CN103922656B - Method for preparing oil well cementing cement briquettes with samarium oxide silicon nitride ceramic composite microbeads - Google Patents
Method for preparing oil well cementing cement briquettes with samarium oxide silicon nitride ceramic composite microbeads Download PDFInfo
- Publication number
- CN103922656B CN103922656B CN201410142230.1A CN201410142230A CN103922656B CN 103922656 B CN103922656 B CN 103922656B CN 201410142230 A CN201410142230 A CN 201410142230A CN 103922656 B CN103922656 B CN 103922656B
- Authority
- CN
- China
- Prior art keywords
- silicon nitride
- nitride ceramics
- samarium trioxide
- cement
- oil well
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Processing Of Solid Wastes (AREA)
- Ceramic Products (AREA)
Abstract
The invention provides a method for preparing oil well cementing cement briquettes with samarium oxide silicon nitride ceramic composite microbeads. The method comprises the steps of preparing samarium oxide silicon nitride ceramic closed cell hollow microbeads, dosing, mixing, stirring and mixing paste, providing test molds and performing strength tests, and is characterized by mixing and stirring 40-50wt% of G-grade oil well cement, 10-15wt% of superfine cement with grain size of 13mu m, 25-35wt% of samarium oxide silicon nitride ceramic closed cell hollow microbeads with grain sizes of 5-35mu m, 5-7wt% of fly ash with ignition loss of 1.1%, 1.5-2wt% of calcium oxide with purity of 99.9%, 0.5-1.0wt% of sodium sulfate and 1-3wt% of micro-silicon uniformly, stirring and mixing paste in a stirrer for 40 seconds in a water cement ratio of 0.5-0.6 (W/C), pouring the paste into test molds, curing the paste in a water bath curing box at a constant temperature of 52 DEG C for 24 hours and 48 hours, soaking the product in cold water for one hour after demolding, and carrying out performance tests.
Description
Technical field
The present invention relates to the method that Samarium trioxide silicon nitride 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
3, between, 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, drift pearl after removing carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, surfaces externally and internally is smooth, volume is large, a kind of rounded, light weight, closed pore is hollow, wear-resisting, high temperature resistant, thermal conductivity is little, intensity is high, drift pearl amount accounts for 0.5 ~ 1.0% of flyash total amount, 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 nitrogen that burning and scission reaction produce, the gas such as hydrogen and carbonic acid gas, 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, to swim in the water surface pulls out and dry, be drift pearl, drift pearl in flyash is canescence, main component is SiO
2account for 70% and AI
2o
3account for 13%, 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 is per ton rises violently 10,000 yuan, and maximum compressive strength 20MPa, fly ash float is suitable only for the low temperature oil-well of less than 2000 meters, so adopt ceramic composite 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~ 0.8g/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 1 g/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.
In patent 200910071314.X, adopt the flyash of non-drift pearl as light-weight additive, in literary composition, the pellet density of flyash is 2.0g/cm
3, cement density 3.1g/cm
3, silica flour density 2.0g/cm
3, only have the density of water to be 1.0g/cm
3, the proportional restriction of consumption of water, can not make density at 1.40 ~ 1.55g/cm
3low-density cement mortar.
Some oil field adopts the non-drift such as kaolin, diatomite pearl as light-weight additive, but tap density is greater than 2.0g/cm
3, wanting preparation density is 1.0 ~ 1.6g/cm
3between grout be impossible.
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, exploitation is progressively by landwards deep layer and the bathypelagic exploitation of land low temperature oil-well, and traditional well cementing material drift pearl can not meet the needs of deep layer high-temperature oil well.
