CN107807230A - Carborundum kaolin ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak - Google Patents
Carborundum kaolin ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak Download PDFInfo
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- CN107807230A CN107807230A CN201711168613.6A CN201711168613A CN107807230A CN 107807230 A CN107807230 A CN 107807230A CN 201711168613 A CN201711168613 A CN 201711168613A CN 107807230 A CN107807230 A CN 107807230A
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- slurries
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- well
- well cementation
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- 238000012360 testing method Methods 0.000 title claims abstract description 64
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000005995 Aluminium silicate Substances 0.000 title claims abstract description 53
- 235000012211 aluminium silicate Nutrition 0.000 title claims abstract description 53
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 52
- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 239000011324 bead Substances 0.000 title claims abstract description 34
- 239000003129 oil well Substances 0.000 title claims abstract description 24
- 238000011056 performance test Methods 0.000 title claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 85
- 239000011148 porous material Substances 0.000 claims abstract description 27
- 239000004568 cement Substances 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000004411 aluminium Substances 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004088 foaming agent Substances 0.000 claims abstract description 11
- 239000010881 fly ash Substances 0.000 claims abstract description 10
- 230000008859 change Effects 0.000 claims abstract description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000292 calcium oxide Substances 0.000 claims abstract description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 235000013312 flour Nutrition 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000010998 test method Methods 0.000 claims abstract 2
- 230000018044 dehydration Effects 0.000 claims description 23
- 238000006297 dehydration reaction Methods 0.000 claims description 23
- 230000006835 compression Effects 0.000 claims description 18
- 238000007906 compression Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 16
- 239000000499 gel Substances 0.000 claims description 10
- 238000006703 hydration reaction Methods 0.000 claims description 10
- 239000011083 cement mortar Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000002474 experimental method Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 230000035699 permeability Effects 0.000 claims description 7
- 230000036571 hydration Effects 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000000378 calcium silicate Substances 0.000 claims description 5
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 5
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000009434 installation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 239000011440 grout Substances 0.000 claims description 3
- 239000002956 ash Substances 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 description 16
- 239000002131 composite material Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000007667 floating Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 3
- 230000002742 anti-folding effect Effects 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000006071 cream Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000001458 anti-acid effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000000703 high-speed centrifugation Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 210000002966 serum Anatomy 0.000 description 2
- 239000004484 Briquette Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001399 aluminium compounds Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/38—Concrete; Lime; Mortar; Gypsum; Bricks; Ceramics; Glass
- G01N33/388—Ceramics
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Ceramic Engineering (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The present invention provides a kind of modified carborundum kaolin ceramic fine bead and prepares oil well anti-gas-leak well cementation test block method of testing,By the wt% of G levels oil-well cement 40~50,The wt% of superfine cement 10~15,Particle diameter is the hollow wt% of carborundum kaolin ceramic fine bead 25~35 of 50~300 μm of modified closed pores,The wt% of flyash 5~7 of loss on ignition 1.1%,Purity 99.9%,The wt% of calcium oxide 1.5~2,1~5wt% of 0.5~1.0wt% of sodium sulphate and silica flour,Obtain compound,The percentage by weight sum of above component is 100%,Compound stirs,Sized mixing with 0.5~0.7 ratio of mud,Add the aluminium foaming agent that compound gross weight is 0.2~0.5%,It is prepared into dilatant slurry,Carry out the density of dilatant slurry,Acid-base value determines,Uniformity test,Rate of change of the density is tested and anti-gas-leak performance test.
Description
Technical field
The present invention relates to carborundum kaolin ceramic fine bead to prepare the well cementation test block performance test of oil well anti-gas-leak, belongs to material
Technology is led.
Background technology
At present, both at home and abroad in oil well cementing, extremely-low density cement is used for HTHP oil well, but use flyash
Floating bead, compression strength is low, and cement slurry density rate of change is big, after the static solidification of cement mortar, leaks air, blind hole, in addition, fine coal
The ratio of the palliatives such as grey floating bead must be controlled within 40%, and otherwise, palliative can influence the pressure resistance of cementing concrete test block
Degree, the density of palliative cement briquette within 40% is in 1.2g/cm3More than, depending merely on the ratio of increase palliative reduces cement
The density of test block is infeasible.
