CN107860904A - Heat-resistance type ceramic fibre lead-zinc ore prepares oil well antiseepage well cementation test block performance test - Google Patents

Heat-resistance type ceramic fibre lead-zinc ore prepares oil well antiseepage well cementation test block performance test Download PDF

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CN107860904A
CN107860904A CN201711168586.2A CN201711168586A CN107860904A CN 107860904 A CN107860904 A CN 107860904A CN 201711168586 A CN201711168586 A CN 201711168586A CN 107860904 A CN107860904 A CN 107860904A
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test block
slurries
well
compound
antiseepage
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冯青
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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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/02Agglomerated materials, e.g. artificial aggregates
    • C04B18/027Lightweight materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

The present invention provides a kind of heat-resistance type ceramic fibre lead-zinc ore and prepares oil well antiseepage well cementation test block performance test, comprises the following steps:The dispensing of antiseepage well cementation test block:By 40~50wt% of G level oil-well cements, 10~15wt% of superfine cement, particle diameter is 50~350 μm of 25~35wt% of lead-zinc ore 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%, ceramic fibre is proportionally added into again, graphite microbeads and swollen resin, stir, carry out barrier performance test.

Description

Heat-resistance type ceramic fibre lead-zinc ore prepares oil well antiseepage well cementation test block performance test
Technical field
The present invention relates to heat-resistance type ceramic fibre lead-zinc ore 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 lead-zinc ore 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:
Heat-resistance type ceramic fibre lead-zinc ore prepares oil well antiseepage well cementation test block performance test, comprises the following steps:
The first step:The preparation of lead-zinc ore closed pore hollow ceramic microspheres:Lead-zinc ore is first broken into 1000 by jaw crusher ~1500 μm of little particle, then 20~100 μm of spheroidal full particles are made by Raymond mill, spheroidal full particle passes through Elevator 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 tables Face melting is fired, cooling, and the hollow pottery of lead-zinc ore closed pore of 50~100 μm of wall thickness, 50~350 μm of particle diameter is obtained through pneumatic separating Porcelain microballon.
Second step, the dispensing of antiseepage well cementation test block:By 40~50wt% of G level oil-well cements, 10~15wt% of superfine cement, grain Footpath is 50~350 μm of footpath, 25~35wt% of lead-zinc ore closed pore hollow ceramic microspheres, 5~7wt% of flyash, pure of loss on ignition 1.1% 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 spent, Obtain compound, the percentage by weight sum of above component is 100%, and activated silica, aluminium and G level oil-well cements react generation Hydrated calcium silicate gel shape material and other gels, the basal body structure hole of cement mortar diminish, and form high vapour lock well cementation test block, drop The permeability of low well cementation test block, improves the flow of pore resistance of well cementation test block, improves test block heat resistance, calcium oxide aquation The substantial amounts of heat of reaction release, improves the temperature of test block, and silica flour and alumina powder G level oil-well cements react and generate aquation silicic acid Calcium 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 The permeability of test 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, antiseepage well cementation test block heatproof slurries:Compound is mixed to get by the percentage by weight sampling of second step, 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% foaming agent, foaming agent are one kind therein in aluminium powder cream, the compound of aluminium or ammonium hydrogen carbonate, add hair Infusion hydration reaction generates bubble, forms the slurries of expansion, reduces the density of slurries, forms high vapour lock well cementation test block, reduces Cement the well test block permeability, improve well cementation test block flow of pore resistance, with well cementation depth increase, 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 ceramic fibre that compound gross weight is 5~8% will be added in the slurries of preparation, by roller rotary spreading, realization is uniformly stirred Mix, 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 vibrations, adds the slurries of ceramic fibre, the increase of test block crushing resistance, fold resistance enhancing after grout cures;
4th step, antiseepage well cementation test block mobility slurries preparation, will the 3rd step prepare slurries in add after nodularization grain Footpath is 20~50 μm of graphite microbeads, and addition is 1~3% graphite microbeads of second step compound weight, then adds second The swollen resin of 0.5~1.0% water imbibition of compound weight is walked, is stirred, increases the mobility of slurries, after grout cures Test block shock resistance, toughness enhancing, swollen resin water suction test block shrinkage factor it is low, reduce test block drop dehydration quantity, slurries Density is 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, barrier performance is tested:The slurries for taking the 4th step to prepare are poured into water-impervious analogue experiment installation, water-impervious simulated experiment Device includes base, central tube, outer tube, top cover labyrinth, lower sealing cover, well-illuminated glass, special high-pressure pressurized equipment, center Pipe runs through outer tube, and center pipe diameter has a plurality of specifications, and between 10~200 centimetres of internal diameter, annular space is formed between central tube and outer tube, By the slurries injection of expansion wherein, central tube and outer tube are respectively equipped with micropore, screen pack are provided with outer tube, top cover labyrinth is with Closure is made up of central tube and the outer seal of tube, special high-pressure pressurized equipment high-pressure pump, pressurized tank and button, mould as needed Intend oil well depth, set the value of digital pressure gauge, from the pressurization of pressurization hole, pressurization scope opens shift knob from 10~350MPa, Gases at high pressure enter central tube interior sealing intracavitary through piping, and when reaching the value of digital pressure gauge setting, constant pressure is seen after 30 minutes The quantity that dehydration is oozed in well-illuminated glass is examined, drops the scope of fluid loss in 10~50mL/30min, the quantity for dropping dehydration is weighing apparatus Measure the most important performance indications of water-impervious.
Containing lead, zinc, sulphur, fluorine, chlorine element and silica, oxidation ferriferous oxide in lead lead-zinc ore, ceramic fibre is one Kind of fibrous light refractory material, have good in light weight, high temperature resistant, heat endurance, low thermal conductivity, specific heat capacity small and mechanical resistant shake Dynamic, the increase of test block crushing resistance, fold resistance enhancing after grout cures, activated silica, aluminium and G improve well cementation test block heat-resisting ability.
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 barrier performance test of the embodiment of the present invention.
1, base 2, lower sealing cover 3, well-illuminated glass 4, screen pack 5, outer tube 6, center wherein in figure Pipe 7, digital pressure gauge 8, top cover labyrinth 9, pressurized tank.
Embodiment
Embodiment 1.
Heat-resistance type ceramic fibre lead-zinc ore prepares oil well antiseepage well cementation test block performance test, comprises the following steps:
The first step:The preparation of lead-zinc ore closed pore hollow ceramic microspheres:Lead-zinc ore is first broken into 1000 by jaw crusher μm little particle, then 70 μm of spheroidal full particles are made by Raymond mill, spheroidal full particle enters cloth by elevator Glassware, then entered by distributing device in expansion furnace, by 800 DEG C of expansions, 1220 DEG C of firings, cooling, form 80 μm of wall thickness, particle diameter 250 μm of lead-zinc ore closed pore hollow ceramic microspheres.
Second step, the dispensing of antiseepage well cementation test block:It is 250 μ by G level oil-well cements 43wt%, superfine cement 15wt%, particle diameter M lead-zinc ore closed pore hollow ceramic microspheres 25wt%, 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, antiseepage well cementation test block heatproof slurries:Compound is mixed to get by the percentage by weight sampling of second step, Compound is stirred, sized mixing with 0.5 ratio of mud, wherein ash is compound, it is 0.2% to add compound gross weight Foaming agent, foaming agent are ammonium hydrogen carbonate, add hydration reaction generation bubble after ammonium hydrogen carbonate, form the slurries of expansion, reduce slurry The density of liquid, high vapour lock well cementation test block is formed, 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 ceramic fibre, ceramic fibre that compound gross weight is 8% will be added in the slurries of preparation Or one kind in polyester fiber, by roller rotary spreading, uniform stirring is realized, adds the slurries of ceramic fibre, grout cures The increase of test block toughness, anti-folding, pull resistance enhancing afterwards;
4th step, antiseepage well cementation test block mobility slurries preparation, will the 3rd step prepare slurries in add after nodularization grain Footpath is 15 μm of graphite solid microbeads, and addition is 2% graphite solid microbeads of second step compound weight, adds second step The swollen resin of 1.0% water imbibition of compound weight, stirs, and increases the mobility of slurries, and the test block after grout cures resists Impact enhancing, swollen resin water suction reduce 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, 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, 40 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 150MPa, 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 15mL/30min.