Summary of the invention
The object of the invention is to overcome the existing drift pearl state of the art, oxidation shirt is utilized to substitute the drift pearl of flyash as additive SINTERING PRODUCTION high-performance silicon nitride ceramics microballon, oxidation shirt is utilized to generate the silicon nitride ceramics solid microbeads of modification as sintering aid generation chemical reaction, high pressure spraying high speed centrifugation rotary spraying technique is adopted at vertical four district's electric furnaces, expand through dehydration, dry, melt surface, balling-up finally forms silicon nitride ceramics closed pore cenosphere, silicon nitride ceramics closed pore cenosphere has higher toughness, high resistance to compression, anti-folding, good mechanical property, meet the requirement of high-temperature oil well well cementation lightening material, silicon nitride ceramics closed pore cenosphere density can be controlled in 0.5g/cm
3~ 0.8g/cm
3, ultimate compression strength is greater than 600MPa, and then preparation 1.0g/cm
3~ 1.5g/cm
3the test block of oil well cementing light weight cement, meets the requirement of long shut-in well well cementing material.
its technical scheme is.
Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, comprises the preparation of Samarium trioxide silicon nitride ceramics compound 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 Samarium trioxide silicon nitride ceramics compound closed pore cenosphere 25 ~ 35wt% of 5 ~ 35 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 Samarium trioxide silicon nitride 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, mobility, carries out compressive property test.
Described Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, by particle diameter 1 ~ 50 μm of silicon nitride powder, particle diameter 1 ~ 45 μm of Samarium trioxide powder by 80 ~ 90wt%:10 ~ 20wt%, by silicon nitride powder, Samarium trioxide proportional sampling mixing and stirring, blank is made at 60 ~ 80MPa pressing machine, 12 ~ 18 hours are fired at 1400 ~ 1650 DEG C of vacuum atmosphere ovens, obtain the sintered compact of Samarium trioxide silicon nitride ceramics matrix material, the sintered compact of Samarium trioxide silicon nitride ceramics matrix material is processed into 10 ~ 35 μm of microballons at balling machine.
Described Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and the weight percent of Samarium trioxide silicon nitride ceramics microballon liquid slurry consists of: 10 ~ 35 μm of Samarium trioxide silicon nitride ceramics compounded microbeads 70 ~ 80wt%: water 20 ~ 30wt%.
Described Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and adding whipping agent in silicon nitride ceramics microballon liquid slurry is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L.
Described Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, Samarium trioxide silicon nitride ceramics compounded microbeads liquid starches abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballon, on the four vertical electric furnaces in district, dehydration expansion temperature 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 ~ 35 μm of Samarium trioxide silicon nitride ceramics compound closed pore cenospheres through classification.
Described Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and Samarium trioxide silicon nitride ceramics compound closed pore cenosphere its floatability is greater than 98%.
Described Samarium trioxide silicon nitride 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 40MPa.
Described Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and the variable density scope of the sampling spot nitriding and oxidizing samarium silicon pottery closed pore cenosphere of same batch of different positions is at ± 0.01 g/cm
3.
Described Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, and the rate of change of the density after cement briquette pressurization is less than 0.02.
Described Samarium trioxide silicon nitride 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.
the present invention has the following advantages.
1, the dependence to flyash floating bead in long-term well cementation can be changed, utilize Samarium trioxide as additive sintered silicon nitride, form the silicon nitride ceramics compounded microbeads of modification, there is the advantages such as ultimate compression strength is high, fold resistance good, high temperature resistant, high through high temperature sintering activity, size is controlled, and ceramic composite can meet the cementing requirements of 6000 ~ ten thousand metres high-temperature oil well.
2, ceramic composite is as oil well cementing light-weight additive, can require proportioning, the sintering temperature technical parameter of determining stupalith, according to ceramic fine bead Particle size requirements, determine rotating spraying shower nozzle aperture according to cementing technology.
3
,this technique is advanced, and technology maturation, product performance are stable, and production cost is low, and output is high, and performance is good, and the density of silicon nitride ceramics microballon can be controlled in 0.5g/cm
3~ 0.8g/cm
3add the early strength that particle diameter 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, 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, within 8 hours, ultimate compression strength is more than 20 MPa.
