CA1117987A - Sintered high density spherical ceramic pellets for gas and oil well proppants and their process of manufacture - Google Patents
Sintered high density spherical ceramic pellets for gas and oil well proppants and their process of manufactureInfo
- Publication number
- CA1117987A CA1117987A CA000339222A CA339222A CA1117987A CA 1117987 A CA1117987 A CA 1117987A CA 000339222 A CA000339222 A CA 000339222A CA 339222 A CA339222 A CA 339222A CA 1117987 A CA1117987 A CA 1117987A
- Authority
- CA
- Canada
- Prior art keywords
- pellets
- bauxite
- impeller
- rotating
- rpm
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
- C01F7/025—Granulation or agglomeration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/14—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating dishes or pans
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
- E21B43/267—Methods for stimulating production by forming crevices or fractures reinforcing fractures by propping
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
Abstract
ABSTRACT OF THE DISCLOSURE
Spherical sintered ceramic pellets having a spher-icity of at least 0.85 and a density of at least 95% of the theoretical density of the ceramic and the process for manufacturing the pellets utilizing a rotatable table mixer with a rotatable impacting impeller. The invention also comprises a method for propping open fractures in a well utilizing the spherical sintered ceramic pellets.
Spherical sintered ceramic pellets having a spher-icity of at least 0.85 and a density of at least 95% of the theoretical density of the ceramic and the process for manufacturing the pellets utilizing a rotatable table mixer with a rotatable impacting impeller. The invention also comprises a method for propping open fractures in a well utilizing the spherical sintered ceramic pellets.
Description
~7 SINT~ D HIG~ ~:NSI~ SPNEF~ICAL CB~IC PELLl~ FOR
GAS AND OIL WELI4 P~OPP~TS AND T~R
PROCESS OF MANU~ACTl~E
B~CKGROUND ûF T~IE INVENTIO~
~) FiQld of the In~n~lon 1~1'58 i~verl~ciorl rel~te~ ~o oil ~nd ga~ w~ll proppan~cs and ~nc~re particularly r~lste~ to s~ntered ceramlc proppant~ and a me~chod for ~i~a~ning a ~racture ln a ~ubterr&nean ~ormatioll in a propped condition by utili~ g the proppAnt.
b) ~5b:~
011 and natural ~as ar~ produc~d riml ~e~ls ha~ng porou~ and perme~le ~u~ter~ar~ o~eiOr'~.
The porosity of the ormatlon p~nle~ ~ form~ti~n to stor~ oil or ga~ d the permeability of ~he for-mation permits the oil or gas fluld to ~ove through the ~onx~cion. PQna~abil:L~y of the ormQ~ioTI i9 essential to permit oil and gas to ~lo~ to a lo~at~ on where lt ca~ be p~ped from th~ well. So~tim~3, the permeability of the formation holdlng ~ch~ ~sas or o~l i8 in~uf:Eicierlt for econo~ic reccav~ry of oll ~nd ga~. In othQr cas~ during opera~ion of the wQll, the perme~bility of the forma~cior~ drop~ eo th~ ~t~nt that further recov~ry bQcom~s ~conomical. In ~ch case~, it i~ necessary to rac~ure ~he forma~ nd prop the fracturea in ~n open conditlon by m~ o:~ a proppant n~teri~l or proppin~s a8ent. Such ~rac~ æ
iB u~ y accompli~hed by hydraullc pr~sYur~ ~nd the propp~n~ mat~rial or propping agent i8 a par-~ciculate ~erial ~uch a~ ~and, gla~ b~ad~ ox cer~c particl~s which ~re carried i~to th~ fractur~ by m~#
of a fluid.
3~7 .~
Sph~rlcal p~rtlcla~ of uxl~fo2~ ~ ar~
~rally ~okrlcrwledged t.o be the mo~t ~fecc~ve p~op-p~nt~ clue to max~ ed permeability. Pox~ th~ r~aso~
a~sumin~ o~he~r prop~rti~ to ~e ~lu~l, sph~rlcal or e~ tially spherical propp~nt~ ~uch a~ rou~d~d s~d gra~ ns 3 me~sllic ~ho~, glas~ be~acls a~d ~d ~:abul~r Dln~ ~r~ pref~rr~d.
Unfort~te~ly, in d~ep wells, wh~rQ high prs~ re~
are ~ncolmtered; e.~;., above abotlt 5000 pllit the fore-going 3pecifically m~ io~d propp~t~ 8r~ ch&r e~-~$rely ~e~fective or h~ve gre~tly r~ducQd pe~ility.
The bo~t o~ ~che ~or~golng speci~ically m~ntion~d prop-pant~ at hi8h pres~ux~s, ~ di~clos~d ~ U. S. P~tont 3,976,138 to Colpo~s, Jr. e~ al, i~ fu~ed alu~ina. Ho~-~ver, ~an fu~ad al~ a, a~ di~clos~d ~n U. S. Pate~:
3,976,138, has dra~tically r2t~d perslleab~l~ty 8~:
pre~sur~s in e~e~s of 5000 pBi.
As disclo~ed ln U. S. Pat~nt 4~06~,718 tss Cook, Jr. et al, tt h~s r~c~ntly bee~ d~scov~r~d tha~t s~n-tered b~ Q urlexpectedly ha~ a p~ ablli~y ~lch i8 superior to ~he pFev~owly m~n~ ed proppaat m~^
terials at pr~s~ur~ ~ilB hlgh ~ 10,000 p~i or highe~.
Unfortu~ately, th~ tered b~t~ ~t~x ~ctu~lly used ~ g ~che measur~m~ta dl~clos~d U. S. P~t~ 4,06~,718, do~ lOt ~v~ ~h# mo~t dQ~
slr~d sph~rical 6hape or highe~t p~ sbility ~l~ce pxior ~o the pre~ent invent~on, i~ was not po~oiblæ to co~r¢lally m~u~c~ur~ ~pher~cal sl~r~d batsxi'c~ p~r-ticle6 ~ving a 8pQ~Ci.fiC gravlty ~ Q~C~88 of about 3.5 ~hlch i8 r~quired to ~ve ~uflci~ co~r~ tr~ngth.
