CN107870110A - Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block - Google Patents
Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block Download PDFInfo
- Publication number
- CN107870110A CN107870110A CN201711168608.5A CN201711168608A CN107870110A CN 107870110 A CN107870110 A CN 107870110A CN 201711168608 A CN201711168608 A CN 201711168608A CN 107870110 A CN107870110 A CN 107870110A
- Authority
- CN
- China
- Prior art keywords
- slurries
- test block
- well cementation
- density
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000012360 testing method Methods 0.000 title claims abstract description 66
- 229910052845 zircon Inorganic materials 0.000 title claims abstract description 54
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 48
- 239000010703 silicon Substances 0.000 title claims abstract description 48
- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- 239000011324 bead Substances 0.000 title claims abstract description 38
- 239000003129 oil well Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000011056 performance test Methods 0.000 title claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 91
- 239000011148 porous material Substances 0.000 claims abstract description 27
- 239000004568 cement Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004411 aluminium Substances 0.000 claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 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
- 239000004088 foaming agent Substances 0.000 claims abstract description 11
- 239000010881 fly ash Substances 0.000 claims abstract description 10
- 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 5
- 238000005070 sampling Methods 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000292 calcium oxide Substances 0.000 claims abstract description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000013312 flour Nutrition 0.000 claims abstract description 4
- 230000018044 dehydration Effects 0.000 claims description 23
- 238000006297 dehydration reaction Methods 0.000 claims description 23
- 230000006835 compression Effects 0.000 claims description 20
- 238000007906 compression Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 16
- 239000000499 gel Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000011083 cement mortar Substances 0.000 claims description 8
- 238000002474 experimental method Methods 0.000 claims description 8
- 238000006703 hydration reaction Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 230000035699 permeability 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
- 238000009434 installation Methods 0.000 claims description 5
- 239000011440 grout Substances 0.000 claims description 4
- 230000036571 hydration Effects 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 239000002956 ash Substances 0.000 claims description 2
- 238000009530 blood pressure measurement Methods 0.000 claims 1
- 238000004088 simulation Methods 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 7
- 239000007789 gas Substances 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000002742 anti-folding effect Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 150000003376 silicon Chemical class 0.000 description 6
- 238000007667 floating Methods 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000005995 Aluminium silicate Substances 0.000 description 3
- 235000012211 aluminium silicate Nutrition 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 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
- 230000001458 anti-acid effect Effects 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 238000001739 density measurement Methods 0.000 description 2
- 230000000694 effects Effects 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 210000002966 serum Anatomy 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 235000020681 well water Nutrition 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 239000004484 Briquette Substances 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000002131 composite material 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
- 238000009792 diffusion process Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 230000033001 locomotion Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000003921 oil Substances 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
- 238000011084 recovery Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- UVGLBOPDEUYYCS-UHFFFAOYSA-N silicon zirconium Chemical class [Si].[Zr] UVGLBOPDEUYYCS-UHFFFAOYSA-N 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
- 230000035882 stress Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
-
- 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
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)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention provides the performance test methods that a kind of silicon zircon ceramic fine bead prepares the well cementation test block of oil well anti-gas-leak,By 40~50wt% of G level oil-well cements,10~15wt% of superfine cement,Particle diameter is 50~250 μm of 25~35wt% of closed pore hollow silicon zircon ceramic fine bead,5~7wt% of flyash of loss on ignition 1.1%,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,Wherein 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 the performance test methods that silicon zircon ceramic fine bead prepares the well cementation test block of oil well anti-gas-leak, belong 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 silicon zircon ceramic material as palliative, improve well cementation and try fast resistance to compression, anti-folding, high temperature resistant, resistance to
The performance of corrosion, adds foaming agent in cement mortar, forms the slurries of expansion, reduces the density of slurries, prevents slurries from cementing the well
Middle to leak air because of weightlessness, anti-pressure ability declines.