The content of the invention
Using modified carborundum kaolin ceramic material as palliative, improve well cementation and try fast resistance to compression, anti-folding, resistance to height
Warm, corrosion resistant performance, adds foaming agent in cement mortar, forms the slurries of expansion, reduces the density of slurries, reduces shaft bottom
Pressure, spawn is generated in hydration process, the basal body structure hole of cement mortar diminishes, and forms the well cementation examination of high vapour lock
Block, the permeability of well cementation test block is reduced, improve the flow of pore resistance of well cementation test block, prevent slurries in well cementation because losing
Weight, leaks air, and anti-pressure ability declines.
Its technical scheme is：
Carborundum kaolin composite material ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak, comprises the following steps：
A, the preparation of the hollow carborundum kaolin ceramic fine bead of modified closed pore：
The preparation of the first step, base-material：By 20~50 μm of carborundum powders of particle diameter, 10~50 μm of kaolin of particle diameter, 20~50 μm of oxidations
Aluminium powder is by weight：70~85wt%：5~20wt%：20~30wt% is sampled, and obtains mixed powder, the percentage by weight of above component
Sum is 100%；
The modified firing of second step, base-material：After the first step is mixed evenly, add mixed powder gross weight 5~
8wt% also primary resins are stirred in mixer, and blank is pressed into harder, are dried 6~12 hours at 100~300 DEG C,
Insulation is fired 2~4 hours in 1500~1650 DEG C of electric reduction furnaces, obtains being modified carborundum kaolin ceramic block by replacing reaction
Body, modified carborundum kaolinization, which studies, point to change, and carborundum kaolin has higher resistance to compression and fracture resistance, high
Ridge soil has stronger adsorptivity to different kinds of ions, alumina refractory performance, modified carborundum kaolin resistance to compression, resists
Folding, anti-erosion, anti-aging, acid and alkali-resistance, resistance to elevated temperatures improve；
The preparation of 3rd step, modified solid silicon carbide kaolin ceramic fine bead：Second step is obtained into carborundum kaolin ceramic block
Body is processed into the solid modified hollow carborundum kaolin composite material pottery of closed pore of 5~50 μm of spherical shapes of particle diameter on balling machine
Porcelain microballon, nodularization processing is that blower fan blows afloat material, and the rotary motion phase mutual friction between material is in spherical particle, and wall thickness is equal
Even, the particle of spherical shape is uniform in each particle stress distribution, and compression strength is big；
It is prepared by the 4th step, the modified hollow carborundum kaolin composite material ceramics slurries of closed pore：The hundred of carborundum kaolin slurry
Divide than composition and be：5~50 μm of wt% of solid silicon carbide kaolin ceramic fine bead 65~70 of particle diameter：The wt% of water 30~35；
5th step, add foaming agent：Urea is added in the carborundum kaolin ceramics slurries prepared to the 4th step, concentration is 1~
3g/L, use N2H4CO, when the temperature in stove is increased to 135 DEG C, is decomposed as foaming agent agent and is produced CO2And NH3, make carborundum
Kaolin ceramic fine bead volume increases；
It is prepared by the 6th step, the modified hollow carborundum kaolin composite material ceramic fine bead of closed pore：5th step mixed serum is abundant
Agitation and filtration, using high-pressure injection high speed centrifugation rotary spraying technique, microballoon is formed, is controlled respectively in multi-region vertical drop oxygen-enriched
On combustion furnace by dehydration, expansion, high temperature sintering, melt surface vitreous, balling-up, by wind-force clean classification obtain wall thickness 15~
100 μm, the hollow carborundum kaolin ceramic fine bead of 50~300 μm of closed pores of particle diameter, floating bead wall thickness prepared by inorganic mineral material
Artificial controllable, compression strength is in 120~300MPa；
B, the modified hollow carborundum kaolin composite material ceramic fine bead of closed pore prepares the well cementation test block of oil well anti-gas-leak：
The first step, the dispensing of anti-gas-leak well cementation test block：By 40~50wt% of G level oil-well cements, 10~15wt% of superfine cement, particle diameter