The prlor ~rt aintered bauxi~e par~lcl~s w~r~
elongated pell~t~ ~hich were tu~ d to forM ro~d~d edges in order co incr~e permaabll~ty. In add~t~on, the ylelds ~f such pellet~ were low compared ~o ~ch~
~mo~t of ma~er~al proce~ed. Rolling th~ p~r~icles - prior ~o ~lnterin~, as dlsc:losed ln column 4 o~ U. S.
Patent 4,068,718, was entirely ln~fectlve dnc~ p~r-t~cle~ having insuficien~ denEl~ty ~ere i~ar~bly ob~
tained.
~
Th~re i8 ~h~reore providad, in accorda~c2 wi~ch th~ pres~t in~ren~ion, ~phe~ical c~ramic p211~st8 02' par-ticles ha~i~8 d~nslties 1~ excass o~ 95 p~rc~nt of th~
theoretlcal de~ sy of the cer~ic ~terl~ ich ~pharlcal particle i8 useful ~ an oil and 8a~
proppant and ~hlch may be additiomllly u~e~ul, in c~r-tain c~rcumsta~ce~, a~ a lubricant~ ~bra~ , filtar med~a, cataly~t support materi~l or b~aritg ~c~rial.
When the particle i~ u~ed as ~ proppan~, ~che cQramic ZO materi~ preferably ~ tered bauxi~, althou~h cth~r cer~mics such as aluminum sil~cate clay~ co~ alI~g al~n~n a~d lron may be used.
~he lnvention further includ~s a procQIls for prop-ping fract~re~ ln oiLl ~nd gll9 WellB 11tili~in8 the p~r-tlcle of the irl~ention by lntroducing the particl~ 9f the invention a~ a propp~nt or proppitlg age~t into a ~lu~d such ~ oil or watex. and in~roduc~ng th6~ proppl~g agent con'cainin~ fluid into ~ ractur~ ln ~he ~ubt~rr~n ~ormation containing the w~ll, th~ cofn~sctlo~ p~ ur~l upon the :~racture beinx at l~a~t 4,000 p~i and us~lly ~3--;
3~
. .
lû, 000 p8i or higher, sald propping agen~ having an ~rage par~icle ~ize be~we~n 0.1 And Z m~llimete~r~.
It ha~ b~en ound tha~ pQrmeabil~t~r at 4,000 p~i or g~eater 18 ~up~rior ~ he p~rmeAbi.l~cy o prior Art e~s~nt~ally spherical ~lntered bauxite mat~r~al.
The ln~en~cio~ addition~lly inoludes a no~el ¢~fi.cierlt proces~ for manuacturing the ~pher~cal 8int~rcd oexa~lc pellet in accordanc~ ch ~che in~rention which comprise~
adding a ~-nter~ble cexam~c powdQr COmps)8itiO~I, which i~ moat de~irably bauxite when the p211et is to be u~ed ;' il8 ~ propp~nt materl~l, having an ~rer~ge par~icl~ ~ize - of betwe~ 0 and about 5 micro~ to a rotaeable ~able m~:cer pro~rided ~th a rotatable imp~ctln~ impell~r which i~ ~he same or ~ r to the on~ de~crlbed ln U. S, Pat~n~c 3, 690, 622 .
The ~cabl~ 18 ro~at~d at rom sbout 10 ~o about 60 rpm and t~e imp~cti~g lm~eller i8 rotated ~o obt~in an impeller tlp speed of rom sbout 25 to about 50 m~t~rs p~r ~econd. Su~icient water i~ add~d to cau~e ~s~n-~0 tially spherical c~ram~c pellet~ to ~orm and af~r ~uch pellQts have forned, from about 5 to about 15 p2re~nt of add~tion~l ceram~c powder by weight of pel~s i~
~ added and the impeller i~ rotated a~ a ~ip ~p~i~d o~ ~
betwRen about 5 a~d abo~ 20 met~r~i per ~eco~d ~or from about 1 to sbout 6 mlnut~s ~hlle rotatln~ the tabl~
~rom about 10 to about 60 rpm.
~he re~ulting p~llo~:8 are ~hen dried at b~two~n ~bout 100 arld ~bout 3~0 degre~ c~ntlgrad~ ~d ~nae~d at alrl~ring temp~r~tur~ unt~l DUXi~ density 18 obtai~ed.
.
7~
6 l~e slnter~d e~r~mlc pellets, in ~ccord~nc~ hth~ lnvet ~ion, ~ve ~ dennity in ea;c~ o g5 p~rcent of the th~or~'cic~l d~nei~y of ~hQ ceramic ~nd ~r~ 3ph~-r cal in ~hape, m¢aaing ~hat th~ r~io of ~hc ~ diamater to maxlmuG~ ~iame~er o p~lle~c~ (8~ r-iclty) o~ r~eated random saT~ple~ o~ pelle~e ~anufactured ln sccord~c¢ wlth the preseT~ n~ B grsat~r ~an 0~.82, a~most alw~ys gre~ter than 0.8$ and r~qu~n~1y ~r~a~-- 10 er ~han 0 . 9 with 9 5 percenc con- d~nce l~nit~ .
In contr~t, the av~rage ratio o~ mS~ um d~ r to m~xi~um diame~er of e~trud~d ~nd ~ bled ~nt~rQd baux-it~ pelle~ ~n accordlance ~th ~che prior a~t i~ g~rall7 19~8 than about 0. 80 .
"Essen~ially spherical", ~18 us~d herein, i3 ~n-tend~d to rnean ~n averag~ ratio of ~lrli~ d~mQter to max:Lmum diamet~r of beeween 0.7 ar~d 0.82.
"Spherical", as uset ~r~ln, ~ intended to x~an an avarage rat~o o~ nimum d~amæter to ~ d~t~r of gr~ater ~han 0. 8~.
