CN103803890B - Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette - Google Patents
Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette Download PDFInfo
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- CN103803890B CN103803890B CN201410088373.9A CN201410088373A CN103803890B CN 103803890 B CN103803890 B CN 103803890B CN 201410088373 A CN201410088373 A CN 201410088373A CN 103803890 B CN103803890 B CN 103803890B
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- 239000004568 cement Substances 0.000 title claims abstract description 103
- 239000000919 ceramic Substances 0.000 title claims abstract description 100
- 239000002131 composite material Substances 0.000 title claims abstract description 96
- 239000003129 oil well Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000004484 Briquette Substances 0.000 title description 45
- 239000002245 particle Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000012360 testing method Methods 0.000 claims abstract description 36
- 239000010881 fly ash Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 15
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000011325 microbead Substances 0.000 claims abstract description 7
- 239000004005 microsphere Substances 0.000 claims abstract 15
- 238000011056 performance test Methods 0.000 claims abstract 3
- 239000011148 porous material Substances 0.000 claims description 40
- 239000000843 powder Substances 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 17
- 230000008859 change Effects 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 11
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 10
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000292 calcium oxide Substances 0.000 claims description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000003763 carbonization Methods 0.000 claims description 7
- 239000011324 bead Substances 0.000 claims description 6
- 238000007667 floating Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 5
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 5
- 235000011151 potassium sulphates Nutrition 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 230000008719 thickening Effects 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 230000002706 hydrostatic effect Effects 0.000 claims description 4
- 229910026551 ZrC Inorganic materials 0.000 claims description 3
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229910021487 silica fume Inorganic materials 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 235000010216 calcium carbonate Nutrition 0.000 claims description 2
- 239000004088 foaming agent Substances 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 2
- 239000011863 silicon-based powder Substances 0.000 claims 2
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
- 239000011575 calcium Substances 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 19
- 239000011440 grout Substances 0.000 description 15
- 230000006835 compression Effects 0.000 description 12
- 238000007906 compression Methods 0.000 description 12
- 239000011521 glass Substances 0.000 description 12
- 235000013312 flour Nutrition 0.000 description 9
- 238000003825 pressing Methods 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 229910052726 zirconium Inorganic materials 0.000 description 8
- 238000012423 maintenance Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 238000000703 high-speed centrifugation Methods 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- 239000011083 cement mortar Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910021353 zirconium disilicide Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- PIRWNASAJNPKHT-SHZATDIYSA-N pamp Chemical compound C([C@@H](C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CCCCN)C(=O)N[C@@H](CCCCN)C(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](CC(N)=O)C(=O)N[C@@H](CCCCN)C(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](C)C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](CO)C(=O)N[C@@H](CCCNC(N)=N)C(N)=O)NC(=O)[C@H](CCC(O)=O)NC(=O)[C@H](CO)NC(=O)[C@H](C)NC(=O)[C@@H](NC(=O)[C@H](CC(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](CCCNC(N)=N)NC(=O)[C@H](C)N)C(C)C)C1=CC=CC=C1 PIRWNASAJNPKHT-SHZATDIYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 239000005354 aluminosilicate glass Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 241001212038 Arcola Species 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000010504 bond cleavage reaction Methods 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 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 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000009671 shengli Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
Landscapes
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
本发明提供陶瓷复合微珠制备低密度油井固井水泥试块的方法，包括陶瓷复合闭孔空心微珠制备、配料、混合、搅拌调浆、试模、强度试验，将G级油井水泥40～50wt%、13μm超细水泥10～15 wt%、粒径为5～50μm的陶瓷复合闭孔空心微珠25～35wt%、烧失量1.1%的粉煤灰5～7wt%、纯度99.9%氧化钙1.5～2wt%、硫酸钠0.5～1.0 wt%和微硅1～3wt%混合搅拌均匀，以0.5～0.6（W/C）的水灰比在搅拌机中搅拌调浆40秒，倒入试模，在恒温52°C的水浴养护箱中养护24小时、48小时，脱模后在凉水中浸泡1小时，进行性能测试。The invention provides a method for preparing a low-density oil well cementing cement test block with ceramic composite microbeads, which includes preparation of ceramic composite closed-cell hollow microbeads, batching, mixing, stirring and mixing, mold testing, and strength test. 50wt%, 13μm ultra-fine cement 10-15wt%, ceramic composite closed-cell hollow microspheres with a particle size of 5-50μm 25-35wt%, loss on ignition 1.1% fly ash 5-7wt%, purity 99.9% oxidation Calcium 1.5-2wt%, sodium sulfate 0.5-1.0wt%, and micro-silicon 1-3wt% are mixed and stirred evenly, and the water-cement ratio is 0.5-0.6 (W/C) in the mixer for 40 seconds, poured into the test mold , maintained in a water bath curing box with a constant temperature of 52°C for 24 hours and 48 hours, soaked in cold water for 1 hour after demoulding, and performed a performance test.
