CN107807027A - High air-resistance type ceramic fibre gold mine slag prepares oil well antiseepage well cementation test block performance test - Google Patents
High air-resistance type ceramic fibre gold mine slag prepares oil well antiseepage well cementation test block performance test Download PDFInfo
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- CN107807027A CN107807027A CN201711168554.2A CN201711168554A CN107807027A CN 107807027 A CN107807027 A CN 107807027A CN 201711168554 A CN201711168554 A CN 201711168554A CN 107807027 A CN107807027 A CN 107807027A
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- 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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
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Abstract
The present invention provides a kind of high air-resistance type ceramic fibre gold mine slag and prepares oil well antiseepage well cementation test block performance test, comprises the following steps：The dispensing of water-impervious well cementation test block：By 40~50wt% of G level oil-well cements, 10~15wt% of superfine cement, particle diameter is 50~250 μm of 25~35wt% of gold mine slag closed pore hollow ceramic microspheres, 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, 1~5wt% of silica flour and 1.0~2wt% of alumina powder samplings, obtain compound, the percentage by weight sum of above component is 100%, compound will be obtained it is equipped with 0.5~0.7 ratio of mud sizing mixing slurries are made, add the foaming agent that compound gross weight is 0.2~0.5%, ceramic fibre is proportionally added into again, graphite microbeads and swollen resin, stir, carry out water-impervious performance test.
Description
Technical field
The present invention relates to high air-resistance type ceramic fibre gold mine slag to prepare oil well antiseepage well cementation test block performance test, belongs to material
Technology is led.
Background technology
At present, both at home and abroad in oil well cementing, cement mortar is used for HTHP oil well, but uses fly ash float,
Compression strength is low, and cement slurry density rate of change is big, and after the static solidification of cement mortar, appearance drop dehydration is excessive, test block shrinkage ratio mistake
Greatly, in addition, the poor toughness of test block, tension, anti-folding, anti-impact force are poor, dehydration is largely dropped, causes blind hole.
The content of the invention
Using gold mine residue material as palliative, silica flour and alumina powder are added, the resistance to compression of well cementation test block is improved, resists
Folding, high temperature resistant, corrosion resistant performance, add foaming agent in cement mortar, form the slurries of expansion, reduce the density of slurries, drop
The low pressure in shaft bottom, adds ceramic fibre slurries, test block toughness, anti-folding increase after grout cures, add graphite microbeads and
The swollen resin of water imbibition, increases the mobility of slurries, and the test block shock resistance enhancing after grout cures, swollen resin water suction reduces
Test block drop dehydration quantity, generates spawn, the basal body structure hole of cement mortar diminishes, and forms high gas in hydration process
Resistance well cementation test block, the permeability of well cementation test block is reduced, improve the flow of pore resistance of well cementation test block.
Its technical scheme is：
High air-resistance type ceramic fibre gold mine slag prepares oil well antiseepage well cementation test block performance test, comprises the following steps：
The first step：The preparation of gold mine slag closed pore hollow ceramic microspheres：Gold mine slag is first broken into 1000 by jaw crusher~
1500 μm of little particle, then 50~100 μm of spheroidal full particles are made by Raymond mill, spheroidal full particle is by carrying
The machine of liter enters distributing device, then is entered by distributing device in expansion sintering furnace, by 800~950 DEG C of expansions, 1000~1500 DEG C of surfaces
Melting is fired, cooling, and the gold mine slag closed pore hollow ceramic through 50~100 μm of wall thickness of pneumatic separating formation, 50~250 μm of particle diameter is micro-
Pearl.