The ~ph~rical pellQt~, in accord~c2 ~:lth tho pr~s~n~c inventio~, are m~ ctur~d by ~e~llg a c~ pas~d~r compo~ition. The sph~ical p~lle~s ar~ not m~u~ctu~d, as in prior ~rt, by fusion of cexamic ma~erlal ollowi3d by solidlficatio~. The cersmlc po~d~r ~y b~
terable eeramlc powder ~uch as powd~rs o~ bau~i~ a~d ~illcon ~arbide. If deslred, ~i~te~g a~ds ~r b~
corporated a$ a ~ar~ of the s~ntorabl~ ceran~c pas-ds~
~<-r l?xampl~, ~hen bau~it~ i8 us~d, b~tonlte cl~ ~sr iron _~_ '' ' s)~ide aiLds ~i~t~r~n~, when eil~con c~rblde ~ wsed, boron, buron carbide, alumlnum diboride, boron nitrlde, boron pho~phlde and oth~r bororl cotnpound~ ~id 0int~irg ~d wh~
aluminum ~ilicate type cl~y~ ar~ u~d, ~lux~8 #uch a~ iron oa:lde ~id sir~tering. Betw~en 0 snd 30 w~lght p~rcent o~
such ~int¢ring a~d~ may be used. The i~GOBt de~ira~le ran of sin~eri~g ald C8~1 be readily d~ermined by tho~ ~kill-ed ~1~ the art d~pendlng upon the p~rt~cular c~r~mlc and aid used. For ~ample, fr~ co 8, pre~r~1bly Q to 3 p~rcent ~d mo8t pre~r~bly ~ecwe~ 0~2 ~nd 1 perc~n~ b~
weight of b~n~con~te aid~ th~ ~ntQr~ng o~ b~ux~t~, from 0.4 to 5 percen~ of a sintering aid ~uch as a boro~
conta~ing compound i~ r~qulr~d or 3int~rin~ of ~lico carblde ~d up to 3û weight perc~nt of a 1uas m~t~ri~l ~uch as sotium c~rbons~e, lit~iiual carbo~at~, f~ld3p~r, man~sanese oxld~, ti'canla~ iron ox~de ~nd ~od~
cates aid slnt~ring of aluminum 81 l~Lcats~ clay~ .
Th~ process comprise0 ~ddi~g a ~ln~erable CQraltliC
powde~ compo~ition hs~ing an a~r~g~ particle 8i2:Q 0~ ~rom b~twee~ 0 and about 5 ~crorl~ to ~ ~ota~abl~ ~abl6~ mi2cer provlded witll a ~o~atable impacting ~ r. ~he ta~le m~y be som~what incl~n~d from th~ hor~zo~tal. The ~11 p~t~cle ~ze is r~quir~d in order to obtain a ~inl~h~d spherical ~ tered c~ramic pellet h~ng su~~ci~n~ d~n-~ity. A c~ramic powdQr av~rag~ p~r~lcle si~ of ~n 3~11~ th~ four micron~ 1~ dcair~l~ a~d the aY~rag~
particle si~e is pr~f~ably b~lo~ 3 ~icro~ ~nd wuellly above 0.5 micro The rota~c~ble tabl~ mixar provided with ~ch~ rot~tabl~
i~opacting imp~llor can be any ouch tev~Lc~ h ~ ~cho dQvice ob~al2lable from ~lrich ~Iach~ Inc~ ~ a3 the Eirtch Mlxer. Such a device 18 provid~d ~ieh a ~ or 3~ ~
inellned clrculsr t~ble whlch can b~ de ~o rot~'ce at a speed of from ~bout 10 to ~bout 6n re~rolutl~2ls p~r ~nut~
~rpm) and i~ prol7lded wi~h a ro~atable impac~ing impeller wh~ch can be mEld~ to rot~t~ at a t~p speed of fr~m about 5 to about 5~ me~ra per ~econd. Th~ c~ntral axl~ o~ th~
~npac~ng in~peller i.8 generally located within ~che mi~er at a positlon off center from the coen~cral axi8 o 'ch~
rotatable t~ble. The table may b~ in ~ hori~orlt~l or inclin~d positlon whQrein che incl~n~, lf a~r, i9 b~t~een 0 and 35 degree~ from the horiæo~tal.
A~fcer ~he ~interable cer~m~c powder compo~i'cion t~
~dded to the mlxer, the ta~le i8 rotat~d at from ~bout 10 to al~out 60 rpm and preferably from ~bout 20 to ~bout 40 rpm and the impacPtng impeller i~ rotated ~o obtain a tip ~peed of from about 25 to ~bou~c 50, prsferably Z5 to abou~
3S, meters per second and ~uffici.~nt wa~er i~ ~dded to cau~e es~enti~lly spherlcal cera~nlc p~llet~ of th~ de~ired ~ize to fo~ de~lredt the imp~ r m~y be illiti~lly rota~ad at from abou'c 5 to about 20 m~ters per second during addltion of one-hal of ~he ~u~lc~ent w~ter ~and sub~equently rotated ~ he h~gher tip ~peed o~ 25 ~o abou~ 50 meter~ p~r ~econd duri~ the ~ddlt~on of tha balanca of the water.
In general, the ~otal qu~nPi~y o~ wat~r which ~
sufficiQnt to oau~e esaenrially sph~ric~l co~c pellets .' to ~orm i.B from about 17 to ~out 20 p~rcent by~ weight oî
~ the c~r~Dic powder and u~ually b~ en about 18 uld ~bo~
20 percent by welght o~ the cer~mic powd~r. l~he tota3 mixin~ time a~t~r addition o an ~rliti~l quantity of ~he su~fi~ient wst~ar to the form~tiorl of e~enti~lly ~ph~r~c~1 pellets o~ the de~ir~ ize i~ fro~ about ~ to about 6 minutes .
I
t~7~
- From abou~c 5 to about 15 perc~ and pr~or~1~ ~om about 8 ~co ~bou~ 10 percen'c of ~ddîtion~l CQ~amiC p~d~r by we~ght of pelle~ i8 ~hen add~d, ~oll~wed ~y rot~l~g the lmpeller at a tip speed of b~ Qn about 5 and abcm'c ~0 meter~ per 3econd, pre~rabl~ be~wQen ab~ué 10 ~d ~out 20 me~ per ~econd Por from about 1 to about 6 an~nut~8 wh~le contlnuing to rotatQ ~e t~bl~ ~ fro~ aboult o about 60 rp~n and pre~er~ly ~rom about 20 ~co abotlt ; 40 rpm.