Description
Technical field
The present invention relates to the method that Ceramic Composite microballon prepares the cement briquette of low density oil well cementing, belong to field of material technology.
Background technology
Current domestic oil well cementing light-weight additive adopts the drift pearl in flyash, and comprise heavy pearl and drift pearl at flyash, heavy pearl density is at 1.1 ~ 2.8g/cm
3between, content accounts for flyash 30 ~ 70%, drift pearl is the glass microballon being less than water-mass density in flyash, drift pearl mainly comprises aluminosilicate glass microballon and porous carbon granule, drift pearl after removing carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, surfaces externally and internally is smooth, volume is large, a kind of rounded, light weight, closed pore is hollow, wear-resisting, high temperature resistant, thermal conductivity is little, intensity is high, drift pearl amount accounts for 0.5 ~ 1% of flyash total amount, aluminosilicate glass microballon is hollow spherosome, drift pearl wherein in flyash it be coal dust in thermal power plant boiler through 1100 ~ 1500 DEG C burning time, clayey material melts becomes microlayer model, in stove turbulent flow hot air acting under at a high speed spin, form perfectly round sial spheroid, the nitrogen that burning and scission reaction produce, the gas such as hydrogen and carbonic acid gas, undergoes rapid expansion in the high temperature aluminum silicon spheroid of melting, under capillary effect, form the glass envelope of hollow, then enter flue to cool rapidly, after sclerosis, become the vitreous state cenosphere of high vacuum, i.e. fly ash float, flyash is put into water stir, leave standstill for some time, because drift pearl density is less than water-mass density, to swim in the water surface pulls out and dry, be drift pearl, flyash floating bead is canescence, main component is SiO
2account for 70% and AL
2o
3account for 13%, loss on ignition is 0.40% ~ 0.574%, density 0.475 ~ 0.574g/cm
3, wall thickness 1.44 ~ 5.41 μm, particle size range is mainly distributed in 147 ~ 84 μm, but the particle diameter of drift pearl is large, and ultimate compression strength is low.
In recent years, due to the impact of northern haze weather, the big-and-middle-sized thermal power generation of China adopts the desulfurization technology of environmental protection, not containing in flyash floats pearl, cause in short supply, only has the drift pearl that middle small coal power plants and arcola do not adopt desulfurization technology supply a small amount of, drift the in short supply of pearl causes price increase, and float that pearl is impure is mixed with flyash, affect cementing quality, drift pearl price is per ton rises violently 10,000 yuan, and maximum compressive strength 20MPa, so adopt composite ceramic material making cenosphere to substitute the drift pearl of flyash, not by the restriction of envrionment conditions, economic benefit is large, market outlook are good.
In reinforcing oil well field, hydrocarbon distribution is wide, and long shut-in well is more and more, and main use of long shut-in well is light weight cement well cementation, and long shut-in well mainly adopts low-density cement mortar, wants to make the density of grout at 1.0g/cm
3~ 1.5g/cm
3between, density must at 0.5g/cm for the lightening material (inorganic mineral material and organic synthesis material composition) of non-drift pearl
3~ 0.85g/cm
3between, (density of G level oil well cement is at 3.1g/cm just to make low-density grout
3, light-weight additive density must be less than 1g/cm
3, just can configure density 1.0g/cm
3~ 1.5g/cm
3between grout, precondition is that light-weight additive addition can not exceed 40% of total amount, otherwise can affect the ultimate compression strength of cement briquette).
