CN103833287B - Titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette - Google Patents
Titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette Download PDFInfo
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- CN103833287B CN103833287B CN201410088375.8A CN201410088375A CN103833287B CN 103833287 B CN103833287 B CN 103833287B CN 201410088375 A CN201410088375 A CN 201410088375A CN 103833287 B CN103833287 B CN 103833287B
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Abstract
The invention provides the method that titanium diboride ceramic microballon prepares the cement briquette of low density oil well cementing, comprise the preparation of titanium diboride ceramic 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 titanium diboride ceramic 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 ~ 1.0wt% 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 ° of C, 48? hour, soak 1 hour in cold water after the demoulding, carry out performance test.
Description
Technical field
The present invention relates to the method that titanium diboride ceramic microballon prepares the cement briquette of low density oil well cementing, 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% 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%, 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~ 0.8g/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).
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 ~ 1.5g/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.
In view of the present situation of domestic well cementing material, adopt titanium diboride ceramic material, prepare ceramic hollow closed pore microballon, utilize TiB2 powder and titanium hydride reaction to generate titanium diboride ceramic material, density can be controlled in 0.5g/cm
3~ 0.8g/cm
3between, can meet the requirement of preparation low-density cement mortar, cement slurry density is at 1.0g/cm
3~ 1.5g/cm
3between, the pressure alleviating deep-seated oil bottom prevents blind hole.
Summary of the invention
The object of the invention is to overcome the existing drift pearl state of the art, titanium diboride ceramic microballon is utilized to substitute the drift pearl of flyash, there is provided a kind of cost low, excellent property, high temperature resistant, high strength, high rigidity, anti-oxidant, corrosion-resistant, the rate of change of the density of cement briquette is made to be less than 0.02, meet the requirement of light-weight cement slurry, closed pore cenosphere prepared by the stupalith adopted, through high temperature sintering, the performance index such as resistance to compression, folding strength exceed the drift pearl of flyash, and ceramic closed pore cenosphere density range is at 0.5g/cm
3~ 0.8g/cm
3controlled, 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.
Comprise the preparation of titanium diboride ceramic 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 titanium diboride ceramic 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), 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 Ceramic Composite 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 titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, by particle diameter 1 ~ 50 μm of TiB2 powder and particle diameter 5 ~ 45 μm of titanium hydride sintering aids 95 ~ 97wt%:3 ~ 5wt% by weight, first by TiB2 powder and titanium hydride sintering aid mixing and stirring, be pressed into blank drying, 2 ~ 3 hours are fired at 1700 ~ 1900 DEG C of vacuum atmosphere ovens, obtain the sintered compact of titanium diboride ceramic material, the sintered compact of titanium diboride ceramic material is processed into 10 ~ 35 μm of microballons at balling machine.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, and the weight percent of titanium diboride ceramic microballon liquid slurry consists of: 10 ~ 35 μm titanium diboride ceramic microballon 70 ~ 80wt%: water 20 ~ 30wt%.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, and adding whipping agent in titanium diboride ceramic microballon liquid slurry is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, titanium diboride ceramic microballon liquid starches abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballon, 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, clean classification through wind-force and obtain 5 ~ 50 μm of titanium diboride ceramic closed pore cenospheres.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, and titanium diboride ceramic closed pore cenosphere its floatability is greater than 95%.
Described titanium diboride ceramic microballon prepares the method for low density 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 20MPa.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, and the variable density scope of the sampling spot titanium diboride ceramic closed pore cenosphere of same batch of different positions is at ± 0.01g/cm
3.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, and the fluid loss that falls of cement briquette is less than 50ml/30min.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, and cement briquette rate of change of the density is less than 0.02.
Described titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, titanium diboride ceramic closed pore cenosphere resistance to hydrostatic pressure intensity 60 ~ 100MPa.
the present invention has the following advantages.