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, and enter body of heater after liquid is fully atomized, drop is at breathing space expanded by heating, expanding volume is relevant with expansion temperature and density of foaming agent, again through sintering, melting, finally formation closed pore cenosphere, preventing from tying wall to improve output, adopting thermal cycling suction, wind-force blowing system, accelerate material in circulation, enhance productivity.
5, adopt purity 99.9% calcium oxide, react with water and generate calcium hydroxide, release amount of heat, improve cement briquette early strength, grout good stability.
6, adopt high pressure spraying high speed centrifugation rotary spraying technique, the rotating speed 24000r/min of motor, adopts the electric furnace that vertical 4th district control respectively.
embodiment.
Embodiment 1.
(1) 1. the preparation of Samarium trioxide silicon nitride ceramics compound closed pore cenosphere is prepared burden and is fired: by particle diameter 1 ~ 15 μm of silicon nitride powder, particle diameter 1 ~ 10 μm of Samarium trioxide powder presses 85wt%:15wt% mixing and stirring, add dehydrated alcohol dispersion agent, blank is made at 70MPa pressing machine, 18 hours are fired at 1400 DEG C of vacuum atmosphere ovens, obtain the sintered compact of Samarium trioxide silicon nitride ceramic material, the sintered compact of Samarium trioxide silicon nitride ceramic material is processed into 10 ~ 15 μm of microballons at balling machine, 2. dosing: get 10 ~ 15 μm silicon nitride ceramics microballon ratio 76wt%: water 24wt%, 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, on vertical four district's electric furnaces, dehydration expansion temperature 810 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 containing Samarium trioxide silicon nitride ceramics compound closed pore cenosphere.
(2) 5 ~ 15 μm are got containing Samarium trioxide silicon nitride ceramics closed pore cenosphere 50g, put into the beaker filling water, 1 minute is stirred with glass stick, leave standstill 5 minutes, observe the suspended state of Samarium trioxide silicon nitride 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) 5 ~ 15 μm of Samarium trioxide silicon nitride ceramics closed pore cenosphere 100g are 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 ceramic fine bead 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) 5 ~ 15 μm of Samarium trioxide silicon nitride ceramics compound closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain Samarium trioxide silicon nitride 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, and particle diameter is greater than 95% at 5 ~ 15 μm.
(5) low density oil well cementing cement briquette batching: Samarium trioxide silicon nitride ceramics compound closed pore cenosphere 35wt%, the flyash 5wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5wt%, the sodium sulfate 0.5wt% and SILICA FUME 3wt% that by G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 10wt%, particle diameter are 5 ~ 15 μm.
(6) mix: get G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 10wt%, particle diameter is 5 ~ 15 μm of silicon nitride ceramics closed pore cenosphere 35wt%, flyash 5wt%, the purity 99.9% calcium oxide 1.5wt% of loss on ignition 1.1%, that sodium sulfate 0.5wt% and SILICA FUME 3wt% puts 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 height 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 (20 MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100 MPa, 150 MPa, 200 MPa) measure the cement briquette density after pressurizeing respectively, 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 silicon nitride ceramics closed pore cenosphere inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density, the density of cement briquette equals the quality of cement briquette and the ratio of volume.
(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 being defined on pressing machine of GB GB/T 177.
(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 being defined on pressing machine of GB GB/T 177.
Embodiment 2.
(1) 1. the preparation of Samarium trioxide silicon nitride ceramics compound closed pore cenosphere is prepared burden and is fired: by particle diameter 20 ~ 35 μm of silicon nitride powders, particle diameter 15 ~ 25 μm of Samarium trioxide powder press 90wt%:10wt% mixing and stirring, add dehydrated alcohol dispersion agent, blank is made at 75MPa pressing machine, 16 hours are fired at 1500 DEG C of vacuum atmosphere ovens, obtain the sintered compact of Samarium trioxide silicon nitride ceramic material, the sintered compact of Samarium trioxide silicon nitride ceramic material is processed into 20 ~ 25 μm of microballons at balling machine, 2. dosing: 20 ~ 25 μm silicon nitride ceramics microballon ratio 78wt%: water 22wt%, 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, expansion temperature that four district's electric furnaces dewater 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 ~ 25 μm of Samarium trioxide silicon nitride ceramics compound closed pore cenospheres.