Its technical scheme is：
Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block, comprises the following steps：
A, the preparation of modified closed pore hollow silicon zircon ceramic fine bead：
The preparation of the first step, base-material：1~50 μm of silicon dioxide powder of particle diameter, 5~50 μm of zirconia powders of particle diameter, 20~50 μm of kaolinites
Soil is by weight：70~85wt%：20~30wt%：5~20wt%, obtains mixed powder, wherein above each component percentage by weight it
With for 100%；
The modified firing of second step, base-material：After the first step is mixed evenly, add mixed powder gross weight 3~
5% phenolic resin is stirred in mixer, and blank is pressed into harder, is dried 6~12 hours at 100~300 DEG C,
Insulation is fired 2~4 hours in 1500~1650 DEG C of electric reduction furnaces, is obtained modified silicon zircon ceramic block by replacing reaction, is changed
The silicon zircon chemical composition of property changes, and zirconium oxide makes silicon zircon intensity enhancing, and kaolin puies forward silicon zircon resistance to elevated temperatures
Height, the increase of molecular link attraction, resistance to compression, anti-folding, anti-erosion, anti-aging, acid and alkali-resistance, resistance to elevated temperatures；
The preparation of 3rd step, modified solid silicon zircon ceramic fine bead：Second step is obtained into silicon zircon ceramic block on balling machine
Be processed into the solid silicon zircon ceramic fine bead of 5~50 μm of spherical shapes of particle diameter, nodularization processing is that blower fan blows afloat material, material it
Between the mutual friction of rotary motion phase be in spherical particle, uniform wall thickness, the particle of spherical shape is uniform in each particle stress distribution,
Compression strength is big；
It is prepared by the 4th step, modified silicon zircon ceramic slurry liquid：The percentage of silicon zircon slurries forms：5~50 μm of solid silicons of particle diameter
The wt% of zircon ceramic fine bead 65~70：The wt% of water 30~35；
5th step, add foaming agent：Urea is added in the silicon zircon ceramics slurries prepared to the 4th step, concentration is 1~3g/L, is used
N2H4CO, when the temperature in stove is increased to 135 DEG C, is decomposed as foaming agent and is produced CO2And NH3, increase ceramic fine bead volume
Greatly.
It is prepared by the 6th step, modified closed pore hollow silicon zircon composite ceramic fine bead：5th step mixed serum is fully stirred
Filtering is mixed, using high-pressure injection high speed centrifugation rotary spraying technique, microballoon is formed, in the oxygen-enriched combustion that multi-region vertical drop controls respectively
Burn on stove by dehydration, expansion, high temperature sintering, melt surface vitreous, balling-up, clean classification by wind-force and obtain wall thickness 15~50
μm, 50~250 μm of closed pore hollow silicon zircon ceramic fine beads of particle diameter, inorganic mineral material prepare floating bead wall thickness it is artificially controllable,
In 120~250MPa, compression strength depends on the content of silicon zircon and forms modified closed pore by high temperature sintering compression strength
Hollow silicon zircon ceramic fine bead；
B, modified closed pore hollow silicon zircon ceramic fine bead 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 50~250 μm of 25~35wt% of closed pore hollow silicon zircon ceramic fine bead, 5~7wt% of flyash, pure of loss on ignition 1.1%
99.9% 1.5~2wt% of calcium oxide, 1~5wt% of 0.5~1.0wt% of sodium sulphate and silica flour, obtain compound, the weight of above component
Percentage sum is 100%, and using the flyash of loss on ignition 1.1%, according to accumulation principle, flyash mainly fills up G level oil well water
Space between two kinds of material particle sizes of mud and closed pore hollow silicon zircon ceramic fine bead, it is tangent when the different particle of particle diameter is tangent two-by-two
Gap between circle is filled by flyash, G levels oil-well cement and glass microballoon grain is combined closely, but should be controlled in usage amount
In certain limit, that is, control in the range of the 5~7% of gross weight, otherwise, influence the intensity of high temperature high voltage resistant test block, next to that through
The flyash of high temperature sintering generation is crossed, it is active, the hydration rate of slurries is significantly improved, the low flyash of loss on ignition needs water
Gray scale is small, contributes to the early strong of test block of cementing the well, and the calcium hydroxide of purity 99.9%, calcium oxide purity is higher, and activity is stronger, aquation speed