1, the dependence to flyash floating bead in long-term well cementation can be changed, it is good that titanium diboride ceramic material has ultimate compression strength height fold resistance, resistant to elevated temperatures ceramic material, high through high temperature sintering activity, size is controlled, and ceramic composite can meet the cementing requirements of warm oil well in 4000 ~ 6000 meters.
2, ceramic composite proportioning, sintering temperature can control, and the spray orifice size of rotating spraying shower nozzle is controlled, and this technique is advanced, and technology maturation, product performance are stable, and production cost is low, and output is high, and performance is good.
3
,the density of titanium diboride ceramic microballon can be controlled in 0.5g/cm
3~ 0.80g/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 jelly be formed, can early strength be improved.
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, expanding volume is relevant with expansion temperature and density of foaming agent, then through sintering, melting, finally formation closed pore cenosphere, prevents knot wall from adopting thermal cycling suction, wind-force blowing system to improve output.
5, 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 titanium diboride ceramic closed pore cenosphere is prepared burden and is fired: by particle diameter 1 ~ 15 μm of TiB2 powder, particle diameter 5 ~ 15 μm of dihydro titanium valves are after 95t%:5wt% mixing and stirring, be pressed into blank drying, 3 hours are fired at 1700 DEG C of vacuum atmosphere ovens, obtain the sintered compact of titanium diboride ceramic material, the sintered compact of titanium diboride ceramic material is processed into 10 ~ 15 μm of microballons at balling machine, 2. dosing: get 10 ~ 15 μm of titanium diboride ceramic microballon 78wt% and water 22wt%, 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 of titanium diboride ceramic closed pore cenospheres.
(2) 5 ~ 15 μm of titanium diboride ceramic 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 titanium diboride ceramic 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 titanium diboride ceramic 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 titanium diboride ceramic closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain titanium diboride ceramic 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 titanium diboride ceramic 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 45wt%, particle diameter 13 μm of superfine cement 10wt%, particle diameter.
(6) mix: get G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 10wt%, particle diameter is 5 ~ 15 μm of titanium diboride ceramic closed pore cenosphere 35wt%, the flyash 5wt% of loss on ignition 1.1%, 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 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 (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa), 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 titanium diboride ceramic 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/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 being defined on pressing machine of GB GB/T177.
Embodiment 2.
(1) 1. the preparation of titanium diboride ceramic closed pore cenosphere is prepared burden and is fired: by particle diameter 20 ~ 35 μm of TiB2 powder, particle diameter 20 ~ 30 μm of dihydro titanium valves are after 96wt%:4wt% mixing and stirring, be pressed into blank drying, 2.5 hours are fired at 1800 DEG C of vacuum atmosphere ovens, obtain the sintered compact of titanium diboride ceramic material, the sintered compact of titanium diboride ceramic material is processed into 20 ~ 25 μm of microballon 2. dosings at balling machine: 20 ~ 25 μm titanium diboride ceramic microballon 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, 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 ~ 30 μm of titanium diboride ceramic closed pore cenospheres.
(2) particle diameter 20 ~ 30 μm of titanium diboride ceramic 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 titanium diboride ceramic 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 titanium diboride ceramic 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 titanium diboride ceramic closed pore cenosphere size distribution are analyzed with laser particle size analyzer: wind-force is cleaned classification and obtain titanium diboride ceramic 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%, particle diameter 13 μm of superfine cement 15wt%, particle diameter be 20 ~ 30 μm of titanium diboride ceramic 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%.
(6) mix: get G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 15wt%, particle diameter is 20 ~ 30 μm of titanium diboride ceramic closed pore cenosphere 30wt%, the flyash 6wt% of loss on ignition 1.1%, 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 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 (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa), 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/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 being defined on pressing machine of GB GB/T177.
Embodiment 3.