(2) particle diameter 20 ~ 25 μm of Samarium trioxide silicon nitride 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 silicon nitride ceramics closed pore cenosphere pearl in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the Samarium trioxide silicon nitride ceramics compound closed pore cenosphere 100g of 20 ~ 25 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 ~ 25 μm of Samarium trioxide silicon nitride ceramics closed pore cenosphere size distribution are analyzed with laser particle size analyzer: wind-force is cleaned classification and obtain Samarium trioxide silicon nitride ceramics 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, and particle diameter is greater than 95% at 20 ~ 25 μm.
(5) low density oil well cementing cement briquette batching: get G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 15 wt%, particle diameter is 20 ~ 25 μm of Samarium trioxide silicon nitride ceramics closed pore cenosphere 30wt%, flyash 6 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 2wt%, sodium sulfate 1wt% and SILICA FUME 1wt%.
(6) mix: get G level oil well cement 45 wt%, particle diameter 13 μm of superfine cement 15wt%, particle diameter is 20 ~ 25 μm of Samarium trioxide silicon nitride ceramics closed pore cenosphere 30wt%, flyash 6wt%, the purity 99.9% calcium oxide 2wt% of loss on ignition 1.1%, that sodium sulfate 1wt% and SILICA FUME 1wt% puts 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 height 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 (20 MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100 MPa, 150 MPa, 200 MPa), 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, the density of cement briquette equals the quality of cement briquette and the ratio of volume.
(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 being defined on pressing machine of GB GB/T 177.
(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 being defined on pressing machine of GB GB/T 177.
Embodiment 3.
(1) 1. the preparation of Samarium trioxide silicon nitride ceramics compound closed pore cenosphere is prepared burden and is fired: by particle diameter 40 ~ 50 μm of silicon nitride powders, after particle diameter 30 ~ 40 μm of Samarium trioxide powder press 88wt%:12wt% mixing and stirring, add dehydrated alcohol dispersion agent, blank is made at 80MPa pressing machine, 14 hours are fired at 1600 DEG C of vacuum atmosphere ovens, obtain the sintered compact of Samarium trioxide silicon nitride ceramic material, the sintered compact of Samarium trioxide silicon nitride ceramic material is processed into 30 ~ 35 μm of microballons at balling machine, 2. dosing: 30 ~ 35 μm of Samarium trioxide silicon nitride ceramics microballons ratio 80wt%: water 20wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 1.0g/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 30 ~ 35 μm of Samarium trioxide silicon nitride ceramics closed pore cenospheres.
(2) 30 ~ 35 μm of Samarium trioxide silicon nitride 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 Samarium trioxide silicon nitride ceramics closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) 30 ~ 35 μm of Samarium trioxide silicon nitride ceramics closed pore cenosphere 100g are 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) 30 ~ 35 μm of Samarium trioxide silicon nitride ceramics closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain Samarium trioxide silicon nitride ceramics 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, and particle diameter is greater than 95% at 30 ~ 35 μm.
(5) low density oil well cementing cement briquette batching: by getting G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 12 wt%, particle diameter is Samarium trioxide silicon nitride ceramics closed pore cenosphere 33wt%, flyash 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5wt%, the sodium sulfate 0.5wt% and SILICA FUME 1wt% of 30 ~ 35 μm.
(6) mix: get G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 12wt%, particle diameter is 35 ~ 35 μm of Samarium trioxide silicon nitride ceramics closed pore cenosphere 33wt%, flyash 7wt%, the purity 99.9% calcium oxide 1.5wt% of loss on ignition 1.1%, that sodium sulfate 0.5wt% and SILICA FUME 1wt% puts into stirrer for mixing is even.