In patent 200910071314.X, adopt the flyash of non-drift pearl as light-weight additive, in literary composition, the pellet density of flyash is 2.0g/cm
3, cement density 3.1g/cm
3, silica flour density 2.0g/cm
3, only have the density of water to be 1.0g/cm
3, the proportional restriction of consumption of water, can not make density at 1.40 ~ 1.55g/cm
3low-density cement mortar.
Some oil field adopts the non-drift such as kaolin, diatomite pearl as light-weight additive, but tap density is greater than 2.0g/cm
3, wanting preparation density is 1.0 ~ 1.5g/cm
3between low-density cement mortar be absolutely not.
Different according to the well cementation degree of depth, usually the oil well of less than 2000 meters low hot-well, low temperature oil-well is cemented the well, and with highdensity grout, (, between 70 ~ 90 DEG C, namely cement slurry density is at 1.8g/cm for the temperature in oil well
3~ 1.9g/cm
3); Be middle hot-well between 2000 ~ 4000 meters, (, between 90 ~ 150 DEG C, namely cement slurry density is at 1.6g/cm for the temperature in oil well for the grout of middle temperature oil well cementing Midst density
3~ 1.7g/cm
3); And be greater than 4000 meters for hot hole, with low-density grout, (, between 150 ~ 240 DEG C, namely cement slurry density is at 1.0g/cm for the temperature in oil well in high-temperature oil well well cementation
3~ 1.5g/cm
3).
Because land low temperature oil-well hydrocarbon resources is gradually reducing, exploitation is progressively by landwards deep layer and the bathypelagic exploitation of land low temperature oil-well, and traditional well cementing material drift pearl can not meet the needs of deep layer high-temperature oil well.
In view of the present situation of domestic well cementing material, adopt ceramic composite new technology, novel process, prepare hollow closed pore ceramic fine bead, zirconium diboride powder, carbonization zirconium powder, zirconia powder and silica flour is utilized to be raw material, zirconium carbide and silica flour repeatedly react generation zirconium diboride-silicon carbide-zirconium disilicide ceramic composite at high temperature, and density can be controlled in 0.5g/cm
3~ 0.85g/cm
3between, can meet the requirement of preparation low-density cement mortar, cement slurry density is at 1.0g/cm
3~ 1.5g/cm
3between, the pressure alleviating deep-seated oil bottom prevents blind hole.
Summary of the invention
The object of the invention is to overcome the existing drift pearl state of the art, utilize zirconium diboride powder, zirconium carbide, zirconium white and silica flour repeatedly react generation zirconium diboride-silicon carbide-zirconium disilicide ceramic composite at high temperature, Ceramic Composite microballon substitutes the drift pearl of flyash, there is provided a kind of cost low, excellent property, high temperature resistant, high strength, high rigidity, rate of change of the density is made to be less than 0.02, meet the requirement of light-weight cement slurry, closed pore cenosphere prepared by the ceramic composite adopted, through high temperature sintering, resistance to compression, the performance index such as folding strength exceed the drift pearl of flyash, pottery closed pore cenosphere density range is at 0.5g/cm
3~ 0.85g/cm
3controlled, and then preparation 1.0g/cm
3~ 1.5g/cm
3the test block of oil well cementing light weight cement, meets the requirement of long shut-in well well cementing material.
Its technical scheme is.