If de~ired, th~ rotation of th~ lmp~ller m~y th~ be - ~topped while the ~cablQ con~inues to rot~t~ fo~ b~
about 1 and about 5 mlnutç~
The impact~nE~ ~mpeller i~ pre~x~ly a d~ett pr~Ylded with perlph¢ral rods or bar~ att~chQd to th~ di~
lQngitudlnal a~ of the rode or bo,r~ is d~lxsbly ~en-tially p~rallel with the ~i~ of rotation of th~ l~pQllor, uhich i~ u~ually a vertical a~i~. The di~meter of t~Q
~p~ller i8 me~sur~d rom the axi~ of rota~lon to the c~
~er o ~he most dist~n~ rod or bar. Tip sp~d i~ tho speed ~ ~he ms~8t di~tan~ rod or b~r.
The di~ter of the iD~pell~r d~p~nd~ upon the si~e of ~h~ ~ixer b~t i~ us,ually less than 25 p~rce~t of th~
d~ te~ of the m~e~. , The imp~ r in mo~ applicat:lons i~ be~:we~n 10 and lO0 centimeter~ dia~te~ ~md usu~lly rota~es a~ fro~n 200 ~o 3750 rpm at the low~r tip llpæed~
of 10 to 20 ~tQr~ per ~colld dep~dislg ~pon imp~ r - diameter and at frGm 500 to 6500 ~p~ at th~ h~gh~r ~cip spQed~ of ~S to 35 meter~ p~r ~co~d d~p~nd~ng upo~
p~ller diamet~r.
The mixer s~y ~l~o b~ provid~d wieh a dsflsctor pl~te to de~l~ct c~ram~c materi~ f20~ th~ ~r ~all and pre~Eerat~ly eo th~ peller.
7~
Th~ r~ultlng pellets Mre d~ied ~t ~ temp~r~cu~ o b~twee~ abou~ 100 ~nd about 3~V~C un'cil pre~E~r~bly 1 than 3 percQnt and mG~t pre~er~bly le~s than 1 p~re~nt moi~cure remains in lthe pellQt~. ~rhe mo~t pr~f~ d drying t~perature 1~ between about 175 and 275C a~d the drying ti~e i8 u~ually bet:w~en a~9ut: 30 and ~bout 60 minute~ he pellet~ are ~hen f~ ced st ~lncering ~empQr~ture un~il ~x~ den~ty i~ o~ained. ~n the ca~e o~ bsuxite having, les~ th~n abou~ 90 p~rce~t ~lumina with ~ub~t~ial qu4~tltities of Fe2O3, SlO2 ~d T~02, 'ch~
fur~cing ~sually occur~ a~ ~ ~eratur~ of be~e~ d~o~c 1,450C and l,~SO~C ~or from about 1 to ~bout 10 m~ute2 and preferably occur~ at from abou~ 1,485~C ~:o about 1,515C for fs:om a~out 2 ~co about 4 mlnut~s.
The density whlch i~ ob~cal~ed ~a ln exc~ of about g5 percent of ~he l:heoretical d~nslty of ~he ~eramlc ma~erial u~ed. Xhe th~crQtical d~ o~ baw~te Yaria~
`' 80meWh~lt due to the ~omewhat di~~r~nt bn~ compo~itiol~s occurrlng ~n nature; howe~ver, th~ th~oretical den~lty of baux~Lte i8 us~lly abou~ 3.72 and th~ ~EPximum d~slty obtain~d a~ a re~ult of the proce~s of 'che l~v~ntion ., exc~eds 3.57 and u~ually 1~ beSw~en abou~ 3.60 and 3.S8.
Slnce ~ulbbling for 10 minu~e~ to 1 hour ~ub~t~ lly ~nhance~ suGh ~moothn~s, ~ flniohed p~ t~ c~n b~
tu~bled if de~ir~d.
Whsn the pelle~ are u~ed as ~ propping ~g~nt for ;. incr~asin~ pen~ea~lllty ~ a ~ubt~rrsne~n ~srth iEons~clo~
pQnetr~ted by a ~ell, the ~ph~rleal pellet~ ara ill~ro-duccd in~o a 1uid and the ~luld cont~Lnin~ th~ prop-ping ag~n~ i3 in'crodu~od in~o a ~rsctur~ whlc~ ha~ a `I compact~on pras~ure 3:~f at lea~t 4 000 p~i~ to d~posi~
l _ 9_ .
7~t~'7 a propp~ng di~trlbut:ion o ~che propplng agen~c ln ~
frag~ The propping d~str~ution i8 u~ually, b~t not neces~arily" ~ multllayer pack a~nd ~he o~erall p~rttcl~
., ~iz~ of the propping agent 1~ be~een 0.1 ~nd 2 a~llim~ter~.
ollawin~ ~ple~ serve to 111us~ra~e ~d ~ot llm~k the ~vention. Unless othe~r~e ~d~c~dJ par~s and p~rcen~ag~s are by weigh~.
P~LE 1.
About 135 kilogr&ms of Surlna~ b~ po~dor h~v-ing an averag;e pareicl~ ~ize o 14~198 tha~ 4 TDicro~ wer~
add~d wi~ aboult 1.35 kilo~r~ms of b~torllt~ clay p~sr to a~ E~r~ck mixer h~ving a pat~ d~meter of about 115 ceIl~imeters, an operatl~g c~paci~y of abs~ut 160 ~logr~
and an ~mpacting imp~ller di~ r of ~bout 27 ~ i~t~r~.
The pa~ ~7A~ ro~ed ~t about 35 rpm a~d t~
pell~r was rota~ced at ~bout 1090 rpDl a~d ~bo~t 82 k~
grams of wa~cer ~a~ ~dded. Ro~a~ o~ t~ pan ~nd ~m-. I pe~ r co~ti~ued for about 1 m~t¢ follo~d b~r incre~s-ing the ~mpeller ~p~d to about 2175 rpm ~nd a2~ addi tion~ll 8~ kilo~r~ms o~ wat~r w~ add~d. Th~ pan ~d iDI-i peller con~inue to rotate until ~eQd p~llets ar~ formæd wl lch contaln le~ 5 percen1: p~llets o a ~ e small~
er thar~ 35 ~ h~ (about 3 mIn~t~s~ Th2 ~ ller i~ th~n r~duc~d to ~bo~t 1090 rp~n and about 9 pou~nds o~ ~hs~ or~-~o~ng bau~cite powd~r co~taining 0.5 p~rc~ l~to~lt~ cl~r i~ ad~d. Ro~at~on o~ She pan and ~pell~r ~ cor~t~u~s for an add~tional 2 ml~utas to forEn ~pherieal p~llo~.