Second step, the dispensing of water-impervious well cementation test block：By 40~50wt% of G level oil-well cements, 10~15wt% of superfine cement,
Particle diameter is 50~250 μm of 25~35wt% of gold mine slag closed pore hollow ceramic microspheres, 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, 1~5wt% of silica flour and 1.0~2wt% of alumina powder samplings, are obtained
To compound, the percentage by weight sum of above component is 100%, and activated silica, aluminium and G level oil-well cements, which react, generates water
Change calcium silicates spawn and other gels, the basal body structure hole of cement mortar diminish, form high vapour lock well cementation test block, reduce
The permeability of well cementation test block, the flow of pore resistance of well cementation test block is improved, improves test block expansion character, calcium oxide aquation is anti-
Substantial amounts of heat should be discharged, improves the temperature of test block, silica flour and alumina powder G level oil-well cements, which react, generates hydrated calcium silicate
Spawn and other gels, the basal body structure hole of cement mortar diminish, and form high vapour lock well cementation test block, reduce well cementation examination
The permeability of block, the flow of pore resistance of well cementation test block is improved, strengthen test block resistance to compression and fracture resistence force；
The preparation of 3rd step, water-impervious well cementation test block dilatant slurry：Mixing is mixed to get by the percentage by weight sampling of second 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% foaming agent, foaming agent is one kind therein in aluminium powder cream, the compound of aluminium or ammonium hydrogen carbonate, is added
Foaming agent hydration reaction generates bubble, forms the slurries of expansion, reduces the density of slurries, forms high vapour lock well cementation test block, reduces
The permeability of well cementation test block, the flow of pore resistance of well cementation test block is improved, with the increase of well cementation depth, high density slurry
Liquid, the bottom of test block pressure increase, easily cause oil well cementing test block weightlessness collapse, section fault rupture, cause oil well infiltration, collapse
Side；The ceramic fibre that compound gross weight is 5~8% will be added in the slurries of preparation, by roller rotary spreading, realized uniform
Stirring, ceramic fibre is a kind of fibrous light refractory material, have good in light weight, high temperature resistant, heat endurance, low thermal conductivity,
Specific heat capacity is small and mechanical resistant vibrations, adds the slurries of ceramic fibre, and the increase of test block crushing resistance, fold resistance after grout cures increase
By force；
The preparation of 4th step, the water-impervious well cementation high vapour lock slurries of test block：Added in slurries prepared by the 3rd step after nodularization
Particle diameter is 20~50 μm of graphite microbeads, and addition is 1~3% graphite microbeads of second step compound weight, then adds the
The swollen resin of 0.5~1.0% water imbibition of two step compound weight, stirs, increases the mobility of slurries, grout cures
Test block shock resistance, toughness enhancing afterwards, the shrinkage factor of swollen resin water suction test block is low, reduces test block drop dehydration quantity, slurries
Density in 0.8~1.2g/cm3；
5th step, testing performance index：
A, the measure of expansion slurry flow rate：Take the 4th step to prepare slurries, pour into slurries flowing speedometer, observe and record slurry
The distance of motion in the flow rate of liquid, i.e. unit interval；
B, the volume density rate of change experiment of test block：4th 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 volume density rate of change experiment that test block is carried out on forcing press, test block
Volume density rate of change is less than 0.02%, and the porosity of test block is low, and permeability is poor；
C, the bleed experiment of test block：The slurries prepared are poured into die trial, die trial is suspended among beaker, beaker mouth hermetic bag
Sealing, slurries take out die trial after test block is frozen into from beaker, weigh the weight that moisture is separated out in beaker, observe slurry
Condition, if layering, i.e., homogeneity, the test block vertical section Density Distribution after solidification are uniform；
D, water-impervious performance test：The slurries for taking the 4th step to prepare are poured into water-impervious analogue experiment installation, and antiseepage Fluid Dynamics are real
Experiment device includes base, central tube, outer tube, top cover labyrinth, lower sealing cover, well-illuminated glass, special high-pressure pressurized equipment, in
Heart pipe runs through outer tube, and center pipe diameter has a plurality of specifications, and between 10~200 centimetres of internal diameter, ring is formed between central tube and outer tube
Sky, by the slurries injection of expansion wherein, central tube and outer tube are respectively equipped with micropore, and screen pack, top cover labyrinth are provided with outer tube
With lower sealing cover by central tube and the outer seal of tube, special high-pressure pressurized equipment is made up of high-pressure pump, pressurized tank and button, according to need
Simulation oil well depth is wanted, sets the value of digital pressure gauge, from the pressurization of pressurization hole, pressurization scope opens switch from 10~350MPa
Button, gases at high pressure enter central tube interior sealing intracavitary through piping, when reaching the value of digital pressure gauge setting, constant pressure 30 minutes
Afterwards, the quantity that dehydration is oozed in well-illuminated glass is observed, drops the scope of fluid loss in 10~50mL/30min, drops the quantity of dehydration
It is the most important performance indications for weighing water-impervious.
Gold mine slag main component is silica and aluminum oxide, has high intensity, corrosion-resistant, high temperature resistant, oxidation resistant property
Can, ceramic fibre is a kind of fibrous light refractory material, has good in light weight, high temperature resistant, heat endurance, low thermal conductivity, ratio
Thermal capacitance is small and mechanical resistant shakes, the increase of test block crushing resistance, fold resistance enhancing after grout cures.
The present invention has advantages below.