Comprise the preparation of Ceramic Composite closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, by G level oil well cement 40 ~ 50wt%, particle diameter 13 μm of superfine cement 10 ~ 15wt%, Ceramic Composite closed pore cenosphere 25 ~ 35 wt% of particle diameter 5 ~ 50 μm, , flyash 5 ~ the 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2wt%, the ratio mixing of sodium sulfate 0.5 ~ 1.0wt% and SILICA FUME 1 ~ 3wt%, with 0.5 ~ 0.6(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, get aliquot and pour one group of two block length into, wide, height is respectively in 53mm*53mm*53mm die trial, difference maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, 48 hours, soak in cold water after the demoulding and carry out cement slurry property test in 1 hour, comprise the mensuration of Ceramic Composite closed pore cenosphere resistance to hydrostatic pressure intensity, cement slurry density measures, withstand voltage density test, sedimentation stability, free liquid amount of precipitation, fluid loss falls, thickening time, the liquidity scale, carries out compressive property test.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, by particle diameter 1 ~ 60 μm of zirconium diboride powder, particle diameter 3 ~ 50 μm of carbonization zirconium powders, particle diameter 1 ~ 45 μm of silica flour is by weight 60 ~ 80wt%:11 ~ 22wt%:9 ~ 18wt% first by zirconium diboride powder, after carbonization zirconium powder and silica flour mixing and stirring, add the zirconium white ball milling of alcohol and powder mix weight 200% again, be pressed into blank drying, at 1450 ~ 1550 DEG C, under 20 ~ 50MPa, vacuum firing 5 ~ 20 minutes, obtain the sintered compact of zirconium diboride ceramics matrix material, the sintered compact of ceramic composite is processed into particle diameter 10 ~ 35 μm of microballons at balling machine.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, and the weight percent of Ceramic Composite microballon liquid slurry consists of: particle diameter 10 ~ 35 μm Ceramic Composite microballon 70 ~ 80wt%: water 20 ~ 30wt%.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, and adding whipping agent in zirconia ceramics compounded microbeads liquid slurry is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, Ceramic Composite microballon liquid starches abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballon, expansion temperature that four district's electric furnaces dewater 800 ~ 850 DEG C, dry sintering temperature 1400 ~ 1600 DEG C, melt surface temperature 1700 ~ 1800 DEG C, become bulb temperature 1400 ~ 1500 DEG C, obtain 5 ~ 50 μm of Ceramic Composite closed pore cenospheres through classification.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, and Ceramic Composite closed pore cenosphere its floatability is greater than 95%.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, and the cement briquette 8 hours ultimate compression strength of preparation is greater than 20MPa, and within 24 hours, ultimate compression strength is greater than 30MPa.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, it is characterized in that: the variable density scope of the sampling spot Ceramic Composite closed pore cenosphere of same batch of different positions is at ± 0.01 g/cm
3.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, and the fluid loss that falls of cement briquette is less than 50ml/30min.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, and cement briquette rate of change of the density is less than 0.02.
Described Ceramic Composite microballon prepares the method for low density oil well cementing cement briquette, it is characterized in that: Ceramic Composite closed pore cenosphere resistance to hydrostatic pressure intensity 100 ~ 400MPa.
the present invention has the following advantages.
1, the dependence to flyash floating bead in long-term well cementation can be changed, chemical reaction is there is and generates zirconium diboride-silicon carbide-zirconium disilicide ceramic composite in stupalith when high temperature sintering, it is good that resultant has ultimate compression strength height fold resistance, resistant to elevated temperatures ceramic material, high through high temperature sintering activity, size is controlled, and ceramic composite can meet the cementing requirements of 6000 ~ 8000 meters of high-temperature oil wells.
2, ceramic composite proportioning, sintering temperature can control, and this technique is advanced, and technology maturation, product performance are stable, and production cost is low, and output is high, and performance is good.
3
,the density of zirconium diboride-silicon carbide-zirconium disilicide Ceramic Composite microballon can be controlled in 0.5g/cm
3~ 0.85g/cm
3add the early strength that 13 μm of superfine cements can increase Behavior of Hardened Cement Paste test block, according to piling up the theoretical space added between SILICA FUME filler particles, G level oil well cement, superfine cement, ceramic fine bead have greater activity through more than 1000 DEG C high temperature sinterings, hydration reaction is fast, can form jelly, can improve early strength, ceramic fine bead performance is better than fly ash float, at military project space industry widespread use.