For 25~35wt% of the hollow carborundum kaolin composite material ceramic fine bead of 50~300 μm of closed pores, the flyash of loss on ignition 1.1%
5~7wt%, the pure wt% of 99.9% calcium oxide 1.5~2,1~5wt% of 0.5~1.0wt% of sodium sulphate and silica flour, obtain compound, with
The percentage by weight sum of upper component is 100%, and using the flyash of loss on ignition 1.1%, according to accumulation principle, flyash is mainly filled out
Space between two kinds of material particle sizes of benefit G levels oil-well cement and the hollow carborundum kaolin ceramic fine bead of closed pore, different of particle diameter
When grain is tangent two-by-two, the gap between tangent circle is filled by flyash, G levels oil-well cement and glass microballoon grain is combined closely,
But it should control within the specific limits, that is, be controlled in the range of the 5~7% of gross weight in usage amount, otherwise, influence high temperature high voltage resistant
The intensity of test block, next to that the flyash generated by high temperature sintering, active, the hydration rate of slurries is significantly improved, burnt
The low flyash of vector needs the ratio of mud small, contributes to the early strong of test block of cementing the well, the calcium hydroxide of purity 99.9%, calcium oxide purity
Higher, activity is stronger, and hydration rate is fast, and generates gelatinous material calcium hydroxide, and beneficial to the early strong of slurries, temperature is to test block
Morning play an important role by force, the calcium hydroxide secondly generated after aquation can adjust the pH value of slurries, in alkalescent in alkalescence
Under the conditions of, the early strength of high temperature high voltage resistant oil-well cement can be improved, sodium sulphate is a kind of fluid loss agent, and drop dehydration effect is bright
It is aobvious, the sodium ion in sodium sulphate, there is counter-infiltration function, diffusion velocity is fast, slurries is separated out part water, sodium sulphate in solidification
How much is dosage, and the drop dehydration to slurries plays an important role, and is reacted using activated silica, aluminium and G level oil-well cements and generates aquation
Gel of calcium silicate shape and other gels, add the flow resistance in cement grout space and the pressure in space, reduce well cementation examination
The space of particle in block, improve the structure of slurries, reduce the permeability of well cementation test block, improve the compactness of well cementation test block and resist
Compressive Strength；
The preparation of second step, anti-gas-leak test block dilatant slurry：Compound is mixed to get by the percentage by weight sampling of the first step, and
Compound is stirred, sized mixing with 0.5~0.7 ratio of mud, wherein ash is compound, adding compound gross weight is
0.2~0.5% aluminium foaming agent, aluminium foaming agent for aluminium powder cream, aluminium powder or aluminium compound in one kind therein, aluminium foaming agent
Hydration reaction generates bubble, forms the slurries of expansion, reduces the density of slurries, reduce pressure, activated silica, aluminium and G accordingly
Level oil-well cement react generation hydrated calcium silicate gel shape material and other gels, the structure hole of cement mortar diminish, resist
The enhancing of pressure property, slurries are aspirated by liquid pump, spray the outer surface to high speed revolving drum, and producing centrifugal force in outer surface of cylinder will
Slurries are shed, and Stirring is shed in realization；
3rd step, testing performance index：
A, the measure of dilatant slurry density：The dilatant slurry for taking second step to prepare, pours into and density is weighed in fluid densitometer, expands
The density of slurries is in 0.8~1.2g/cm3Between, for the density of this slurries extremely-low density, the compression strength of test block is big, uses
Modified carborundum kaolin ceramic material, improve the resistance to compression of the hollow carborundum kaolin composite material ceramic fine bead of closed pore, resist
Folding, anti-erosion, ageing resistace；
B, the measure of dilatant slurry acid-base value：The dilatant slurry for taking second step to prepare, is poured into pH value tester, shows pH value,
The pH value of dilatant slurry is between 9.0~10.5；