(7) get in (6) that to mix sample a little, pour in beaker, by 0.5(W/C) the water cement ratio modulation grout of 5, 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 height 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 (20 MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100 MPa, 150 MPa, 200 MPa), 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 silicon nitride ceramics closed pore cenosphere inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density, the density of cement briquette equals the quality of cement briquette and the ratio of volume.
(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 being defined on pressing machine of GB GB/T 177.
(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 being defined on pressing machine 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%, 13 μm of superfine cement Shengli Oil Field special cement factories produce.
Claims (6)
1. Samarium trioxide silicon nitride ceramics compounded microbeads prepares the method for oil well cementing cement briquette, comprise the preparation of Samarium trioxide silicon nitride ceramics compound closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, it is characterized in that: by particle diameter 1 ~ 50 μm of silicon nitride powder, particle diameter 1 ~ 45 μm of Samarium trioxide powder is by 80 ~ 90wt%:10 ~ 20wt%, by silicon nitride powder, Samarium trioxide proportional sampling mixing and stirring, blank is made at 60 ~ 80MPa pressing machine, 12 ~ 18 hours are fired at 1400 ~ 1650 DEG C of vacuum atmosphere ovens, obtain the sintered compact of Samarium trioxide silicon nitride ceramics matrix material, the sintered compact of Samarium trioxide silicon nitride ceramics matrix material is processed into 10 ~ 35 μm of microballons at balling machine, the weight percent of Samarium trioxide silicon nitride ceramics microballon liquid slurry consists of: 10 ~ 35 μm of Samarium trioxide silicon nitride ceramics compounded microbeads 70 ~ 80wt%: water 20 ~ 30wt%, adding whipping agent in silicon nitride ceramics microballon liquid slurry is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L, Samarium trioxide silicon nitride ceramics compounded microbeads liquid starches abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballon, on the four vertical electric furnaces in district, dehydration expansion temperature 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 ~ 35 μm of Samarium trioxide silicon nitride ceramics closed pore cenospheres through classification, by G level oil well cement 40 ~ 50wt%, particle diameter 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the Samarium trioxide silicon nitride ceramics compound closed pore cenosphere 25 ~ 35wt% of 5 ~ 35 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, in high 53mm*53mm*53mm die trial respectively, 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 Samarium trioxide silicon nitride 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, mobility, carry out compressive property test.
2. Samarium trioxide silicon nitride ceramics compounded microbeads according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: Samarium trioxide silicon nitride ceramics compound closed pore cenosphere its floatability is greater than 98%.
3. Samarium trioxide silicon nitride 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 40MPa.
4. Samarium trioxide silicon nitride ceramics compounded microbeads according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: the variable density scope of the sampling spot Samarium trioxide silicon nitride ceramics closed pore cenosphere of same batch of different positions is at ± 0.01 g/cm
3.
5. Samarium trioxide silicon nitride ceramics compounded microbeads according to claim 1 prepares the method for oil well cementing cement briquette, it is characterized in that: the rate of change of the density after cement briquette pressurization is less than 0.02.