4
,utilize vertical four district high temperature Cheng Zhulu, adopt high pressure spraying high speed centrifugation rotary spraying technique, spraying sheet aperture decides granular size, enter body of heater after liquid is fully atomized, drop is at breathing space expanded by heating, and expanding volume is relevant with expansion temperature and density of foaming agent, again through sintering, melting, finally formation closed pore cenosphere, prevent from tying wall to improve output, adopt thermal cycling suction, wind-force blowing system, blower fan adopts speed control by frequency variation blower fan.
5, adopt purity 99.9% calcium oxide, react with water and generate calcium hydroxide, release amount of heat, improve cement briquette early strength.
embodiment.
Embodiment 1.
(1) 1. the preparation of Ceramic Composite closed pore cenosphere is prepared burden and is fired: by particle diameter 1 ~ 15 μm of zirconium diboride powder, particle diameter 3 ~ 20 μm of carbonization zirconium powders, particle diameter 1 ~ 15 μm of silica flour is after 70wt%:15wt%:15wt% mixing and stirring, add the zirconium white ball milling of alcohol and powder mix weight 200% again, be pressed into blank drying, at 1450 DEG C, under 30MPa, vacuum firing 15 minutes, obtain the sintered compact of ceramic composite, the sintered compact of ceramic composite is processed into particle diameter 10 ~ 15 μm of microballons at balling machine, 2. dosing: particle diameter 10 ~ 15 μm Ceramic Composite microballon 78wt%: water 22wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 1g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, vertical four district's electric furnaces dewater expansion temperature 800 DEG C, dry sintering temperature 1400 DEG C, melt surface temperature 1700 DEG C, become bulb temperature 1400 DEG C, clean classification through wind-force and obtain 5 ~ 15 μm of Ceramic Composite closed pore cenospheres.
(2) get 5 ~ 15 μm of Ceramic Composite closed pore cenosphere 50g, put into the beaker filling water, stir 1 minute with glass stick, leave standstill 5 minutes, observe the suspended state of Ceramic Composite closed pore cenosphere in beaker, the drift pearl in beaker and heavy pearl are taken out oven dry respectively and weighs, calculate its floatability.
(3) 5 ~ 15 μm of Ceramic Composite closed pore cenosphere grain 100g are got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, being poured into by the sample of Ceramic Composite microballon fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, and calculates percentage of damage and records static-pressure-resisting value and compressive strength.
(4) 5 ~ 15 μm of Ceramic Composite hole cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain Ceramic Composite closed pore cenosphere and take 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough, observed and recorded sample particle diameter distributes.
(5) low density oil well cementing cement briquette batching: be the Ceramic Composite closed pore cenosphere 35wt% of 5 ~ 15 μm, the flyash 5wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5wt% and micro-silicon 3wt% by G level oil well cement 45wt%, 13 μm of superfine cement 10wt%, particle diameter.
(6) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 10wt%, particle diameter is 5 ~ 15 μm of Ceramic Composite closed pore cenosphere 35wt%, the flyash 5wt% of loss on ignition 1.1%, that purity 99.9% calcium oxide 1.5wt%, sodium sulfate 0.5wt% and micro-silicon 3wt% put into stirrer for mixing is even.
(7) get in (6) that to mix sample a little, pour in beaker, by 0.5(W/C) water cement ratio modulation grout, stir with glass stick, pour in mud scale and weigh density.
(8) at temperature 28 DEG C ± 1 DEG C, with 0.5(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout stability and homogeneity.
(9) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm, high 53mm.
(10) observe weigh and record free liquid amount of precipitation, fall fluid loss, the thickening time, the liquidity scale.