C, the uniformity test of slurries：Take second step to prepare dilatant slurry and pour into settlement barrel, homogeneity is observed after 0.5 hour, surely
Qualitative, homogeneity is that the hollow carborundum kaolin composite material ceramic fine bead of closed pore mutually merges with slurries, and stability is no longer
Floating fluctuation, microballon are evenly distributed in dilatant slurry up and down；
D, the rate of change of the density experiment of test block：Second step is prepared into slurries, pours into one group of three pieces of length and width, high respectively 53mm*
In 53mm*53mm die trials, conserved respectively 24 hours, 48 hours, 96 hours, after the demoulding in the water-bath curing box of 52 DEG C of constant temperature
Soaked 1 hour in cold water, the test block after solidification is put into the enterprising line density rate of change of forcing press tests, and rate of change of the density is less than
0.02%；
E, anti-gas-leak performance test：Gas leakage occurs in slurries in process of setting, i.e., from mecystasis to the process of Solid State Transformation
In, the dilatant slurry for taking second step to prepare is poured into gas leakage analogue experiment installation, and gas leakage analogue experiment installation includes support, remote control
Oblique angle regulator, central tube, outer tube, pressurization hole, pressure tap, top cover labyrinth, lower sealing cover, the screen pack of electric digital display,
Central tube runs through outer tube, and center pipe diameter has a plurality of specifications, between 10~200 centimetres of internal diameter, is formed between central tube and outer tube
Annular space, annular space are mineshaft annulus, and central tube is provided with micropore with outer tube, by the slurries injection of expansion wherein, other parts
Rack-mount, test bracket angle of inclination is in the gap of influence of 0~90 ° of change to gas leakage, central tube and outer tube to slurry
The influence of liquid setting time and gas leakage, influence, the density of slurries influence to gas leakage of the quantity of dehydration to gas leakage drops, slurries lose
Again to the influence of gas leakage, hydration reaction drop dehydration is excessive, causes volume contraction excessive, and pressure is directly proportional to depth, from pressurization hole
Pressurization, pressurization scope pressure tap access digital pressure sensor, measure the slurries static pressure that annular space expands, mistake from 1~350MPa
Filter screen be provided with leak-off hole metering drop dehydration quantity, fluid loss should in 10~50mL/30min, single-factor measure respectively density,
Dehydration, drops in the influence of inclination angle, pressure to drop dehydration, the influence of multiple-factor density, inclination angle, force combination measurement to drop dehydration
It is how much directly related with gas leakage, and record and measure test bit, drop dehydration excessively causes the space and crack of test block, prevents slurries
It is weightless in solidification, cement the well test block gas leakage the reason for one of be due to cement the well test block density it is bigger, compressive load per unit area is bigger,
With well cementation depth down, base pressure is bigger, collapses, and using expanding cement, the density of slurries is reduced, so as to reduce
The pressure in shaft bottom, spawn is generated in hydration process, the basal body structure hole of cement mortar diminishes, and forms high vapour lock well cementation examination
Block, the permeability of well cementation test block is reduced, improve the flow of pore resistance of well cementation test block.
The present invention has advantages below.
1st, the displacement reaction by thermal reduction, generates the modified ceramic material containing high silicon, improves carborundum kaolin and closes
The performance such as the resistance to compression of hole hollow ceramic microspheres, anti-folding, anti-erosion, anti-aging.
2nd, using the slurries of expansion, the density of slurries is reduced, so as to reduce the pressure in shaft bottom.
3rd, activated silica, aluminium and G level oil-well cements, which react, generates hydrated calcium silicate gel shape material and other gels, water
The basal body structure hole of mud diminishes, and forms high vapour lock well cementation test block, reduces the permeability of well cementation test block, improves well cementation examination
The flow of pore resistance of block.
