CN107748248A - Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious - Google Patents

Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious Download PDF

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CN107748248A
CN107748248A CN201711167569.7A CN201711167569A CN107748248A CN 107748248 A CN107748248 A CN 107748248A CN 201711167569 A CN201711167569 A CN 201711167569A CN 107748248 A CN107748248 A CN 107748248A
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test block
impervious
slurries
water
well
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王金萍
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Zibo Vocational Institute
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/38Concrete; Lime; Mortar; Gypsum; Bricks; Ceramics; Glass
    • G01N33/383Concrete or cement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples

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Abstract

The present invention provides a kind of Anti-pressure glass fibre vermiculite and prepares the well cementation test block performance test of oil well water-impervious, 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 50~200 μm of 25~35wt% of vermiculite 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%, the ratio of mud that obtained compound is equipped with to 0.5~0.7 is sized mixing slurries is made, add the foaming agent that compound gross weight is 0.2~0.5%, glass fibre is proportionally added into again, graphite microbeads and swollen resin, stir, carry out water-impervious performance test.

Description

Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious
Technical field
The present invention relates to Anti-pressure glass fibre vermiculite to prepare the well cementation test block performance test of oil well water-impervious, belongs to material skill Art 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, resistance to compression, anti-impact force are poor, dehydration is largely dropped, causes blind hole.
The content of the invention
Using vermiculite material as palliative, add silica flour and alumina powder, improve the resistance to compression of well cementation test block, resistance to compression, High temperature resistant, corrosion resistant performance, add foaming agent in cement mortar, form the slurries of expansion, reduce the density of slurries, reduce The pressure in shaft bottom, the slurries added in glass fibre, test block toughness, resistance to compression 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:
Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious, comprises the following steps:
The first step:The preparation of vermiculite closed pore hollow ceramic microspheres:Vermiculite is first broken into 1000~1500 μm by jaw crusher Little particle, then 20~100 μm of spherical granules are made by Raymond mill, spherical granules enter distributing device by elevator, Entered again by distributing device in expansion sintering furnace, fired by 800~950 DEG C of expansions, 1000~1500 DEG C of melt surfaces, cooling, warp Pneumatic separating forms 50~100 μm of wall thickness, the vermiculite closed pore hollow ceramic microspheres of 50~200 μm of particle diameter.
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 50~200 μm of 25~35wt% of vermiculite 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, the sampling of silica flour 1~5wt% and 1.0~2wt% alumina powder, 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 heat resistance, 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 compressive resistance;
The preparation of 3rd step, water-impervious well cementation test block toughness reinforcing resistance to compression slurries:It is mixed to get by the percentage by weight sampling of second step Compound, compound is stirred, sized mixing with 0.5~0.7 ratio of mud, wherein ash is compound, it is total to add compound Weight is 0.2~0.5% foaming agent, and foaming agent is one kind therein in aluminium powder cream, the compound of aluminium or ammonium hydrogen carbonate, Foaming agent hydration reaction generation bubble is added, forms the slurries of expansion, reduces the density of slurries, forms high vapour lock well cementation test block, The permeability of well cementation test block is reduced, improves the flow of pore resistance of well cementation test block, with the increase of well cementation depth, high density Slurries, 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 glass fibre that compound gross weight is 5~8% will be added in the slurries of preparation, by roller rotary spreading, realized equal Even stirring, adds the slurries of glass fibre, test block test block high mechanical strength, crushing resistance enhancing after grout cures;
4th step, water-impervious well cementation test block shock resistance slurries 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 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 bottom in well-illuminated glass is observed, the scope of fluid loss is dropped in 10~50mL/30min, drops dehydration Quantity is to weigh the most important performance indications of water-impervious.