1st, using the slurries of expansion, the density of slurries is reduced, so as to reduce the pressure in shaft bottom.
2nd, ceramic fibre is a kind of fibrous light refractory material, has that in light weight, high temperature resistant, heat endurance be good, heat conduction
Rate is low, specific heat capacity is small and mechanical resistant vibrations, add the test block fold resistance after the grout cures of ceramic fibre enhancing, toughness increase,
Anti- folding, pull resistance enhancing.
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 water-impervious performance test of the embodiment of the present invention.
1, base 2 wherein in figure, lower sealing cover 3, well-illuminated glass 4, screen pack 5, outer tube 6, central tube 7,
Digital pressure gauge 8, top cover labyrinth 9, pressurized tank.
Embodiment
Embodiment 1.
High air-resistance type ceramic fibre gold mine slag prepares oil well antiseepage well cementation test block performance test, comprises the following steps：
The first step：The preparation of gold mine slag closed pore hollow ceramic microspheres：Gold mine slag is first broken into 1000 μm by jaw crusher
Little particle, then 100 μm of spheroidal full particles are made by Raymond mill, spheroidal full particle enters cloth by elevator
Device, then entered by distributing device in expansion furnace, by 800 DEG C of expansions, 1200 DEG C of firings, cooling, 80 μm of wall thickness is formed, forms particle diameter
200 μm of golden gangue minerals closed pore hollow ceramic microspheres.
Second step, the dispensing of water-impervious well cementation test block：It is by G level oil-well cements 43wt%, superfine cement 15wt%, particle diameter
200 μm of golden gangue minerals closed pore hollow ceramic microspheres 25wt%, the flyash 7wt% of loss on ignition 1.1%, the calcium oxide of purity 99.9%
2wt%, sodium sulphate 1.0wt%, silica flour 5wt% and alumina powder 2wt% samplings, obtain compound, the percentage by weight of above component
Sum is 100%, and activated silica, aluminium and G level oil-well cements, which react, generates hydrated calcium silicate gel shape material and other gels,
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 well cementation
The flow of pore resistance of test block, improve test block expansion character；
The preparation of 3rd step, water-impervious well cementation test block dilatant slurry：Mixing is mixed to get by the percentage by weight sampling of second step
Material, compound is stirred, sized mixing with 0.5 ratio of mud, wherein ash is compound, adds compound gross weight as 0.2%
Foaming agent, foaming agent is ammonium hydrogen carbonate, adds hydration reaction generation bubble after ammonium hydrogen carbonate, forms the slurries of expansion, reduce
The density of slurries, high vapour lock well cementation test block is formed, reduce the permeability of well cementation test block, improve the flow of pore of well cementation test block
Resistance, with well cementation depth increase, the bottom of test block pressure increase, easily cause oil well cementing test block weightlessness collapse, section
Fault rupture, cause oil well infiltration, landslide, the preparation of the water-impervious well cementation high vapour lock slurries of test block：It is mixed by being added in the slurries of preparation
The ceramic fibre that material gross weight is 8% is closed, by roller rotary spreading, uniform stirring is realized, adds the slurries of ceramic fibre, starch
The increase of test block toughness, anti-folding, pull resistance enhancing after liquid solidification；
4th step, water-impervious well cementation test block mobility slurries preparation, will the 3rd step prepare slurries in add after nodularization
Particle diameter is 15 μm of graphite solid microbeads, and addition is 2% graphite solid microbeads of second step compound weight, adds second
The swollen resin of 1.0% water imbibition of compound weight is walked, is stirred, increases the mobility of slurries, the test block after grout cures
Shock resistance strengthens, and swollen resin water suction reduces test block drop dehydration quantity, and the density of slurries is in 1.1g/cm3；
5th step, testing performance index：
A, the measure of expansion slurry flow rate：Take the 4th step to prepare slurries, pour into slurries flowing speedometer, observe and record slurry
The flow rate of liquid, the distance of motion in the unit interval；
B, the volume density rate of change experiment of test block：4th 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 volume density rate of change experiment that test block is carried out on forcing press, test block
Volume density rate of change is less than 0.02%, and the porosity of test block is low, and permeability is poor；
C, the bleed experiment of test block：The slurries prepared are poured into die trial, die trial is suspended among beaker, beaker mouth hermetic bag
Sealing, slurries take out die trial after test block is frozen into from beaker, weigh the weight that moisture is separated out in beaker, slurries are not stratified,
It is uniform without the test block vertical section Density Distribution after bleed, solidification；
D, water-impervious performance test：The slurries for taking the 4th step to prepare are poured into water-impervious analogue experiment installation, and antiseepage Fluid Dynamics are real
Experiment device includes base 1, central tube 6, outer tube 5, top cover labyrinth 8, lower sealing cover 2, well-illuminated glass 3, special high-pressure pressurization
Equipment, central tube 6 run through outer tube 5, and the diameter of central tube 6 has plurality of specifications, 55 centimetres of internal diameter, formed between central tube 6 and outer tube 5
Annular space, the slurries of expansion being injected into annular space, central tube 6 and outer tube 5 are respectively equipped with micropore, screen pack 4 are provided with outer tube 5, on
Closure 8 and lower sealing cover 2 seal central tube 6 and outer tube 5, and special high-pressure pressurized equipment is by high-pressure pump, pressurized tank 9 and button
Composition, simulation oil well depth as needed, the value of digital pressure gauge 7 is adjusted, from the pressurization of pressurization hole, pressurizeed 250MPa, and opening is opened
Button is closed, gases at high pressure enter the interior sealing intracavitary of central tube 6 through piping, observed after 30 minutes in well-illuminated glass 3 and ooze mistake
The quantity of water, fluid loss scope is in 25mL/30min.