(11) mensuration of cement briquette rate of change of the density, measure 24 and 48 hours cement briquette density, cement briquette is put into pressing machine pressurization (20 MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100 MPa, 200 MPa, 300 MPa), measure the cement briquette density after pressurization, rate of change of the density equals: (after pressurization, density deducts 24 and 48 hours cement briquette density)/24 and 48 hours cement briquette density, if rate of change of the density is greater than 0.02, illustrate that Ceramic Composite microballon inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density, the density of cement briquette equals the quality of cement briquette and the ratio of volume.
(12) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
(13) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
Embodiment 2.
(1) 1. the preparation of Ceramic Composite closed pore cenosphere is prepared burden and is fired: by particle diameter 20 ~ 35 μm of zirconium diboride powder, particle diameter 25 ~ 35 μm of carbonization zirconium powders and particle diameter 20 ~ 30 μm of silica flours after 75wt%:20wt%:5wt% mixing and stirring, add the zirconium white ball milling of alcohol and powder mix weight 200% again, be pressed into blank drying, 1500 DEG C, under 25MPa, vacuum firing 12 minutes, obtain the sintered compact of ceramic composite, the sintered compact of ceramic composite is processed into 20 ~ 25 μm of microballons at balling machine; 2. dosing: 20 ~ 25 μm Ceramic Composite microballon 75wt%: water 25wt%, in liquid slurry, add lightweight potassium sulfate whipping agent, concentration is 1.5g/L, 3. filters: by macrobead and Impurity removal; 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, expansion temperature that four district's electric furnaces dewater 820 DEG C, dry sintering temperature 1500 DEG C, melt surface temperature 1750 DEG C, become bulb temperature 1450 DEG C, clean classification through wind-force and obtain 20 ~ 30 μm of Ceramic Composite closed pore cenospheres.
(2) get 20 ~ 30 μm of Ceramic Composite closed pore cenosphere 50g, put into the beaker filling water, stir 1 minute with glass stick, leave standstill 5 minutes, observe the suspended state of Ceramic Composite closed pore cenosphere in beaker, the drift pearl in beaker and heavy pearl are taken out oven dry respectively and weighs, calculate its floatability.
(3) the Ceramic Composite closed pore cenosphere 100g of 20 ~ 30 μm is got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, being poured into by the sample of drift pearl fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, and calculates percentage of damage and records static-pressure-resisting value and compressive strength.
(4) 20 ~ 30 μm of Ceramic Composite closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain Ceramic Composite closed pore cenosphere and take 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough, observed and recorded sample particle diameter distributes.
(5) low density oil well cementing cement briquette batching: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter be 20 ~ 30 μm of Ceramic Composite closed pore cenosphere 30wt%, the flyash 6wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 2wt%, sodium sulfate 1wt% and micro-silicon 1wt%.
(6) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter is 20 ~ 30 μm of Ceramic Composite closed pore cenosphere 30wt%, the flyash 6wt% of loss on ignition 1.1%, that purity 99.9% calcium oxide 2wt%, sodium sulfate 1wt% and micro-silicon 1wt% put into stirrer for mixing is even.
(7) get in (6) that to mix sample a little, pour in beaker, by 0.6(W/C) water cement ratio modulation grout, stir with glass stick, pour in mud scale and weigh density.
(8) at temperature 28 DEG C ± 1 DEG C, with 0.6(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout stability and homogeneity.
(9) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm, high 53mm.
(10) observed and recorded free liquid amount of precipitation, fluid loss, thickening time, the liquidity scale fall.
(11) mensuration of cement briquette rate of change of the density, measure 24 and 48 hours cement briquette density, cement briquette is put into pressing machine pressurization (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa, 200MPa, 300MPa), measure the cement briquette density after pressurization, rate of change of the density equals: (after pressurization, density deducts 24 and 48 hours cement briquette density)/24 and 48 hours cement briquette density, if rate of change of the density is greater than 0.02, illustrate that Ceramic Composite microballon inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density, the density of cement briquette equals the quality of cement briquette and the ratio of volume.
(12) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
(13) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
Embodiment 3.