(1) 1. the preparation of titanium diboride ceramic closed pore cenosphere is prepared burden and is fired: by particle diameter 40 ~ 50 μm of TiB2 powder, particle diameter 35 ~ 45 μm of dihydro titanium valves are after 97wt%:3wt% mixing and stirring, be pressed into blank drying, 2 hours are fired at 1900 DEG C of vacuum atmosphere ovens, obtain the sintered compact of titanium diboride ceramic material, the sintered compact of titanium diboride ceramic material is processed into 30 ~ 35 μm of microballons at balling machine, 2. dosing: 30 ~ 35 μm titanium diboride ceramic microballon 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 titanium diboride ceramic closed pore cenospheres.
(2) 35 ~ 50 μm of titanium diboride ceramic 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 titanium diboride ceramic closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) 35 ~ 50 μm of titanium diboride ceramic 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) 35 ~ 50 μm of titanium diboride ceramic closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain titanium diboride ceramic 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: by getting G level oil well cement 45wt%, particle diameter 13 μm of superfine cement 12wt%, particle diameter is titanium diboride ceramic 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%, particle diameter 13 μm of superfine cement 12wt%, particle diameter is 35 ~ 50 μm of titanium diboride ceramic closed pore cenosphere 33wt%, the flyash 7wt% of loss on ignition 1.1%, 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) 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 (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa), 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 titanium diboride ceramic 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/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 being defined on pressing machine 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. titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette, comprise the preparation of titanium diboride ceramic 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 TiB2 powder and particle diameter 5 ~ 45 μm of titanium hydride sintering aids 95 ~ 97wt%:3 ~ 5wt% by weight, first by TiB2 powder and titanium hydride sintering aid mixing and stirring, be pressed into blank drying, 2 ~ 3 hours are fired at 1700 ~ 1900 DEG C of vacuum atmosphere ovens, obtain the sintered compact of titanium diboride ceramic material, the sintered compact of titanium diboride ceramic material is processed into 10 ~ 35 μm of microballons at balling machine, the weight percent of titanium diboride ceramic microballon liquid slurry consists of: particle diameter 10 ~ 35 μm titanium diboride ceramic microballon 70 ~ 80wt%: water 20 ~ 30wt%, adding whipping agent in titanium diboride ceramic microballon liquid slurry is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L, titanium diboride ceramic microballon liquid starches abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballon, 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, clean classification through wind-force and obtain 5 ~ 50 μm of titanium diboride ceramic closed pore cenospheres, by G level oil well cement 40 ~ 50wt%, particle diameter 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the titanium diboride ceramic 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 titanium diboride ceramic 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. titanium diboride ceramic microballon according to claim 1 prepares the method for low density oil well cementing cement briquette, it is characterized in that: titanium diboride ceramic closed pore cenosphere its floatability is greater than 95%.
3. titanium diboride ceramic microballon according to claim 1 prepares the method for low density 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 20MPa.
4. titanium diboride ceramic microballon according to claim 1 prepares the method for low density oil well cementing cement briquette, it is characterized in that: the variable density scope of the titanium diboride ceramic closed pore cenosphere of the sampling spot of same batch of different positions is at ± 0.01g/cm
3.
5. titanium diboride ceramic microballon according to claim 1 prepares the method for low density oil well cementing cement briquette, it is characterized in that: the fluid loss that falls of cement briquette is less than 50ml/30min.
6. titanium diboride ceramic microballon according to claim 1 prepares the method for low density oil well cementing cement briquette, it is characterized in that: cement briquette rate of change of the density is less than 0.02.
7. titanium diboride ceramic microballon according to claim 1 prepares the method for low density oil well cementing cement briquette, it is characterized in that: titanium diboride ceramic closed pore cenosphere resistance to hydrostatic pressure intensity 60 ~ 100MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1356291A (en) * | 2001-12-29 | 2002-07-03 | 中国核动力研究设计院 | Non-pressure sinter process for compact ZrB2 or TiB2 ceramic material |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1356291A (en) * | 2001-12-29 | 2002-07-03 | 中国核动力研究设计院 | Non-pressure sinter process for compact ZrB2 or TiB2 ceramic material |
| 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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