CN103467019A - Method for preparing low-density oil well cementing cement briquettes by using vanadium carbide microspheres - Google Patents
Method for preparing low-density oil well cementing cement briquettes by using vanadium carbide microspheres Download PDFInfo
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- CN103467019A CN103467019A CN2013103885498A CN201310388549A CN103467019A CN 103467019 A CN103467019 A CN 103467019A CN 2013103885498 A CN2013103885498 A CN 2013103885498A CN 201310388549 A CN201310388549 A CN 201310388549A CN 103467019 A CN103467019 A CN 103467019A
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- vanadium carbide
- oil well
- closed pore
- well cementing
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Abstract
The invention provides a method for preparing low-density oil well cementing cement briquettes by using vanadium carbide blind-hole hollow microspheres. The method comprises preparation of vanadium carbide hollow microspheres, dosing, mixing, stirring and size-mixing, die testing and strength test, and is characterized by carrying out stirring and size-mixing for 40s to 55 to 65wt% of G-grade oil well cement, 25 to 35wt% of blind-hole hollow vanadium carbide microspheres with particle size of 10-100mu m, 5 to 7wt% of fly ash with loss on ignition of 1.1%, 1.5 to 2wt% of calcium oxide with purity of 99.9%, 0.5 to 1.0wt% of sodium sulfate and 1 to 3wt% of micro-silicon in a stirrer according to a water cement ratio of 0.5-0.7 (W/C), pouring into two test molds in one group, wherein length, width and height of each test mold are 53mm, 53mm and 53mm respectively, curing for 24h and 48h in a water-bath curing box at the constant temperature of 52 DEG C, immersing for 1h in cold water after de-molding, and then carrying out strength test.
Description
Technical field
The present invention relates to a kind ofly with vanadium carbide closed pore cenosphere, prepare the method for low density oil well cementing cement briquette, belong to the material technology field.
Background technology
Current domestic well cementation light-weight additive adopts the pearl that floats in flyash, at flyash, comprises heavy pearl and floats pearl, and heavy pearl density is at 1.1～2.8g/cm
3between, content accounts for flyash 30～70%, and floating pearl is the glass microballon that is less than water-mass density in flyash, floats pearl and mainly comprises aluminosilicate glass microballon and porous carbon granule, the pearl that floats of removing after carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, surfaces externally and internally is smooth, and volume is large, is a kind of rounded, light weight, closed pore is hollow, wear-resisting, high temperature resistant, thermal conductivity is little, intensity is high, float the pearl amount and account for 0.5～1% of flyash total amount, the aluminosilicate glass microballon is the hollow spherosome.
Floating pearl it be that coal dust is in thermal power plant boiler during through 1100～1500 ° of C burning in flyash wherein, the clayey material is melt into micro-drop, spin at a high speed under the hot air acting of turbulent flow in stove, form perfectly round sial spheroid, the gases such as nitrogen, hydrogen and carbonic acid gas that burning and scission reaction produce, in the high temperature aluminum silicon spheroid of melting, expand rapidly, under capillary effect, form the glass envelope of hollow, then enter flue cooling rapidly, after sclerosis, become the vitreous state cenosphere of high vacuum, i.e. fly ash float.
Flyash is put into to water and stir, standing for some time, be less than water-mass density owing to floating pearl density, will swim on the water surface and pull out and dry, be and float pearl.
In recent years, due to the impact of haze weather, the big-and-middle-sized thermal power generation of China adopted the desulfurization technology of environmental protection, and not containing and floating pearl in flyash, caused in short supply.
According to well cementation degree of depth difference, usually the oil well below 2000 meters low hot-well, (the interior temperature of oil well is between 70～90 ° of C, and cement slurry density is at 1.8 g/cm for highdensity grout for the low temperature oil well cementing
3～1.9 g/cm
3); Be middle hot-well between 2000～4000 meters, middle temperature oil well cementing with in the grout of density (temperature in oil well is between 90～150 ° of C, and cement slurry density is at 1.6 g/cm
3～1.7 g/cm
3); Below 4000 meters is hot hole, and (the interior temperature of oil well is between 150～240 ° of C, and cement slurry density is at 1.0 g/cm for low-density grout for high-temperature oil well well cementation
3～1.5 g/cm
3).
