mix: get G level oil well cement 40wt%, 13 μm of superfine cement 15wt%, particle diameter is high resistance to compression quartz-ceramics compound 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.
(7) get in (6) 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.
(8) 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 stability and homogeneity.
(9) 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, high 53mm.
(10) observe weigh and record free liquid amount of precipitation, fall fluid loss, the thickening time, the liquidity scale.
(11) mensuration of cement briquette rate of change of the density, measure 24 and 48 hours cement briquette density, cement briquette is put into pressing machine pressurization (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa, 120MPa, 150MPa, 180MPa, 200MPa, 250MPa, 280MPa), measure the cement briquette density after pressurization, rate of change of the density equals: (after pressurization, density deducts 24 and 48 hours cement briquette density)/24 and 48 hours cement briquette density, if rate of change of the density is greater than 0.02, illustrate that Ceramic Composite microballon inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density.
(12) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by the regulation of GB GB/T177.
(13) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by the regulation of GB GB/T177.
Embodiment 2.
(1) 1. the preparation of high resistance to compression quartz-ceramics compound closed pore cenosphere is prepared burden and is fired: by particle diameter 25 ~ 40 μm of silica powders, particle diameter 25 ~ 35 μm of zirconia powders, particle diameter 30 ~ 45 μm of silicon nitride powders are by weight: after 75wt%:15wt%:10wt% mixing and stirring, add powder mix gross weight 4wt% binding agent again to stir in stirrer, be pressed into blank, 200 DEG C of dryings 11 hours, fire 1600 DEG C of insulations and within 3.5 hours, obtain containing high resistance to compression quartz-ceramics composite sintered material, 20 ~ 25 μm of microballons will be processed at balling machine containing zirconium white silicon nitride height resistance to compression quartz-ceramics Composite Sintering body, 2. dosing: 20 ~ 25 μm high resistance to compression quartz-ceramics compounded microbeads 75wt%: water 25wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 1.5g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, on four district's electric furnaces through dehydration expansion temperature 820 DEG C, dry sintering temperature 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 high resistance to compression quartz-ceramics compound closed pore cenospheres.
(2) 20 ~ 30 μm high resistance to compression quartz-ceramics compound 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 high resistance to compression quartz-ceramics compound closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the high resistance to compression quartz-ceramics compound 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, and calculates percentage of damage and records static-pressure-resisting value and compressive strength.
(4) 20 ~ 30 μm of Ceramic Composite closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain high resistance to compression Ceramic Composite closed pore cenosphere and take 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 particle diameter distributes.
(5) low density oil well cementing cement briquette batching: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter is high resistance to compression quartz-ceramics compound 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.
(6) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter is high resistance to compression quartz-ceramics compound 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.
(7) get in (6) 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.
(8) 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 stability and homogeneity.
(9) 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, high 53mm.
(10) observed and recorded free liquid amount of precipitation, fluid loss, thickening time, the liquidity scale fall.
(11) mensuration of cement briquette rate of change of the density, measure 24 and 48 hours cement briquette density, cement briquette is put into pressing machine pressurization (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa, 120MPa, 150MPa, 180MPa, 200MPa, 250MPa, 280MPa), measure the cement briquette density after pressurization, rate of change of the density equals: (after pressurization, density deducts 24 and 48 hours cement briquette density)/24 and 48 hours cement briquette density, if rate of change of the density is greater than 0.02, illustrate that Ceramic Composite microballon inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density.
(12) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by the regulation of GB GB/T177.
(13) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by the regulation of GB GB/T177.
Embodiment 3.
(1) 1. the preparation of high resistance to compression quartz-ceramics compound closed pore cenosphere is prepared burden and is fired: by particle diameter 45 ~ 60 μm of silica powders, particle diameter 40 ~ 50 μm of zirconia powders, particle diameter 50 ~ 60 μm of silicon nitrides are by weight: after 80wt%:5wt%:15wt% mixing and stirring, add powder mix gross weight 5wt% binding agent again to stir in stirrer, be pressed into blank, 300 DEG C of dryings 10 hours, fire 1550 DEG C of insulations and within 4 hours, obtain containing high resistance to compression quartz-ceramics composite sintered material, quartz-ceramics compound closed pore cenosphere material sintered compact is processed into 30 ~ 35 μm of microballons at balling machine, 2. dosing: 30 ~ 35 μm high resistance to compression quartz-ceramics compounded microbeads 80wt%: water 20wt%, 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, four district's electric furnaces dewater expansion 850 DEG C, dry sintering temperature 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 quartz-ceramics compound closed pore cenospheres.
(2) 35 ~ 50 μm of quartz-ceramics compound 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 quartz-ceramics compound closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the high resistance to compression quartz-ceramics compound closed pore cenosphere 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.
(4) 35 ~ 50 μm of quartz-ceramics compound closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain quartz-ceramics compound closed pore cenosphere and claim 50g to pour beaker into add 100g water, stir with glass stick, pour in laser particle size analyzer test trough, observed and recorded sample particle diameter distributes.
(5) 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 quartz-ceramics compound 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.