The main component of vermiculite is silica, aluminum oxide, iron oxide and magnesia, calcium oxide hydration reaction, is produced a large amount of Heat, generation calcium hydroxide is in as a form of gel, and silica, aluminum oxide generation calcium silicates, and calcium oxide is activator, excited cement Activity, flyash is strong water absorbent, by high temperature sintering, there is higher activity, adds the slurries of glass fibre, grout cures Test block high mechanical strength afterwards, crushing resistance enhancing;
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, glass fibre has that heat resistance is strong, corrosion resistance is good, high mechanical strength, after adding the grout cures of glass fibre The enhancing of test block crushing resistance, toughness increase, resistance to compression, 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.
Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious, comprises the following steps:
The first step:The preparation of vermiculite closed pore hollow ceramic microspheres:Vermiculite is first broken into 1000 μm small by jaw crusher Particle, then 50 μm of spherical granules are made by Raymond mill, spherical granules enter distributing device by elevator, then by distributing device Into in expansion furnace, fired by 800 DEG C of expansions, 1200 DEG C of melt surfaces, cooling, form 80 μm of wall thickness, the leech of 150 μm of particle diameter Stone closed pore hollow ceramic microspheres.
Second step, the dispensing of water-impervious well cementation test block:It is by G level oil-well cements 40wt%, superfine cement 15wt%, particle diameter 150 μm of vermiculite closed pore hollow ceramic microspheres 28wt%, the flyash 7wt% of loss on ignition 1.1%, the calcium oxide 2wt% of purity 99.9%, sulphur Sour sodium 1.0wt%, silica flour 5wt% and alumina powder 2wt% samplings, obtain compound, the percentage by weight sum of above component is 100%, activated silica, aluminium and G level oil-well cements, which react, generates hydrated calcium silicate gel shape material and other gels, cement mortar Basal body structure hole diminish, form the well cementation test block of high vapour lock, reduce the permeability of well cementation test block, improve well cementation test block Flow of pore resistance, improve test block heat resistance;
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 aluminium powder cream, adds hydration reaction generation bubble after aluminium powder cream, forms the slurries of expansion, reduce slurries Density, form the well cementation test block of high vapour lock, reduce the permeability of well cementation test block, improve the flow of pore resistance of well cementation test block Power, with well cementation depth increase, the bottom of test block pressure increase, easily cause oil well cementing test block weightlessness collapse, cross-sectional layers Fracture, cause oil well infiltration, landslide;The preparation of water-impervious well cementation test block resistance to compression slurries:Compound will be added in the slurries of preparation Gross weight is 8% glass fibre, by roller rotary spreading, realizes uniform stirring, adds the slurries of glass fibre, slurries coagulate Test block high mechanical strength, crushing resistance enhancing after Gu;
4th step, water-impervious well cementation test block mobility slurries preparation, will the 3rd step prepare slurries in add after nodularization Particle diameter is 25 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 1.0g/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, and slurries are not stratified, Test block vertical section Density Distribution after solidification is uniform, i.e. homogeneity;
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, 50 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 200MPa, 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 20mL/30min.

Claims (1)

1. Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious, 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 50~200 μm of 25~35wt% of vermiculite 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 mixed Material, the percentage by weight sum of above component is 100%, the preparation of vermiculite closed pore hollow ceramic microspheres:First vermiculite is broken by jaw 20~100 μm of spherical granules, spheroidal is made into 1000~1500 μm of little particle, then by Raymond mill in broken crusher machine Grain enters distributing device by elevator, then is entered by distributing device in expansion sintering furnace, 1000 are expanded by 800~950 DEG C~ 1500 DEG C of melt surfaces are fired, cooling, and the vermiculite closed pore sky of 50~100 μm of wall thickness, 50~200 μm of particle diameter is formed through pneumatic separating Heart ceramic fine bead;
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:Compound gross weight is added in slurries prepared by second step For 5~8% glass fibre, by roller rotary spreading, uniform stirring is realized, adds the slurries of glass fibre, after grout cures Test block high mechanical strength, crushing resistance enhancing;
4th step, water-impervious well cementation test block shock resistance slurries 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 Test block shock 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.
CN201711167569.7A 2017-11-21 2017-11-21 Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious Pending CN107748248A (en)

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Application publication date: 20180302