~hQ p~ t~ ~re eh~n dried ~3r ~bouc 30 ~uts~ st ; ! about 225~G in a rotati~g tra~ dryer and ~re the~ 1~od at abo~ 15GO~C: for about thr@~ ut~. The ~i~ld o~ u0ei~ul ;~, pell~ts ~ g a ~lz~ betw~n 14 and 60 ~rit 1~ Jator ~` :
- ' ~ 10-~
~.~
than 9O percQnt. r~e re~ul~cing p~llet~ ~ave ~ d~n~l~cy o~
about 3. 64 and ~ ~ph~ricl~y of sbout O . 9 .
~X~I.E 2 About 450 kllograms of Surina~ ~auxi~Q powdQr having a~ av~rag~ particle size o~ les~ th~ 4 micron~ w~r~ bl~nd-ed wlt~ about 4.$ kilograms o Be~conlte clag~ ~d ~out 164 kilograms of w~ter ln a ~ mulle~. The r~sulting putt~ ke material i~ then extruded ~chrou~h a~ ei8ht 1Inch extrud~r at room temperature with a water cool~d baQ~r~l. Th~ dle ~z~
cor~e~,ponds to the dlameter o a lO to 12 gr~ t p~tic10.
The resulting ex~ruded material i,~ dried for on~ hour at 260~C a~d granu~atlon iB ~ccomplished in a S~olce~ re-ciprocating f~ranula~or followad by a four minute pa83 through a Bllmger. Dust i~ r~ ed by sifting ~d rour~d-~d shap~s axe generated by t~ibling. The r~ult~g pell~t~
are s~nt~red a~ ~n ~ample 1.
The yield of ueeful pelle~a h~v:Lng ~ size be~woen 14 ansl 60 gr~t i8 1¢~1 than 80 p~reent. The resulti~g p~llet~
haYe a don~ity of about 3.64 and h~ve a ~ph~rlc~ty o~
than abo~t 0.8.
~D?Ll~ 3 ~ .
Bawc~te powde~ cont~lnlng 3 ~eigh~ p~rc~nt b~ onite w~ pelletized by rolllng ln ~ F~rro-Tach p~ tiz~r and fir~d in a ro~cary kiln ~ 1525-C for 3 mirlu~e0r 1525"C
in a ro~a~y ki}n wa,~ ln~,u~lcie~ ~or d~n~i~t~tlox ~ndicat~d by the whi~ce 4010r.
Pell~t~ w~re th6~n f~red a~ ~ g~l8 kll2l o~
at 1525C. Th~ irlng~t~at~mæn~ alt~d 1B appJlr~t Bp~Cii~lC ~raYlty of 3.30.
I~X~WLE 4.
Th~ permeab:Llity ln d~rcies o~ th~ pæll~, ~nu~
~actured ln ~ccor~anc~ ~ith Examplo 1 ~a,~ co~psr~sd ~th .
.~
.`
~he per~eabili~y in darci~ o th~ pell~ manufac~ur~d -, in ~ccord~c~3 wlth Example 2 in ~% KCl ~olution ~t 200~
at variou~ ~ppli~d pr~s~ures. ThQ re~ul~ ar~ sha~
TABLE: A.
T~BLE A
Pr~s~ur~ P~rmsa~lity Pe~ablll~y 2000 285 30~ -40~0 274 251 60~0 248 242 ~000 233 ~22 10000 2~2 213 example clearly ~h~w~ that th~ p~ t~ ccor-dsD~ce with ~che inv~ntion show be~7e~n above 4 ~nd abov~
9% bet~r 1s~w at p~e~sur~3~ o 4000 p~i ~o 10,000 p~i.
EXA~D?LE 5 .
Th~ p~ t~ of ~ample 1 ~;ere c~par~d for com~
pre~lbility with th~ pellets o~ ~ple 2 ~t 16,000 p~i lmd~r a pi~ton in a eo~flnod t~ . A b~d o~ about 0.25 lr~ch of th~ palle~s of ~he in~entlon iTI the te~t ~h~ed a compressibility o betwe~T~ 40 a~d 56 tbous~d~hs of ~ inch; where~, the pellet~ of Ex~pl~ 2 ~tbr ~he 88mQ conditio~s arld thicknes~ ~how~d a co~pres~l~iltty o~ bet~een 52 a~d 60 thoueandths of ~n i~ch.
1 .
'~
.
.
GAS AND OIL WELI4 P~OPP~TS AND T~R
PROCESS OF MANU~ACTl~E
B~CKGROUND ûF T~IE INVENTIO~
~) FiQld of the In~n~lon 1~1'58 i~verl~ciorl rel~te~ ~o oil ~nd ga~ w~ll proppan~cs and ~nc~re particularly r~lste~ to s~ntered ceramlc proppant~ and a me~chod for ~i~a~ning a ~racture ln a ~ubterr&nean ~ormatioll in a propped condition by utili~ g the proppAnt.
b) ~5b:~
011 and natural ~as ar~ produc~d riml ~e~ls ha~ng porou~ and perme~le ~u~ter~ar~ o~eiOr'~.