Claims (1)

1. heat-resistance type ceramic fibre lead-zinc ore 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 50~350 μm of 25~35wt% of lead-zinc ore 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 lead-zinc ore closed pore hollow ceramic microspheres:First by lead Zinc ore is broken into 1000~1500 μm of little particle by jaw crusher, then 20~100 μm of spheroidals are made by Raymond mill Full particle, spheroidal full particle enters distributing device by elevator, then is entered by distributing device in expansion sintering furnace, passes through 800~950 DEG C of expansions, 1000~1500 DEG C of melt surfaces are fired, cooling, and 50~100 μm of wall thickness, particle diameter are obtained through pneumatic separating 50~350 μm of lead-zinc ore closed pore hollow ceramic microspheres;
The preparation of second step, antiseepage well cementation test block heatproof slurries:Compound is mixed to get by the percentage by weight sampling of the first step, Compound is stirred, sized mixing with 0.5~0.7 ratio of mud, ash is compound, add compound gross weight for 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, antiseepage well cementation test block expansion resistance to compression slurries:Will second step prepare slurries in add gross weight be 5~ 8% ceramic fibre, by roller rotary spreading, uniform stirring is realized, add the slurries of ceramic fibre, the examination after grout cures Block high mechanical strength, fold resistance enhancing;
The preparation of 4th step, antiseepage well cementation test block mobility slurries:The grain after nodularization is added in slurries prepared by the 3rd step Footpath is 20~50 μm of graphite microbeads, and addition is 1~3% graphite microbeads of first step compound weight, then adds first The swollen resin of 0.5~1.0% water imbibition of compound weight is walked, is stirred, increases the mobility of slurries, after grout cures Test block crushing resistance increase, fold resistance enhancing, swollen resin water suction reduce test block drop dehydration quantity;
5th step, barrier performance test:The slurries for taking the 4th step to prepare are poured into water-impervious analogue experiment installation, antiseepage Fluid Dynamics Experimental provision 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.
CN201711168586.2A 2017-11-21 2017-11-21 Heat-resistance type ceramic fibre lead-zinc ore prepares oil well antiseepage well cementation test block performance test Pending CN107860904A (en)

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CN117169039A (en) * 2023-11-02 2023-12-05 江苏信尚机械制造有限公司 Wear-resistant steel product wear-resistant testing device and method
CN117169039B (en) * 2023-11-02 2024-04-05 江苏信尚机械制造有限公司 Wear-resistant steel product wear-resistant testing device and method

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