Summary of the invention
The object of the invention is to overcome the defect that prior art exists, provide a kind of cost low, excellent property, can replace the pearl of wafing in flyash, by the method for organic synthesis, makes closed pore cenosphere, density range 0.5 g/cm
3～0.7g/cm
3, and then configuration low density 1.0 g/cm
3～1.5g/cm
3the preparation method of oil well cementing cement briquette, meet the well cementing material requirement of different depths.
its technical scheme is.
Comprise the preparation of vanadium carbide microballon, batching, mix, stirring is sized mixing, die trial, strength trial, it is characterized in that: by G level oil well cement 55～65 wt%, hollow vanadium carbide microballon 25～35 wt% of the closed pore that particle diameter is 10～100 μ m, flyash 5～7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5～2 wt%, sodium sulfate 0.5～1.0 wt% and micro-silicon 1～3 wt%, with 0.5～0.7(W/C) water cement ratio stir and size mixing 40 seconds in stirrer, pour die trial (one group of two block length into, wide, high 53mm*53mm*53mm respectively), in the water-bath maintaining box of 52 ° of C of constant temperature, maintenance is 24 hours, 48 hours, after the demoulding, in cold water, soak 1 hour, make a strength test.
Describedly a kind ofly with vanadium carbide closed pore cenosphere, prepare the method for low density oil well cementing cement briquette, it is characterized in that: by particle diameter 1～30 μ m Vanadium Pentoxide in FLAKES and resol weight ratio 1:0.8～1, become powder mix in stirrer for mixing, at the temperature of 40～100 ° of C, solidify, and then make 50～100 μ m powder, by 50～100 μ m powder mixs at 1～3Mpa briquetting press upper holder block, on the electric furnace of 1300～1800 ° of C, sintering obtains the vanadium carbide block in 5～8 hours, block vanadium carbide is made to 5～30 μ m circular solids microballoons on balling machine.
Describedly a kind ofly with vanadium carbide closed pore cenosphere, prepare the method for low density oil well cementing cement briquette, it is characterized in that: the weight percent of vanadium carbide liquid slurry consists of: 5～30 μ m vanadium carbide 60～70 wt%, water 30～40 wt%.
Describedly a kind ofly with vanadium carbide closed pore cenosphere, prepare the preparation method of low density oil well cementing cement briquette, it is characterized in that: adding whipping agent in vanadium carbide liquid slurry is light calcium carbonate, and the concentration of use is 1～3g/L.
Described vanadium carbide closed pore cenosphere prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: vanadium carbide liquid is starched to abundant agitation and filtration, adopt the high speed centrifugation rotary spraying technique, form on microballoon ， tetra-district's electric furnaces and obtain 10～100 μ m vanadium carbide closed pore cenospheres through dehydration expansion, sintering, melting, balling-up through classification.
Describedly a kind ofly with vanadium carbide closed pore cenosphere, prepare the preparation method of low density oil well cementing cement briquette, it is characterized in that: the microballon its floatability of preparation is greater than 90%.
Describedly a kind ofly with vanadium carbide closed pore cenosphere, prepare the preparation method of low density oil well cementing cement briquette, it is characterized in that: 8 hours ultimate compression strength of the cement briquette of preparation is greater than 10MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
The present invention has the following advantages.
1, can make the required lightening material of oil well cementing by methodology of organic synthesis.
2, be not subject to the restriction of envrionment conditions, the high-activity carbon that can utilize resol to form reduces Vanadium Pentoxide in FLAKES fully for carbon source and generates vanadium carbide.
3, vanadium carbide closed pore cenosphere particle diameter is controlled, and the particle diameter of particle is determined according to actual needs.
4, this technical matters advanced person, product performance are stable, and production cost is low, and output is high, and performance is good, has opened up the synthetic virgin material new way of well cementation.
Embodiment
Embodiment 1.