Degree is fast, and generates gelatinous material calcium hydroxide, and beneficial to the early strong of slurries, temperature plays an important role by force to the morning of test block,
Secondly the calcium hydroxide generated after aquation can adjust the pH value of slurries, under weak basic condition, can improve high temperature resistant in alkalescence
The early strength of high pressure oil wells cement, sodium sulphate are a kind of fluid loss agents, and drop dehydration effect is obvious, the sodium ion in sodium sulphate,
With counter-infiltration function, diffusion velocity is fast, slurries is separated out part water in solidification, and how much is sodium sulphate dosage, to the drop of slurries
Dehydration plays an important role, and is reacted generation hydrated calcium silicate gel shape and other solidifying using activated silica, aluminium and G level oil-well cements
Glue, the flow resistance in cement grout space and the pressure in space are added, reduce the space of particle in well cementation test block, improve slurry
The structure of liquid, the permeability of well cementation test block is reduced, improve the compactness and compression strength of well cementation test block；
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 are one kind therein in the compound of aluminium foaming agent, aluminium powder or aluminium, and aluminium foams
Agent hydration reaction generates bubble, forms the slurries of expansion, reduces the density of slurries, reduces pressure accordingly, activated silica, aluminium with
G level oil-well cements 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, the testing performance index of anti-gas-leak well cementation test block：
A, the density measurement of dilatant slurry：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 silicon zircon ceramic material, the resistance to compression of raising closed pore hollow silicon zircon ceramic fine bead, anti-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 closed pore hollow silicon zircon ceramic fine bead mutually merges with slurries, and stability is no longer floating fluctuation up and down, micro-
Pearl is evenly distributed in dilatant slurry；
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 tries fast variable density
Rate is less than 0.02%；
E, the performance test of anti-gas-leak well cementation test block：Gas leakage occurs in slurries in process of setting, i.e., from mecystasis to solid-state
During transformation, the dilatant slurry for taking second step to prepare is poured into gas leakage analogue experiment installation, gas leakage analogue experiment installation bag
Include support, the oblique angle regulator of remote control electric digital display, central tube, outer tube, pressurization hole, pressure tap, top cover labyrinth, lower sealing
Lid, screen pack, central tube run through outer tube, and center pipe diameter has a plurality of specifications, between 10~200cm of internal diameter, central tube and outer tube
Between form annular space, annular space is mineshaft annulus, and central tube is provided with micropore with outer tube, and the slurries of expansion are injected wherein, its
Its part is rack-mount, and test bracket angle of inclination is in influence of 0~90 ° of change to gas leakage, central tube and outer tube
Gap to the influence of grout cures time and gas leakage, influence of the quantity to gas leakage for dropping dehydration, slurries density to the shadow of gas leakage
Ringing, influence of the slurries weightlessness to gas leakage, hydration reaction drop dehydration is excessive, causes volume contraction excessive, and pressure is directly proportional to depth,
From the pressurization of pressurization hole, for pressurization scope from 1~300MPa, pressure tap accesses digital pressure sensor, the slurries of measurement annular space expansion
Static pressure, screen pack are provided with the quantity of leak-off hole metering drop dehydration, and fluid loss it is excessive should to drop dehydration in 10~50mL/30min
Causing the space and crack of test block, single-factor measures density, inclination angle, pressure to dropping the influence of dehydration respectively, multiple-factor density,
The influence of inclination angle, force combination measurement to drop dehydration, how much directly related with gas leakage drop dehydration is, prevents slurries from being lost in solidification
Weight, the gas leakage of test block of cementing the well be one of reason 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
Power, spawn is generated in hydration process, the basal body structure hole of cement mortar diminishes, and forms high vapour lock well cementation test block, reduces
The permeability of well cementation test block, improve the flow of pore resistance of well cementation test block.