The porosity of the ormatlon p~nle~ ~ form~ti~n to stor~ oil or ga~ d the permeability of ~he for-mation permits the oil or gas fluld to ~ove through the ~onx~cion. PQna~abil:L~y of the ormQ~ioTI i9 essential to permit oil and gas to ~lo~ to a lo~at~ on where lt ca~ be p~ped from th~ well. So~tim~3, the permeability of the formation holdlng ~ch~ ~sas or o~l i8 in~uf:Eicierlt for econo~ic reccav~ry of oll ~nd ga~. In othQr cas~ during opera~ion of the wQll, the perme~bility of the forma~cior~ drop~ eo th~ ~t~nt that further recov~ry bQcom~s ~conomical. In ~ch case~, it i~ necessary to rac~ure ~he forma~ nd prop the fracturea in ~n open conditlon by m~ o:~ a proppant n~teri~l or proppin~s a8ent. Such ~rac~ æ
iB u~ y accompli~hed by hydraullc pr~sYur~ ~nd the propp~n~ mat~rial or propping agent i8 a par-~ciculate ~erial ~uch a~ ~and, gla~ b~ad~ ox cer~c particl~s which ~re carried i~to th~ fractur~ by m~#
of a fluid.
3~7 .~
Sph~rlcal p~rtlcla~ of uxl~fo2~ ~ ar~
~rally ~okrlcrwledged t.o be the mo~t ~fecc~ve p~op-p~nt~ clue to max~ ed permeability. Pox~ th~ r~aso~
a~sumin~ o~he~r prop~rti~ to ~e ~lu~l, sph~rlcal or e~ tially spherical propp~nt~ ~uch a~ rou~d~d s~d gra~ ns 3 me~sllic ~ho~, glas~ be~acls a~d ~d ~:abul~r Dln~ ~r~ pref~rr~d.
Unfort~te~ly, in d~ep wells, wh~rQ high prs~ re~
are ~ncolmtered; e.~;., above abotlt 5000 pllit the fore-going 3pecifically m~ io~d propp~t~ 8r~ ch&r e~-~$rely ~e~fective or h~ve gre~tly r~ducQd pe~ility.
The bo~t o~ ~che ~or~golng speci~ically m~ntion~d prop-pant~ at hi8h pres~ux~s, ~ di~clos~d ~ U. S. P~tont 3,976,138 to Colpo~s, Jr. e~ al, i~ fu~ed alu~ina. Ho~-~ver, ~an fu~ad al~ a, a~ di~clos~d ~n U. S. Pate~:
3,976,138, has dra~tically r2t~d perslleab~l~ty 8~:
pre~sur~s in e~e~s of 5000 pBi.
As disclo~ed ln U. S. Pat~nt 4~06~,718 tss Cook, Jr. et al, tt h~s r~c~ntly bee~ d~scov~r~d tha~t s~n-tered b~ Q urlexpectedly ha~ a p~ ablli~y ~lch i8 superior to ~he pFev~owly m~n~ ed proppaat m~^
terials at pr~s~ur~ ~ilB hlgh ~ 10,000 p~i or highe~.
Unfortu~ately, th~ tered b~t~ ~t~x ~ctu~lly used ~ g ~che measur~m~ta dl~clos~d U. S. P~t~ 4,06~,718, do~ lOt ~v~ ~h# mo~t dQ~
slr~d sph~rical 6hape or highe~t p~ sbility ~l~ce pxior ~o the pre~ent invent~on, i~ was not po~oiblæ to co~r¢lally m~u~c~ur~ ~pher~cal sl~r~d batsxi'c~ p~r-ticle6 ~ving a 8pQ~Ci.fiC gravlty ~ Q~C~88 of about 3.5 ~hlch i8 r~quired to ~ve ~uflci~ co~r~ tr~ngth.
The prlor ~rt aintered bauxi~e par~lcl~s w~r~
elongated pell~t~ ~hich were tu~ d to forM ro~d~d edges in order co incr~e permaabll~ty. In add~t~on, the ylelds ~f such pellet~ were low compared ~o ~ch~
~mo~t of ma~er~al proce~ed. Rolling th~ p~r~icles - prior ~o ~lnterin~, as dlsc:losed ln column 4 o~ U. S.
Patent 4,068,718, was entirely ln~fectlve dnc~ p~r-t~cle~ having insuficien~ denEl~ty ~ere i~ar~bly ob~
tained.
~
Th~re i8 ~h~reore providad, in accorda~c2 wi~ch th~ pres~t in~ren~ion, ~phe~ical c~ramic p211~st8 02' par-ticles ha~i~8 d~nslties 1~ excass o~ 95 p~rc~nt of th~
theoretlcal de~ sy of the cer~ic ~terl~ ich ~pharlcal particle i8 useful ~ an oil and 8a~
proppant and ~hlch may be additiomllly u~e~ul, in c~r-tain c~rcumsta~ce~, a~ a lubricant~ ~bra~ , filtar med~a, cataly~t support materi~l or b~aritg ~c~rial.
When the particle i~ u~ed as ~ proppan~, ~che cQramic ZO materi~ preferably ~ tered bauxi~, althou~h cth~r cer~mics such as aluminum sil~cate clay~ co~ alI~g al~n~n a~d lron may be used.
~he lnvention further includ~s a procQIls for prop-ping fract~re~ ln oiLl ~nd gll9 WellB 11tili~in8 the p~r-tlcle of the irl~ention by lntroducing the particl~ 9f the invention a~ a propp~nt or proppitlg age~t into a ~lu~d such ~ oil or watex. and in~roduc~ng th6~ proppl~g agent con'cainin~ fluid into ~ ractur~ ln ~he ~ubt~rr~n ~ormation containing the w~ll, th~ cofn~sctlo~ p~ ur~l upon the :~racture beinx at l~a~t 4,000 p~i and us~lly ~3--;
3~
. .
lû, 000 p8i or higher, sald propping agen~ having an ~rage par~icle ~ize be~we~n 0.1 And Z m~llimete~r~.
It ha~ b~en ound tha~ pQrmeabil~t~r at 4,000 p~i or g~eater 18 ~up~rior ~ he p~rmeAbi.l~cy o prior Art e~s~nt~ally spherical ~lntered bauxite mat~r~al.
The ln~en~cio~ addition~lly inoludes a no~el ¢~fi.cierlt proces~ for manuacturing the ~pher~cal 8int~rcd oexa~lc pellet in accordanc~ ch ~che in~rention which comprise~
adding a ~-nter~ble cexam~c powdQr COmps)8itiO~I, which i~ moat de~irably bauxite when the p211et is to be u~ed ;' il8 ~ propp~nt materl~l, having an ~rer~ge par~icl~ ~ize - of betwe~ 0 and about 5 micro~ to a rotaeable ~able m~:cer pro~rided ~th a rotatable imp~ctln~ impell~r which i~ ~he same or ~ r to the on~ de~crlbed ln U. S, Pat~n~c 3, 690, 622 .