(1) 1. preparation of vanadium carbide closed pore cenosphere preparation: particle diameter 1～10 μ m Vanadium Pentoxide in FLAKES is become to powder mix with resol weight ratio 1:0.8 in stirrer for mixing, at the temperature of 40 ° of C, solidify, and then make 50 μ m powder, by 50 μ m powder at 1Mpa briquetting press upper holder block, on the electric furnace of 1300 degree, sintering obtains the vanadium carbide block in 5 hours, block vanadium carbide is made to 5～10 μ m circular solids microballoons on balling machine.2. dosing: the weight percent of vanadium carbide liquid slurry consists of: particle diameter 5～10 μ m vanadium carbide 60 wt%,, water 40 wt%, add the light calcium carbonate whipping agent in vanadium carbide liquid slurry, concentration is 1g/L, 3. stirs: by proportioning, good vanadium carbide solution is put into agitator and is stirred; 4. filter: by macrobead and Impurity removal; 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form process dehydration expansion, sintering, melting, balling-up on microballoon ， tetra-district's electric furnaces, through classification, obtain 10～30 μ m vanadium carbide closed pore cenospheres.
(2) low density oil well cementing cement briquette batching: get hollow vanadium carbide microballon 25 wt% of closed pore of G level oil well cement 65 wt%, 10～30 μ m, flyash 5 wt%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5 wt% and micro-silicon 3.0 wt% of loss on ignition 1.1%.
(3) mix: get hollow vanadium carbide microballon 25 wt% of closed pore of G level oil well cement 65 wt%, 10～30 μ m, flyash 5 wt%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5 wt% and micro-silicon 3.0 wt% of loss on ignition 1.1% and mix.
(4) get in (3) mix sample a little, pour in beaker, by 0.7 water cement ratio modulation grout,, with glass stick, stir, pour weighing density in mud scale into.
(5) under 28 ° of C ± 1 ° C of temperature, with 0.7(W/C) water cement ratio pour the corrugation agitator into, under even low speed, in 20 seconds, all mix, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, within standing 5 minutes, observe the grout homogeneity.
(6) grout be stirred is poured in the die trial of a group two, the specification of die trial is long 53mm, the high 53mm of wide 53mm.
(7) maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked 1 hour after the demoulding in cold water, by the regulation of GB GB/T 177, carries out ultimate compression strength and folding strength test and rate of change of the density experiment.
(8) maintenance 48 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked 1 hour after the demoulding in cold water, by the regulation of GB GB/T 177, carries out ultimate compression strength and folding strength test and rate of change of the density experiment.
Embodiment 2.
(1) 1. preparation of vanadium carbide closed pore cenosphere preparation: particle diameter 10～20 μ m Vanadium Pentoxide in FLAKESs are become to powder mix with resol weight ratio 1:0.9 in stirrer for mixing, at the temperature of 70 ° of C, solidify, and then make 70 μ m powder, by 70 μ m powder at 2Mpa briquetting press upper holder block, on the electric furnace of 1500 degree, sintering obtains the vanadium carbide block in 6 hours, block vanadium carbide is made to 10～20 μ m circular solids microballoons on balling machine.2. dosing: the weight percent of vanadium carbide liquid slurry consists of: particle diameter 10～20 μ m vanadium carbide 65 wt%,, water 35 wt%, adding light calcium carbonate in vanadium carbide liquid slurry is whipping agent, concentration is 2g/L, 3. stirs: by proportioning, good vanadium carbide solution is put into agitator and is stirred; 4. filter: by macrobead and Impurity removal; 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form process dehydration expansion, sintering, melting, balling-up on microballoon ， tetra-district's electric furnaces, through classification, obtain 40～60 μ m vanadium carbide closed pore cenospheres.
(2) low density oil well cementing cement briquette batching: flyash 6 wt% of hollow vanadium carbide microballon 30 wt% of the closed pore of G level oil well cement 60 wt%, 40～60 μ m, loss on ignition 1.1%, purity 99.9% calcium oxide 2.0 wt%, sodium sulfate 0.5 wt% and micro-silicon 1.5 wt% are fully mixed.
(3) mix: flyash 6 wt% of hollow vanadium carbide microballon 30 wt% of the closed pore of G level oil well cement 60 wt%, 40～60 μ m, loss on ignition 1.1%, purity 99.9% calcium oxide 2.0 wt%, sodium sulfate 0.5 wt% and micro-silicon 1.5 wt% are fully mixed.