Claims (1)
1. high air-resistance type ceramic fibre gold mine slag prepares oil well antiseepage well cementation test block performance test, comprise the following steps：
The first step, the dispensing of water-impervious 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 gold mine slag closed pore hollow ceramic microspheres, 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, 1~5wt% of silica flour and 1.0~2wt% of alumina powder samplings, are obtained
To compound, the percentage by weight sum of above component is 100%, the preparation of gold mine slag closed pore hollow ceramic microspheres：First by gold mine
Slag is broken into 1000~1500 μm of little particle by jaw crusher, then by Raymond mill 50~100 μm of spheroidals to be made solid
Particle, spheroidal full particle enter distributing device by elevator, then are entered by distributing device in expansion sintering furnace, by 800~
950 DEG C of expansions, 1000~1500 DEG C of melt surfaces are fired, cooling, through pneumatic separating formed 50~100 μm of wall thickness, particle diameter 50~
250 μm of gold mine slag closed pore hollow ceramic microspheres；
The preparation of second step, water-impervious 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, and ash is compound, adds compound gross weight as 0.2
~0.5% foaming agent, foaming agent hydration reaction generation bubble is added, form the slurries of expansion, reduce the density of slurries；
The preparation of 3rd step, water-impervious well cementation test block resistance to compression slurries：It is 5~8% that gross weight is added in slurries prepared by second step
Ceramic fibre, by roller rotary spreading, realize uniform stirring, add the slurries of ceramic fibre, the test block after grout cures
High mechanical strength, crushing resistance enhancing；
4th step, water-impervious well cementation the high vapour lock slurries of test block preparation, will the 3rd step prepare slurries in add after nodularization
Particle diameter is 20~50 μm of graphite microbeads, and addition is 1~3% graphite microbeads of first step compound weight, then adds the
The swollen resin of 0.5~1.0% water imbibition of one step compound weight, stirs, increases the mobility of slurries, grout cures
The increase of test block crushing resistance, fold resistance enhancing afterwards, swollen resin water suction reduce test block drop dehydration quantity；
5th step, water-impervious performance test：The slurries for taking the 4th step to prepare are poured into water-impervious analogue experiment installation, water-impervious mould
Draft experiment device includes base（1）, central tube（6）, outer tube（5）, top cover labyrinth（8）, lower sealing cover（2）, well-illuminated glass
（3）, special high-pressure pressurized equipment, central tube passes through（6）Wear outer tube（5）, central tube（6）Diameter has plurality of specifications, central tube（6）With
Outer tube（5）Between form annular space, by the injection of the slurries of expansion wherein, central tube（6）And outer tube（5）Micropore is respectively equipped with, outside
Pipe（5）It is provided with screen pack（4）, top cover labyrinth（8）And lower sealing cover（2）By central tube（6）And outer tube（5）Sealing, special height
Pressurized equipment is pressed by high-pressure pump, pressurized tank（9）With button composition, digital pressure gauge（7）Composition, simulation oil well depth as needed
Degree, set digital pressure gauge（7）Value, open shift knob, gases at high pressure enter central tube through piping（6）Annular seal space
It is interior, reach digital pressure gauge（7）During the value of setting, constant pressure observes well-illuminated glass after 30 minutes（3）In ooze the number of dehydration
Amount.
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Application publication date: 20180316 |