The ~cabl~ 18 ro~at~d at rom sbout 10 ~o about 60 rpm and t~e imp~cti~g lm~eller i8 rotated ~o obt~in an impeller tlp speed of rom sbout 25 to about 50 m~t~rs p~r ~econd. Su~icient water i~ add~d to cau~e ~s~n-~0 tially spherical c~ram~c pellet~ to ~orm and af~r ~uch pellQts have forned, from about 5 to about 15 p2re~nt of add~tion~l ceram~c powder by weight of pel~s i~
~ added and the impeller i~ rotated a~ a ~ip ~p~i~d o~ ~
betwRen about 5 a~d abo~ 20 met~r~i per ~eco~d ~or from about 1 to sbout 6 mlnut~s ~hlle rotatln~ the tabl~
~rom about 10 to about 60 rpm.
~he re~ulting p~llo~:8 are ~hen dried at b~two~n ~bout 100 arld ~bout 3~0 degre~ c~ntlgrad~ ~d ~nae~d at alrl~ring temp~r~tur~ unt~l DUXi~ density 18 obtai~ed.
.
7~
6 l~e slnter~d e~r~mlc pellets, in ~ccord~nc~ hth~ lnvet ~ion, ~ve ~ dennity in ea;c~ o g5 p~rcent of the th~or~'cic~l d~nei~y of ~hQ ceramic ~nd ~r~ 3ph~-r cal in ~hape, m¢aaing ~hat th~ r~io of ~hc ~ diamater to maxlmuG~ ~iame~er o p~lle~c~ (8~ r-iclty) o~ r~eated random saT~ple~ o~ pelle~e ~anufactured ln sccord~c¢ wlth the preseT~ n~ B grsat~r ~an 0~.82, a~most alw~ys gre~ter than 0.8$ and r~qu~n~1y ~r~a~-- 10 er ~han 0 . 9 with 9 5 percenc con- d~nce l~nit~ .
In contr~t, the av~rage ratio o~ mS~ um d~ r to m~xi~um diame~er of e~trud~d ~nd ~ bled ~nt~rQd baux-it~ pelle~ ~n accordlance ~th ~che prior a~t i~ g~rall7 19~8 than about 0. 80 .
"Essen~ially spherical", ~18 us~d herein, i3 ~n-tend~d to rnean ~n averag~ ratio of ~lrli~ d~mQter to max:Lmum diamet~r of beeween 0.7 ar~d 0.82.
"Spherical", as uset ~r~ln, ~ intended to x~an an avarage rat~o o~ nimum d~amæter to ~ d~t~r of gr~ater ~han 0. 8~.
The ~ph~rical pellQt~, in accord~c2 ~:lth tho pr~s~n~c inventio~, are m~ ctur~d by ~e~llg a c~ pas~d~r compo~ition. The sph~ical p~lle~s ar~ not m~u~ctu~d, as in prior ~rt, by fusion of cexamic ma~erlal ollowi3d by solidlficatio~. The cersmlc po~d~r ~y b~
terable eeramlc powder ~uch as powd~rs o~ bau~i~ a~d ~illcon ~arbide. If deslred, ~i~te~g a~ds ~r b~
corporated a$ a ~ar~ of the s~ntorabl~ ceran~c pas-ds~
~<-r l?xampl~, ~hen bau~it~ i8 us~d, b~tonlte cl~ ~sr iron _~_ '' ' s)~ide aiLds ~i~t~r~n~, when eil~con c~rblde ~ wsed, boron, buron carbide, alumlnum diboride, boron nitrlde, boron pho~phlde and oth~r bororl cotnpound~ ~id 0int~irg ~d wh~
aluminum ~ilicate type cl~y~ ar~ u~d, ~lux~8 #uch a~ iron oa:lde ~id sir~tering. Betw~en 0 snd 30 w~lght p~rcent o~
such ~int¢ring a~d~ may be used. The i~GOBt de~ira~le ran of sin~eri~g ald C8~1 be readily d~ermined by tho~ ~kill-ed ~1~ the art d~pendlng upon the p~rt~cular c~r~mlc and aid used. For ~ample, fr~ co 8, pre~r~1bly Q to 3 p~rcent ~d mo8t pre~r~bly ~ecwe~ 0~2 ~nd 1 perc~n~ b~
weight of b~n~con~te aid~ th~ ~ntQr~ng o~ b~ux~t~, from 0.4 to 5 percen~ of a sintering aid ~uch as a boro~
conta~ing compound i~ r~qulr~d or 3int~rin~ of ~lico carblde ~d up to 3û weight perc~nt of a 1uas m~t~ri~l ~uch as sotium c~rbons~e, lit~iiual carbo~at~, f~ld3p~r, man~sanese oxld~, ti'canla~ iron ox~de ~nd ~od~
cates aid slnt~ring of aluminum 81 l~Lcats~ clay~ .
Th~ process comprise0 ~ddi~g a ~ln~erable CQraltliC
powde~ compo~ition hs~ing an a~r~g~ particle 8i2:Q 0~ ~rom b~twee~ 0 and about 5 ~crorl~ to ~ ~ota~abl~ ~abl6~ mi2cer provlded witll a ~o~atable impacting ~ r. ~he ta~le m~y be som~what incl~n~d from th~ hor~zo~tal. The ~11 p~t~cle ~ze is r~quir~d in order to obtain a ~inl~h~d spherical ~ tered c~ramic pellet h~ng su~~ci~n~ d~n-~ity. A c~ramic powdQr av~rag~ p~r~lcle si~ of ~n 3~11~ th~ four micron~ 1~ dcair~l~ a~d the aY~rag~
particle si~e is pr~f~ably b~lo~ 3 ~icro~ ~nd wuellly above 0.5 micro The rota~c~ble tabl~ mixar provided with ~ch~ rot~tabl~
i~opacting imp~llor can be any ouch tev~Lc~ h ~ ~cho dQvice ob~al2lable from ~lrich ~Iach~ Inc~ ~ a3 the Eirtch Mlxer. Such a device 18 provid~d ~ieh a ~ or 3~ ~
inellned clrculsr t~ble whlch can b~ de ~o rot~'ce at a speed of from ~bout 10 to ~bout 6n re~rolutl~2ls p~r ~nut~
~rpm) and i~ prol7lded wi~h a ro~atable impac~ing impeller wh~ch can be mEld~ to rot~t~ at a t~p speed of fr~m about 5 to about 5~ me~ra per ~econd. Th~ c~ntral axl~ o~ th~
~npac~ng in~peller i.8 generally located within ~che mi~er at a positlon off center from the coen~cral axi8 o 'ch~
rotatable t~ble. The table may b~ in ~ hori~orlt~l or inclin~d positlon whQrein che incl~n~, lf a~r, i9 b~t~een 0 and 35 degree~ from the horiæo~tal.