Brief description of the drawings
Fig. 1 is the test platform structure schematic diagram of the anti-gas-leak performance test of the embodiment of the present invention.
1, support 2, the oblique angle regulator 3 of remote control electric digital display, lower sealing cover 4, beaker wherein in figure
5th, screen pack 6, outer tube 7, central tube 8, top cover labyrinth 9, pressure tap 10, pressurization hole 11, compression pump 12, number
Word pressure sensor.
Embodiment
Embodiment 1.
Carborundum kaolin ceramic fine bead prepares oil well anti-gas-leak test block performance test, comprises the following steps：
A, the preparation of carborundum kaolin closed pore hollow ceramic microspheres：
The preparation of the first step, base-material：25 μm of carborundum kaolin powder of particle diameter, 40 μm of kaolin of particle diameter, 30 μm of alumina powders are pressed
Weight ratio：70wt%：15wt%：15wt% is sampled；
The modified firing of second step, base-material：After the first step is mixed evenly, the 5wt% of mixed powder gross weight is added
Also primary resin is stirred in mixer, and blank is pressed into harder, is dried 10 hours at 150 DEG C, in 1500 DEG C of reduction electricity
Insulation is fired 4 hours in stove, obtains being modified carborundum kaolin ceramic block, modified carborundum kaolinite by replacing reaction
Native chemical composition changes, and aluminum oxide improves carborundum kaolin heat resistance, the increase of molecular link attraction, resistance to compression, resists
Folding, anti-erosion, anti-aging, acid and alkali-resistance, resistance to elevated temperatures improve；
The preparation of 3rd step, modified solid silicon carbide kaolin ceramic fine bead：Second step is obtained into carborundum kaolin block to exist
The solid silicon carbide kaolin ceramic fine bead of 30 μm of spherical shapes of particle diameter is processed on balling machine.
It is prepared by the 4th step, carborundum kaolin ceramics slurries：The percentage of carborundum kaolin slurry forms：Particle diameter
30 μm of solid silicon carbide kaolin ceramic fine bead 70wt%：Water 30wt%.
5th step, add foaming agent：Urea is added in the carborundum kaolin ceramics slurries prepared to the 4th step, concentration is
2.5g/L, use N2H4CO, when the temperature in stove is increased to 135 DEG C, is decomposed as foaming agent agent and is produced CO2And NH3, make ceramics
Microballon volume increases.
It is prepared by the 6th step, the modified hollow carborundum kaolin ceramic fine bead of closed pore：5th step mixed serum is sufficiently stirred
Filtering, using high-pressure injection high speed centrifugation rotary spraying technique, microballoon is formed, on the combustion furnace of multi-region vertical drop zonal control
By being dehydrated, expanding, high temperature sintering, melt surface vitreous, balling-up, clean classification by wind-force and obtain 250 μm of hollow carbon of closed pore
SiClx kaolin ceramic fine bead, carborundum kaolin closed pore hollow ceramic microspheres wall thickness is at 50 μm, more than the wall of other floating beads
Thickness, compression strength is in 200MPa.
B, the modified hollow carborundum kaolin ceramic fine bead of closed pore prepares oil well anti-gas-leak test block.
The first step, the dispensing of anti-gas-leak test block：G level oil-well cements 45wt%, superfine cement 15wt%, particle diameter are 250 μm
The hollow carborundum kaolin ceramic fine bead 30wt% of closed pore, loss on ignition 1.1% 20 μm of flyash 5wt% of particle diameter, the hydrogen of purity 99.9%
Calcium oxide 2.0wt%, sodium sulphate 1.0wt% and 5 μm of silica flour 2wt% of particle diameter, obtain compound.
The preparation of second step, anti-gas-leak test block dilatant slurry：Mixing is mixed to get by the percentage by weight sampling of the first step
Material, and compound is stirred, to be sized mixing with 0.55 ratio of mud, add aluminium powder cream, aluminium powder cream hydration reaction generates bubble,
The slurries of expansion are formed, reduce the density of slurries, activated silica, aluminium and G oil-well cements, which react, generates hydrated calcium silicate gel
Shape material and other gels, the basal body structure hole of cement mortar diminish, and slurries are aspirated by liquid pump, and high speed revolving drum is arrived in spraying
Outer surface, outer surface of cylinder produce centrifugal force slurries are shed, realization shed Stirring.