6. Samarium trioxide silicon nitride 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410142230.1A CN103922656B (en) | 2014-04-10 | 2014-04-10 | Method for preparing oil well cementing cement briquettes with samarium oxide silicon nitride ceramic composite microbeads |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410142230.1A CN103922656B (en) | 2014-04-10 | 2014-04-10 | Method for preparing oil well cementing cement briquettes with samarium oxide silicon nitride ceramic composite microbeads |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103922656A CN103922656A (en) | 2014-07-16 |
| CN103922656B true CN103922656B (en) | 2015-06-10 |
Family
ID=51141087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410142230.1A Expired - Fee Related CN103922656B (en) | 2014-04-10 | 2014-04-10 | Method for preparing oil well cementing cement briquettes with samarium oxide silicon nitride ceramic composite microbeads |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103922656B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078521B (en) * | 2019-05-13 | 2021-06-11 | 西北工业大学 | Submicron silicon nitride hollow microsphere and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557657A (en) * | 2010-12-29 | 2012-07-11 | 苏州中锆新材料科技有限公司 | Method for producing high-hardness samarium oxide compounded silicon nitride ceramic |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2842903B1 (en) * | 2002-07-23 | 2004-11-19 | Schlumberger Services Petrol | PROPELLER DEVICE FOR ACQUIRING DATA IN A FLOW |
-
2014
- 2014-04-10 CN CN201410142230.1A patent/CN103922656B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557657A (en) * | 2010-12-29 | 2012-07-11 | 苏州中锆新材料科技有限公司 | Method for producing high-hardness samarium oxide compounded silicon nitride ceramic |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103922656A (en) | 2014-07-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103601430B (en) | Method of preparing low-density well cementation cement check block of oil well by utilizing silicon carbide ceramic microbeads | |
| CN103880359B (en) | Silica alumina composite ceramics microballon prepares oil well cementing cement briquette method | |
| CN103467023B (en) | Method for preparing low density oil well cementing cement test blocks by using pitchstone | |
| CN103803888B (en) | A kind of silicon oxynitride Ceramic Composite microballon prepares the method for oil well cementing cement briquette | |
| CN103880360B (en) | A kind of quartz-ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette | |
| CN103467018B (en) | Preparation method for preparing low-density oil well cementing cement briquettes by vermiculites | |
| CN103467016B (en) | Preparation method for preparing low-density oil well cement test block from composite ceramic microbeads | |
| CN103803883B (en) | Method for preparing oil well cementing cement briquette with silicon carbide/boron carbide hollow ceramic microbeads | |
| CN103880362B (en) | Method for preparing low-density cement briquette for oil well cementation by use of silicon nitride ceramic microbeads | |
| CN104531111A (en) | Method for manufacturing high temperature and high pressure resisting oil well cementing test block through silicon kaolin ceramic microbeads | |
| CN103435307B (en) | Method for preparing low-density oil well cement briquettes by using hafnium carbide microbeads | |
| CN103467017B (en) | Method for preparing low-density oil well cementing cement briquette by using glass microsphere | |
| CN103803892B (en) | Method for preparing low-density oil well cementing cement block employing zirconia ceramic composite microspheres | |
| CN103803890B (en) | Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette | |
| CN103408264B (en) | Method for preparing low-density cement testing block for oil well cementation by using tantalum carbide microbeads | |
| CN103833286B (en) | Zirconium diboride ceramics microballon prepares the method for low density oil well cementing cement briquette | |
| CN103408263B (en) | Preparation method for preparing low-density bond cement check block for oil well by microcrystal glass beads | |
| CN103803889B (en) | High resistance to compression quartz-ceramics compounded microbeads prepares the method for oil well cementing cement briquette | |
| CN103922656B (en) | Method for preparing oil well cementing cement briquettes with samarium oxide silicon nitride ceramic composite microbeads | |
| CN103880358B (en) | A kind of composite ceramics closed pore cenosphere prepares the method for oil well cementing cement briquette | |
| CN103803891B (en) | Boron nitride titanium carbonitride Ceramic Composite microballon prepares oil well cementing cement briquette method | |
| CN103467019B (en) | Method for preparing low-density oil well cementing cement briquettes by using vanadium carbide microspheres | |
| CN103833287B (en) | Titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette | |
| CN103819150B (en) | Preparation method for oil well cementing cement briquette by adopting tungsten carbide silicon dioxide composite ceramics micro-beads | |
| CN104326763B (en) | Niobium (Nb) boride ceramic fine bead prepares the method for high temperature high voltage resistant oil well cementing test block |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Yang Xueyong Inventor before: Guo Zhidong |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170406 Address after: 465200 Gushi County, Xinyang City, the town of the village of the town of the village of the village of the village of the six miles of the group of Patentee after: Yang Xueyong Address before: 255086 Zibo high tech Industrial Development Zone, Shandong high Chong Park, block D, room 1012 Patentee before: Shandong University of Technology |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150610 Termination date: 20170410 |