(4) get in (3) mix sample a little, pour in beaker, by 0.6 water cement ratio modulation grout,, with glass stick, stir, pour weighing density in mud scale into.
(5) under 28 ° of C ± 1 ° C of temperature, with 0.6(W/C) water cement ratio pour the corrugation agitator into, under even low speed, in 20 seconds, all mix, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, within standing 5 minutes, observe the grout homogeneity.
(6) grout be stirred is poured in the die trial of a group two, the specification of die trial is long 53mm, the high 53mm of wide 53mm.
(7) maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked 1 hour after the demoulding in cold water, by the regulation of GB GB/T 177, carries out ultimate compression strength and folding strength test and rate of change of the density experiment.
(8) maintenance 48 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked 1 hour after the demoulding in cold water, by the regulation of GB GB/T 177, carries out ultimate compression strength and folding strength test and rate of change of the density experiment.
Embodiment 3.
(1) 1. preparation of vanadium carbide closed pore cenosphere preparation: particle diameter 20～30 μ m Vanadium Pentoxide in FLAKESs are become to powder mix with resol weight ratio 1:1 in stirrer for mixing, at the temperature of 100 ° of C, solidify, and then make 100 μ m powder, by 100 μ m powder at 3Mpa briquetting press upper holder block, on the electric furnace of 1800 ° of C, sintering obtains the vanadium carbide block in 8 hours, block vanadium carbide is made to 20～30 μ m circular solids microballoons on balling machine.2. dosing: the weight percent of vanadium carbide liquid slurry consists of: particle diameter 20～30 μ m vanadium carbide 70 wt%,, water 40 wt%, adding light calcium carbonate in vanadium carbide liquid slurry is whipping agent, concentration is 3g/L, 3. stirs: by proportioning, good vanadium carbide solution is put into agitator and is stirred; 4. filter: by macrobead and Impurity removal; 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form process dehydration expansion, sintering, melting, balling-up on microballoon ， tetra-district's electric furnaces, through classification, obtain 70～100 μ m vanadium carbide closed pore cenospheres.
(2) low density oil well cementing cement briquette batching: flyash 7 wt% of hollow vanadium carbide microballon 35 wt% of the closed pore of G level oil well cement 55 wt%, 70～100 μ m, loss on ignition 1.1%, purity 99.9% calcium oxide 1.0 wt%, sodium sulfate 1.0 wt% and micro-silicon 1.0 wt% are fully mixed.
(3) mix: flyash 7 wt% of hollow vanadium carbide microballon 35 wt% of the closed pore of G level oil well cement 55 wt%, 70～100 μ m, loss on ignition 1.1%, purity 99.9% calcium oxide 1.0 wt%, sodium sulfate 1.0 wt% and micro-silicon 1.0 wt% are fully mixed.
(4) get in (3) mix sample a little, pour in beaker, by 0.5 water cement ratio modulation grout,, with glass stick, stir, pour weighing density in mud scale into.
(5) under 28 ° of C ± 1 ° C of temperature, with 0.5(W/C) water cement ratio pour the corrugation agitator into, under even low speed, in 20 seconds, all mix, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, within standing 5 minutes, observe the grout homogeneity.
(6) grout be stirred is poured in the die trial of a group two, the specification of die trial is long 53mm, the high 53mm of wide 53mm.
(7) maintenance 24 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked 1 hour after the demoulding in cold water, by the regulation of GB GB/T 177, carries out ultimate compression strength and folding strength test and rate of change of the density experiment.
(8) maintenance 48 hours in the water-bath maintaining box of 52 ° of C of constant temperature is soaked 1 hour after the demoulding in cold water, by the regulation of GB GB/T 177, carries out ultimate compression strength and folding strength test.
Claims (7)
1. one kind prepares the method for low density oil well cementing cement briquette with vanadium carbide closed pore cenosphere, comprise the preparation of vanadium carbide microballon, batching, mix, stirring is sized mixing, die trial, strength trial, it is characterized in that: by G level oil well cement 55～65 wt%, hollow vanadium carbide microballon 25～35 wt% of the closed pore that particle diameter is 10～100 μ m, flyash 5～7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5～2 wt%, sodium sulfate 0.5～1.0 wt% and micro-silicon 1～3 wt%, with 0.5～0.7(W/C) water cement ratio stir and size mixing 40 seconds in stirrer, pour die trial (one group of two block length into, wide, high 53mm*53mm*53mm respectively), in the water-bath maintaining box of 52 ° of C of constant temperature, maintenance is 24 hours, 48 hours, after the demoulding, in cold water, soak 1 hour, make a strength test.