Oil-producing region is in safe operation state, improve the quality of well recovery, slurries are in process of setting, constriction coefficient
It is small, solve the weightlessness of slurries, reduce the density of slurries, spawn forms film, stops the invasion of aqueous vapor, be anti-well cementation
The key technology of gas leakage.
Using low-density cement mortar, palliative ratio is excessive, and compression strength declines, and weightlessness easily occurs in slurries well cementing process,
Palliative ratio is too small, and cement slurry density is excessive, and base pressure is bigger, collapses, and is the technical barrier that can not go beyond, and uses
Material it is different, its chemical property is also different.
The present invention has advantages below.
1st, the displacement reaction by thermal reduction, generates the modified ceramic material containing high silicon, it is hollow to improve silicon zircon closed pore
The performance such as the resistance to compression of ceramic fine bead, 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 structural representation of the testing stand 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 5, mistake wherein in figure
Filter screen 6, outer tube 7, central tube 8, top cover labyrinth 9, pressure tap 10, pressurization hole 11, compression pump 12, digital pressure sensing
Device.
Embodiment
Embodiment 1.
Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block, comprises the following steps：
A, the preparation of silicon zircon closed pore hollow ceramic microspheres：
The preparation of the first step, base-material：By 20 μm of silicon dioxide powders of particle diameter, 30 μm of zirconia powders of particle diameter, 20 μm of kaolin by weight
Than：70wt%：20wt%：10wt% is sampled.
The modified firing of second step, base-material：After the first step is mixed evenly, mixed powder gross weight is added
5wt% phenolic resin is stirred in mixer, and blank is pressed into harder, is dried 10 hours at 150 DEG C, at 1500 DEG C also
Insulation is fired 4 hours in former electric furnace, and modified silicon zircon ceramic block, modified silicon zircon chemical composition are obtained by replacing reaction
Changing, zirconium oxide makes silicon zircon intensity enhancing, and kaolin improves silicon zircon heat resistance, the increase of molecular link attraction,
Resistance to compression, anti-folding, anti-erosion, anti-aging, acid and alkali-resistance, resistance to elevated temperatures improve.
The preparation of 3rd step, modified solid silicon zircon ceramic fine bead：Second step is obtained into silicon zircon block on balling machine
It is processed into the solid silicon zircon ceramic fine bead of 30 μm of spherical shapes of particle diameter.
It is prepared by the 4th step, silicon zircon ceramics slurries：The percentage of silicon zircon slurries forms：30 μm of solid silicon zircons of particle diameter
Ceramic fine bead 70wt%：Water 30wt%.
5th step, add foaming agent：Urea, concentration 1.5g/ are added in the silicon zircon ceramics slurries prepared to the 4th step
L, use N2H4CO, when the temperature in stove is increased to 135 DEG C, is decomposed as foaming agent and is produced CO2And NH3, make ceramic fine bead volume
Increase.
It is prepared by the 6th step, modified closed pore hollow silicon zircon ceramic fine bead：5th step mixed serum is sufficiently stirred filtering, adopted
With high-pressure injection high speed centrifugation rotary spraying technique, microballoon is formed, by de- on the combustion furnace of multi-region vertical drop zonal control
Water, expansion, high temperature sintering, melt surface vitreous, balling-up, clean classification by wind-force and obtain 150 μm of closed pore hollow silicon zircon potteries
Porcelain microballon, closed pore hollow silicon zircon ceramic fine bead wall thickness is at 35 μm, and more than the wall thickness of other floating beads, compression strength is in 200MPa.
B, modified closed pore hollow silicon zircon ceramic fine bead 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 150 μm
Closed pore hollow silicon zircon ceramic fine bead 30wt%, loss on ignition 1.1% 20 μm of flyash 5wt% of particle diameter, the calcium hydroxide of purity 99.9%
2.0wt%, sodium sulphate 1.0wt% and 5 μm of silica flour 2wt% of particle diameter, obtain compound.