3rd step, testing performance index：
A, the measure of dilatant slurry density：Take second step to prepare slurries, pour into and density is weighed in fluid densitometer, dilatant slurry
Density is in 0.85g/cm3Between, the density of this slurries is extremely-low density, and the compression strength of test block is big, using modified carbonization
Silicon kaolin ceramic material, the resistance to compression of raising carborundum kaolin closed pore hollow ceramic microspheres, anti-folding, anti-erosion, ageing resistance
Energy.
B, the measure of dilatant slurry acid-base value：Take second step to prepare slurries, pour into pH value tester, show pH value, it is swollen
The pH value of swollen slurries is 9.5.
C, the uniformity test of slurries：Take second step to prepare dilatant slurry and pour into settlement barrel, observed after 0.5 hour homogeneous
Property, stability, homogeneity is that the hollow carborundum kaolin ceramic fine bead of closed pore mutually merges with slurries, and stability is no longer up and down
Floating fluctuation, microballon are evenly distributed in the slurries of expansion.
D, the rate of change of the density experiment of test block：Second step is prepared into slurries, the slurries being stirred pour into one group of two block length,
It is wide, high to be respectively in 53mm*53mm*53mm die trials, conserved respectively in the water-bath curing box of 52 DEG C of constant temperature 24 hours, it is 48 small
When, 96 hours, soaked 1 hour in cold water after the demoulding, by the test block after solidification be put on forcing press carry out test block density become
Rate is tested.
E, the performance test of anti-gas-leak well cementation test block：The dilatant slurry for taking second step to make pours into gas leakage analogue experiment installation
In, gas leakage analogue experiment installation includes support 1, the oblique angle regulator 2 of remote control electric digital display, central tube 7, outer tube 6, pressurization
Hole 10, pressure tap 9, top cover labyrinth 8, lower sealing cover 3, screen pack 5, wherein, central tube 7 runs through outer tube 6, and central tube 7 can be changed,
Annular space is formed between central tube 7 and outer tube 6, wherein, other parts are arranged on support 1 for the slurries injection of expansion, remote control electricity
The oblique angle regulator 2 of dynamic digital display makes the angle of inclination of support 1 for 35 °, 50 centimetres of the gap of central tube 7 and outer tube 6, measurement angle
Spend influence to grout cures, drop influence of the quantity of dehydration to gas leakage, the density of slurries in 0.85g/cm3To the shadow of gas leakage
Ring, drop dehydration is excessive caused by the space and crack of test block, and slurries weightlessness causes compression strength to decline, and pressure is with depth into just
Than being pressurizeed with compression pump 11 from pressurization hole 10, being pressurized to 280MPa, digital pressure sensor 12, the slurries of measurement annular space expansion
Static pressure, screen pack 5 are provided with the quantity of leak-off hole metering drop dehydration, and the drop fluid loss in beaker 4 is in 20mL/30min, unit
Drop dehydration meets cementing requirements in time, and single-factor measures the influence of density, inclination angle, pressure to drop dehydration, Jin Erying respectively
The gas leakage of oil well is rung, the influence of multiple-factor density, inclination angle, force combination measurement to drop dehydration, how much straight with gas leakage drops dehydration
Correlation is connect, the density for test block of cementing the well is bigger, and compressive load per unit area is bigger, and with well cementation depth down, base pressure is bigger, occurs
Collapse, using modified closed pore hollow silicon zircon ceramic fine bead, the slurries of expansion, reduce the density of slurries, solve slurries
Weightlessness, the pressure in shaft bottom is reduced, spawn is generated in hydration process, the basal body structure hole of cement mortar becomes
It is small, high vapour lock well cementation test block is formed, the flow of pore resistance of well cementation test block is improved, reduces the permeability of well cementation test block, carry
The high flow of pore resistance of well cementation test block.