2. according to claim 1ly a kind ofly with vanadium carbide closed pore cenosphere, prepare the method for low density oil well cementing cement briquette, it is characterized in that: by particle diameter 1～30 μ m Vanadium Pentoxide in FLAKES and resol weight ratio 1:0.8～1, become powder mix in stirrer for mixing, at the temperature of 40～100 ° of C, solidify, and then make 50～100 μ m powder, by 50～100 μ m powder mixs at 1～3Mpa briquetting press upper holder block, on the electric furnace of 1300～1800 ° of C, sintering obtains the vanadium carbide block in 5～8 hours, block vanadium carbide is made to 5～30 μ m circular solids microballoons on balling machine.
3. according to claim 1ly a kind ofly with vanadium carbide closed pore cenosphere, prepare the method for low density oil well cementing cement briquette, it is characterized in that: the weight percent of vanadium carbide liquid slurry consists of: 5～30 μ m vanadium carbide 60～70 wt%,, water 30～40 wt%.
4. a kind of preparation method who prepares the cement briquette of low density oil well cementing with the vanadium carbide microballon according to claim 1 is characterized in that: adding whipping agent in vanadium carbide liquid slurry is light calcium carbonate, and the concentration of use is 1～3g/L.
5. vanadium carbide closed pore cenosphere according to claim 1 prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: vanadium carbide liquid is starched to abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, through dehydration expansion, sintering, melting, balling-up, through classification, obtain 10～100 μ m vanadium carbide closed pore cenospheres on four district's electric furnaces.
6. according to claim 1ly a kind ofly with vanadium carbide closed pore cenosphere, prepare the preparation method of low density oil well cementing cement briquette, it is characterized in that: the vanadium carbide closed pore cenosphere its floatability of preparation is greater than 90%.
7. according to claim 1ly a kind ofly with vanadium carbide closed pore cenosphere, prepare the preparation method of low density oil well cementing cement briquette, it is characterized in that: 8 hours ultimate compression strength of the cement briquette of preparation is greater than 10MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592963A (en) * | 2015-01-06 | 2015-05-06 | 山东理工大学 | Method for preparing oil well cementing test block resistant to high temperatures and high pressures from aluminum diatomite ceramic microspheres |
Citations (3)
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|---|---|---|---|---|
| CN1367768A (en) * | 1999-07-29 | 2002-09-04 | 索菲泰克公司 | Low-density and Low-porosity cementing slurry for oil wells or the like |
| CN1721353A (en) * | 2004-07-12 | 2006-01-18 | 四川嘉华企业（集团）股份有限公司 | High strength and low density oil well cement |
| CN103045214A (en) * | 2013-01-16 | 2013-04-17 | 西南石油大学 | Plugging thixotropic cement paste for oil-gas well and preparation method for same |
-
2013
- 2013-09-02 CN CN201310388549.8A patent/CN103467019B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367768A (en) * | 1999-07-29 | 2002-09-04 | 索菲泰克公司 | Low-density and Low-porosity cementing slurry for oil wells or the like |
| CN1721353A (en) * | 2004-07-12 | 2006-01-18 | 四川嘉华企业（集团）股份有限公司 | High strength and low density oil well cement |
| CN103045214A (en) * | 2013-01-16 | 2013-04-17 | 西南石油大学 | Plugging thixotropic cement paste for oil-gas well and preparation method for same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592963A (en) * | 2015-01-06 | 2015-05-06 | 山东理工大学 | Method for preparing oil well cementing test block resistant to high temperatures and high pressures from aluminum diatomite ceramic microspheres |
| CN104592963B (en) * | 2015-01-06 | 2018-03-06 | 山东理工大学 | The method that aluminium diatomite ceramic fine bead prepares high-temperature-resistant high-pressure-resistant oil well cementing test block |
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| CN103467019B (en) | 2015-06-17 |
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