Second step, anti-gas-leak well cementation test block dilatant slurry preparation：Mixed by the percentage by weight sampling of the first step
Stir to compound, and by compound, sized mixing with 0.60 ratio of mud, add the aluminium that compound gross weight is 0.35%
Powder cream, aluminium powder cream hydration reaction generate bubble, form the slurries of expansion, reduce the density of slurries, activated silica, aluminium and G oil well water
Mud react generation hydrated calcium silicate gel shape material and other gels, the basal body structure hole of cement mortar diminish, slurries lead to
Liquid pump suction is crossed, sprays the outer surface to high speed revolving drum, producing centrifugal force in outer surface of cylinder sheds slurries, realizes and throws
Spill Stirring.
3rd step, the testing performance index of anti-gas-leak well cementation test block：
A, the density measurement of dilatant slurry：Take second step to prepare slurries, pour into and density is weighed in fluid densitometer, dilatant slurry
Density is in 0.95g/cm3Between, the density of this slurries is extremely-low density, and the compression strength of test block is big, using modified silicon zirconium
Native ceramic material, the resistance to compression of raising closed pore hollow silicon zircon ceramic microballon, anti-folding, anti-erosion, ageing resistace.
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 closed pore hollow silicon zircon ceramic fine bead mutually merges with slurries, and stability is no longer to float ripple up and down
Dynamic, microballon is 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, the test block after solidification is put into the enterprising line density rate of change of forcing press tries
Test.
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 15 °, 30 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 0.95g/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 200MPa, 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. silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block, 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 50~250 μm of 25~35wt% of closed pore hollow silicon zircon ceramic fine bead, 5~7wt% of flyash of loss on ignition 1.1%, purity
99.9% 1.5~2wt% of calcium oxide, 0.5~1.0wt% of sodium sulphate and 1~5wt% of silica flour samplings, obtain compound, wherein 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 testing performance index of anti-gas-leak well cementation test block：It is real that the dilatant slurry for taking second step to make pours into gas leakage simulation
In experiment device, gas leakage analogue experiment installation includes support（1）, remote control electric digital display oblique angle regulator（2）, 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）Through outer tube（6）, central tube（7）Diameter has plurality of specifications, central tube（7）With outer tube（6）Between form annular space, will expand
Slurries injection wherein, other parts are arranged on support（1）On, switch board is provided with keyboard, is changed by input parameter and watched
The corner of motor is taken, and then changes 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, drop dehydration influence of the quantity to gas leakage,
Influence of the density of slurries to gas leakage, influence of the slurries weightlessness to gas leakage, uses compression pump（11）From pressurization hole（10）Pressurization, pressure measurement
Hole（9）Access digital pressure sensor（12）, the slurries static pressure that annular space expands is measured, simulates the pressure value of different depth, mistake
Filter screen（5）The quantity of leak-off hole metering drop dehydration is provided with, drop dehydration enters beaker（4）In, single-factor measures density, inclined respectively
The influence of oblique angle, pressure to drop dehydration, the influence of multiple-factor density, inclination angle, force combination measurement to drop dehydration, drop dehydration are more
It is few directly related with gas leakage, and measured value is recorded, 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 modified closed pore hollow silicon zircon ceramic fine bead, the slurries of expansion, drop
The density of low slurries, the weightlessness of slurries is avoided, reduce the pressure in shaft bottom, spawn, cement are generated in hydration process
The basal body structure hole of slurry diminishes, and forms high vapour lock well cementation test block, reduces the permeability of well cementation test block, improve well cementation test block