(6) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 12wt%, particle diameter is closed pore hollow quartz-ceramics compound 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.
(7) get in (6) 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.
(8) 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 stability and homogeneity.
(9) 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, high 53mm.
(10) observed and recorded free liquid amount of precipitation, fluid loss, thickening time, the liquidity scale fall.
(11) mensuration of cement briquette rate of change of the density, measure 24 and 48 hours cement briquette density, cement briquette is put into pressing machine pressurization (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa, 120MPa, 150MPa, 180MPa, 200MPa, 250MPa, 280MPa), measure the cement briquette density after pressurization, rate of change of the density equals: (after pressurization, density deducts 24 and 48 hours cement briquette density)/24 and 48 hours cement briquette density, if rate of change of the density is greater than 0.02, illustrate that Ceramic Composite microballon inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density.
(12) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by the regulation of GB GB/T177.
(13) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by the regulation of GB GB/T177.
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%, 13 μm of superfine cement Shengli Oil Field special cement factories.
Claims (7)
1. high resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette, comprise the preparation of high resistance to compression quartz-ceramics compound closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, it is characterized in that: by particle diameter 1 ~ 60 μm of silica powder, particle diameter 5 ~ 50 μm of zirconium whites, particle diameter 5 ~ 60 μm of silicon nitrides are by weight 70 ~ 85wt%:5 ~ 20wt%:10 ~ 30wt%, wherein particle diameter 1 ~ 60 μm of silica powder, the weight percent sum of particle diameter 5 ~ 50 μm of zirconium whites and particle diameter 5 ~ 60 μm of each components of silicon nitride is 100%, first by silica powder, after zirconia powder and silicon nitride powder mixing and stirring, 2 ~ 5wt% the binding agent adding powder mix gross weight again stirs in stirrer, be pressed into blank, 100 ~ 300 DEG C of dryings 6 ~ 12 hours, 2 ~ 4 hours are fired 1200 ~ 1650 DEG C of insulations, obtain containing zirconium white silicon nitride height resistance to compression quartz-ceramics Composite Sintering body, 10 ~ 35 μm of microballons are processed at balling machine containing zirconium white silicon nitride height resistance to compression quartz-ceramics Composite Sintering body, the weight percent of high resistance to compression quartz-ceramics compounded microbeads liquid slurry consists of: 10 ~ 35 μm containing zirconium white silicon nitride height resistance to compression quartz-ceramics compounded microbeads 70 ~ 80wt%: water 20 ~ 30wt%, adding whipping agent in high resistance to compression quartz-ceramics compounded microbeads liquid slurry is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L, abundant agitation and filtration is starched containing zirconium white silicon nitride height resistance to compression quartz-ceramics compounded microbeads liquid, 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 containing zirconium white silicon nitride height resistance to compression quartz-ceramics compound closed pore cenosphere through classification, by G level oil well cement 40 ~ 50wt%, 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the high resistance to compression quartz-ceramics compound 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 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 in cold water after the demoulding and carry out cement slurry property test in 1 hour, comprise the mensuration of quartz-ceramics compound 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, carry out compressive property test.
2. high resistance to compression quartz-ceramics compounded microbeads 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 20MPa, and within 24 hours, ultimate compression strength is greater than 30MPa.
3. high resistance to compression quartz-ceramics compounded microbeads according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: the density range ± 0.01g/cm of the high resistance to compression quartz-ceramics compound closed pore cenosphere of same batch of different sampling spot
3.
4. high resistance to compression quartz-ceramics compounded microbeads 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. high resistance to compression quartz-ceramics compounded microbeads according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: be greater than 95% containing zirconium white silicon nitride height resistance to compression quartz-ceramics compound closed pore cenosphere its floatability.
6. high resistance to compression quartz-ceramics compounded microbeads 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.
7. high resistance to compression quartz-ceramics compounded microbeads according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: quartz-ceramics compound closed pore cenosphere resistance to hydrostatic pressure intensity 120 ~ 280MPa.
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| CN1453239A (en) * | 2003-05-29 | 2003-11-05 | 上海交通大学 | Large grain spherical sub-micron/nano composite fiber-ceramic powder |
| CN101591191A (en) * | 2008-11-21 | 2009-12-02 | 中材高新材料股份有限公司 | Zirconia reinforced silicon nitride/quartz-matrix ceramic composite material and preparation method thereof |
| CN103601430A (en) * | 2013-11-20 | 2014-02-26 | 山东理工大学 | Method of preparing low-density well cementation cement check block of oil well by utilizing silicon carbide ceramic microbeads |
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| CN1453239A (en) * | 2003-05-29 | 2003-11-05 | 上海交通大学 | Large grain spherical sub-micron/nano composite fiber-ceramic powder |
| CN101591191A (en) * | 2008-11-21 | 2009-12-02 | 中材高新材料股份有限公司 | Zirconia reinforced silicon nitride/quartz-matrix ceramic composite material and preparation method thereof |
| CN103601430A (en) * | 2013-11-20 | 2014-02-26 | 山东理工大学 | Method of preparing low-density well cementation cement check block of oil well by utilizing silicon carbide ceramic microbeads |
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