Claims (1)
1. carborundum kaolin ceramic fine bead prepares oil well anti-gas-leak well cementation test block method of testing, comprise the following steps：
The first step, the dispensing of anti-gas-leak well cementation test block：By 40~50wt% of G level oil-well cements, 10~15wt% of superfine cement, particle diameter
For 25~35wt% of the hollow carborundum kaolin ceramic fine bead of 50~300 μm of closed pores, loss on ignition 1.1% 5~7wt% of flyash,
1.5~the 2wt% of calcium oxide of purity 99.9%, 0.5~1.0wt% of sodium sulphate and 1~5wt% of silica flour samplings, obtain compound, above group
The percentage by weight sum divided is 100%；
The preparation of second step, anti-gas-leak well cementation test block dilatant slurry：Mixing is mixed to get by the percentage by weight sampling of the first step
Material, compound is stirred, sized mixing with 0.5~0.7 ratio of mud, wherein ash is compound, adds compound gross weight
For 0.2~0.5% aluminium foaming agent, aluminium foaming agent hydration reaction generates bubble, forms the slurries of expansion, reduces the density of slurries,
Activated silica, aluminium and G level oil-well cements, which react, generates hydrated calcium silicate gel shape material and other gels, adds cement mortar
The flow resistance of liquid air gap and the pressure in space, reduce the space of particle in well cementation test block, improve the structure of slurries, reduce solid
The permeability of well test block, the compactness and compression strength of well cementation test block are improved, slurries are aspirated by liquid pump, are sprayed to rotation at a high speed
Walk around the outer surface of cylinder, produce centrifugal force in outer surface of cylinder and shed slurries, Stirring is shed in realization；
3rd step, the performance test of anti-gas-leak well cementation test block：The dilatant slurry for taking second step to make pours into gas leakage simulated experiment dress
In putting, gas leakage analogue experiment installation includes support（1）, remote control electric digital display oblique angle regulator（2）, central tube（7）, it is outer
Pipe（6）, pressurization hole（10）, pressure tap（9）, top cover labyrinth（8）, lower sealing cover（3）, screen pack（5）, wherein central tube（7）Pass through
Wear outer tube（6）, central tube（7）Diameter has plurality of specifications, central tube（7）With outer tube（6）Between form annular space, by the slurries of expansion
Wherein, other parts are arranged on support for injection（1）On, switch board is provided with keyboard, changes servomotor by input parameter
Corner, and then change support（1）Angle of inclination, test bracket（1）Influence of the different angles of inclination to gas leakage, central tube
（7）With outer tube（6）Gap to the influence of grout cures time and gas leakage, influence of the quantity to gas leakage of dropping dehydration, slurries
Influence of the density to gas leakage, influence of the slurries weightlessness to gas leakage, uses compression pump（11）From pressurization hole（10）Pressurization, pressure tap（9）
Access digital pressure sensor（12）, the slurries static pressure that annular space expands is measured, simulates the pressure value of different depth, screen pack
（5）The quantity of leak-off hole metering drop dehydration is provided with, drop dehydration enters beaker（4）Middle single-factor measure respectively density, inclination angle,
Pressure to drop dehydration influence, multiple-factor density, inclination angle, force combination measurement to drop dehydration influence, drop dehydration how much with
Gas leakage is directly related, and records and measure test bit, and the density for test block of cementing the well is bigger, and compressive load per unit area is bigger, with well cementation
Depth down, base pressure is bigger, collapses, using the modified hollow carborundum kaolin ceramic fine bead of closed pore, expansion
Slurries, the density of slurries is reduced, reduce the pressure in shaft bottom, spawn, the matrix of cement mortar are generated in hydration process
Structure hole diminishes, and forms high vapour lock well cementation test block, reduces the permeability of well cementation test block, improves the hole stream of well cementation test block
Dynamic resistance.
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Application publication date: 20180316 |