Flow of pore resistance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711168608.5A CN107870110A (en) | 2017-11-21 | 2017-11-21 | Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711168608.5A CN107870110A (en) | 2017-11-21 | 2017-11-21 | Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107870110A true CN107870110A (en) | 2018-04-03 |
Family
ID=61754372
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711168608.5A Pending CN107870110A (en) | 2017-11-21 | 2017-11-21 | Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107870110A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111537418A (en) * | 2020-04-27 | 2020-08-14 | 哈尔滨工业大学 | Method for evaluating grouting performance of cement asphalt composite concrete cementing material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592694A (en) * | 2015-01-04 | 2015-05-06 | 和县科嘉阀门铸造有限公司 | Nano calcium carbonate modified polytetrafluoroethylene composite material for sealing valve |
-
2017
- 2017-11-21 CN CN201711168608.5A patent/CN107870110A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592694A (en) * | 2015-01-04 | 2015-05-06 | 和县科嘉阀门铸造有限公司 | Nano calcium carbonate modified polytetrafluoroethylene composite material for sealing valve |
Non-Patent Citations (2)
| Title |
|---|
| 李红梅 等: "机械发泡式低密度泡沫水泥浆的实验研究", 《钻采工艺》 * |
| 郭胜来 等: "考虑失水影响的固井水泥浆失重模拟实验装置设计", 《实验室研究与探索》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111537418A (en) * | 2020-04-27 | 2020-08-14 | 哈尔滨工业大学 | Method for evaluating grouting performance of cement asphalt composite concrete cementing material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100500794C (en) | Gas channeling preventing cement slurry for cementing oil field | |
| CN102060460B (en) | Inorganic cement capillary crystalline waterproofing agent and production process thereof | |
| CN108008121A (en) | Silicon vanadine ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block | |
| CN103224772A (en) | Well cementation cement slurry, preparation method and application thereof | |
| CN102010166A (en) | Method for preparing micro expanded inorganic heat insulation mortar | |
| CN107860895A (en) | Sial terracotta ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak | |
| CN110407528A (en) | A kind of mixing cured soil body road basement material of steel slag | |
| CN108007736A (en) | Ferronickel alumina porcelain microballon prepares oil well anti-gas-leak well cementation test block performance test methods | |
| CN107870110A (en) | Silicon zircon ceramic fine bead prepares the performance test methods of oil well anti-gas-leak well cementation test block | |
| CN103184044A (en) | Thermo-sensitive sand consolidation, channeling sealing and well completion integrated chemical system used for steam injection for thermal recovery | |
| CN108037272A (en) | Aluminium ore soil ceramic fine bead prepares the test method of oil well anti-gas-leak well cementation test block performance | |
| CN107870109A (en) | Sial husky ginger soil ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak | |
| CN108007746A (en) | Zircon English ceramic fine bead prepares the performance test of oil well anti-gas-leak well cementation test block | |
| CN107860896A (en) | Silicon-aluminum bentonite ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak | |
| CN108037273A (en) | Sial white bind ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak | |
| CN108037271A (en) | Sial brunisolic soil ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak | |
| CN107807230A (en) | Carborundum kaolin ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak | |
| CN108007740A (en) | Silicon aluminum boron sand ceramic fine bead prepares the performance test of oil well anti-gas-leak well cementation test block | |
| CN108051571A (en) | Zirconium kaolin ceramic fine bead prepares oil well anti-gas-leak well cementation test block performance test methods | |
| CN107976532A (en) | Aluminium wollastonite ceramics microballon prepares the performance test of oil well anti-gas-leak well cementation test block | |
| CN107884554A (en) | Silicon kaolin ceramic fine bead prepares oil well anti-gas-leak well cementation test block performance test methods | |
| CN107884553A (en) | Sial alumina porcelain microballon prepares the method for testing of oil well anti-gas-leak well cementation test block | |
| CN107860900A (en) | Mica kaolin ceramic fine bead prepares oil well anti-gas-leak well cementation test block performance test methods | |
| CN108007737A (en) | Sial red soil ceramic fine bead prepares the well cementation test block performance test of oil well anti-gas-leak | |
| CN107860899A (en) | Modified silicon aluminum ceramic microspheres prepare the well cementation test block of oil well anti-gas-leak and performance test |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180403 |
|
| WD01 | Invention patent application deemed withdrawn after publication |