(1) 1. the preparation of Ceramic Composite closed pore cenosphere is prepared burden and is fired: by particle diameter 40 ~ 60 μm of zirconium diboride powder, particle diameter 40 ~ 50 μm of carbonization zirconium powders and particle diameter 35 ~ 45 μm of silica flours are after 78wt%:12 wt%:10 wt% mixing and stirring, add the zirconium white ball milling of alcohol and powder mix weight 200% again, be pressed into blank drying, at 1550 DEG C, under 25MPa, vacuum firing 10 minutes, obtain the sintered compact of ceramic composite, the sintered compact of ceramic composite is processed into 30 ~ 35 μm of microballons at balling machine, 2. dosing: 30 ~ 35 μm of Ceramic Composite microballon 80 wt%: water 20 wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 2g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, four district's electric furnaces dewater expansion 850 DEG C, dry sintering temperature 1600 DEG C, melt surface temperature 1800 DEG C, become bulb temperature 1500 DEG C, clean classification through wind-force and obtain 35 ~ 50 μm of Ceramic Composite closed pore cenospheres.
(2) get 35 ~ 50 μm of Ceramic Composite closed pore cenosphere 50g, put into the beaker filling water, stir 1 minute with glass stick, leave standstill 5 minutes, observe the suspended state of Ceramic Composite closed pore cenosphere in beaker, the drift pearl in beaker and heavy pearl are taken out oven dry respectively and weighs, calculate its floatability.
(3) 35 ~ 50 μm of Ceramic Composite closed pore cenosphere 100g are got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, being poured into by the sample of drift pearl fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, and calculates percentage of damage and static-pressure-resisting and compressive strength.
(4) 35 ~ 50 μm of Ceramic Composite closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain Ceramic Composite closed pore cenosphere and take 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough, observed and recorded sample particle diameter distributes.
(5) low density oil well cementing cement briquette batching: by getting G level oil well cement 45wt%, 13 μm of superfine cement 12wt%, particle diameter is Ceramic Composite closed pore cenosphere 33wt%, the flyash 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5wt%, sodium sulfate 0.5wt% and micro-silicon 1wt% of 35 ~ 50 μm.
(6) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 12wt%, particle diameter is 35 ~ 50 μm of Ceramic Composite closed pore cenosphere 33 wt%, the flyash 7wt% of loss on ignition 1.1%, that purity 99.9% calcium oxide 1.5wt%, sodium sulfate 0.5wt% and micro-silicon 1wt% put into stirrer for mixing is even.
(7) get in (6) that to mix sample a little, pour in beaker, by 0.5(W/C) the water cement ratio modulation grout of 5, stir with glass stick, pour in mud scale and weigh density.
(8) at temperature 28 DEG C ± 1 DEG C, with 0.55(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout stability and homogeneity.
(9) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm, high 53mm.
(10) observed and recorded free liquid amount of precipitation, fluid loss, thickening time, the liquidity scale fall.
(11) mensuration of cement briquette rate of change of the density, measure 24 and 48 hours cement briquette density, cement briquette is put into pressing machine pressurization (20MPa, 30MPa, 45MPa, 60MPa, 75MPa, 100MPa, 200MPa, 300MPa), measure the cement briquette density after pressurization, rate of change of the density equals: (after pressurization, density deducts 24 and 48 hours cement briquette density)/24 and 48 hours cement briquette density, if rate of change of the density is greater than 0.02, illustrate that Ceramic Composite microballon inhomogeneity of wall thickness is even, percentage of damage is high, after pressurization, density increases, do not reach standard, the degree of rate of change of the density and off-design density, the density of cement briquette equals the quality of cement briquette and the ratio of volume.
(12) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
(13) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by being defined on pressing machine of GB GB/T 177.
Note: G level oil well cement is Qi Yin cement mill, Shandong, the prosperous sub-calcium industry of purity 99.9% calcium oxide Shandong Zibo, the flyash Huaneng Group Xin Dian power plant of loss on ignition 1.1%, 13 μm of superfine cement Shengli Oil Field special cement factories.
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