A~fcer ~he ~interable cer~m~c powder compo~i'cion t~
~dded to the mlxer, the ta~le i8 rotat~d at from ~bout 10 to al~out 60 rpm and preferably from ~bout 20 to ~bout 40 rpm and the impacPtng impeller i~ rotated ~o obtain a tip ~peed of from about 25 to ~bou~c 50, prsferably Z5 to abou~
3S, meters per second and ~uffici.~nt wa~er i~ ~dded to cau~e es~enti~lly spherlcal cera~nlc p~llet~ of th~ de~ired ~ize to fo~ de~lredt the imp~ r m~y be illiti~lly rota~ad at from abou'c 5 to about 20 m~ters per second during addltion of one-hal of ~he ~u~lc~ent w~ter ~and sub~equently rotated ~ he h~gher tip ~peed o~ 25 ~o abou~ 50 meter~ p~r ~econd duri~ the ~ddlt~on of tha balanca of the water.
In general, the ~otal qu~nPi~y o~ wat~r which ~
sufficiQnt to oau~e esaenrially sph~ric~l co~c pellets .' to ~orm i.B from about 17 to ~out 20 p~rcent by~ weight oî
~ the c~r~Dic powder and u~ually b~ en about 18 uld ~bo~
20 percent by welght o~ the cer~mic powd~r. l~he tota3 mixin~ time a~t~r addition o an ~rliti~l quantity of ~he su~fi~ient wst~ar to the form~tiorl of e~enti~lly ~ph~r~c~1 pellets o~ the de~ir~ ize i~ fro~ about ~ to about 6 minutes .
I
t~7~
- From abou~c 5 to about 15 perc~ and pr~or~1~ ~om about 8 ~co ~bou~ 10 percen'c of ~ddîtion~l CQ~amiC p~d~r by we~ght of pelle~ i8 ~hen add~d, ~oll~wed ~y rot~l~g the lmpeller at a tip speed of b~ Qn about 5 and abcm'c ~0 meter~ per 3econd, pre~rabl~ be~wQen ab~ué 10 ~d ~out 20 me~ per ~econd Por from about 1 to about 6 an~nut~8 wh~le contlnuing to rotatQ ~e t~bl~ ~ fro~ aboult o about 60 rp~n and pre~er~ly ~rom about 20 ~co abotlt ; 40 rpm.
If de~ired, th~ rotation of th~ lmp~ller m~y th~ be - ~topped while the ~cablQ con~inues to rot~t~ fo~ b~
about 1 and about 5 mlnutç~
The impact~nE~ ~mpeller i~ pre~x~ly a d~ett pr~Ylded with perlph¢ral rods or bar~ att~chQd to th~ di~
lQngitudlnal a~ of the rode or bo,r~ is d~lxsbly ~en-tially p~rallel with the ~i~ of rotation of th~ l~pQllor, uhich i~ u~ually a vertical a~i~. The di~meter of t~Q
~p~ller i8 me~sur~d rom the axi~ of rota~lon to the c~
~er o ~he most dist~n~ rod or bar. Tip sp~d i~ tho speed ~ ~he ms~8t di~tan~ rod or b~r.
The di~ter of the iD~pell~r d~p~nd~ upon the si~e of ~h~ ~ixer b~t i~ us,ually less than 25 p~rce~t of th~
d~ te~ of the m~e~. , The imp~ r in mo~ applicat:lons i~ be~:we~n 10 and lO0 centimeter~ dia~te~ ~md usu~lly rota~es a~ fro~n 200 ~o 3750 rpm at the low~r tip llpæed~
of 10 to 20 ~tQr~ per ~colld dep~dislg ~pon imp~ r - diameter and at frGm 500 to 6500 ~p~ at th~ h~gh~r ~cip spQed~ of ~S to 35 meter~ p~r ~co~d d~p~nd~ng upo~
p~ller diamet~r.
The mixer s~y ~l~o b~ provid~d wieh a dsflsctor pl~te to de~l~ct c~ram~c materi~ f20~ th~ ~r ~all and pre~Eerat~ly eo th~ peller.
7~
Th~ r~ultlng pellets Mre d~ied ~t ~ temp~r~cu~ o b~twee~ abou~ 100 ~nd about 3~V~C un'cil pre~E~r~bly 1 than 3 percQnt and mG~t pre~er~bly le~s than 1 p~re~nt moi~cure remains in lthe pellQt~. ~rhe mo~t pr~f~ d drying t~perature 1~ between about 175 and 275C a~d the drying ti~e i8 u~ually bet:w~en a~9ut: 30 and ~bout 60 minute~ he pellet~ are ~hen f~ ced st ~lncering ~empQr~ture un~il ~x~ den~ty i~ o~ained. ~n the ca~e o~ bsuxite having, les~ th~n abou~ 90 p~rce~t ~lumina with ~ub~t~ial qu4~tltities of Fe2O3, SlO2 ~d T~02, 'ch~
fur~cing ~sually occur~ a~ ~ ~eratur~ of be~e~ d~o~c 1,450C and l,~SO~C ~or from about 1 to ~bout 10 m~ute2 and preferably occur~ at from abou~ 1,485~C ~:o about 1,515C for fs:om a~out 2 ~co about 4 mlnut~s.
The density whlch i~ ob~cal~ed ~a ln exc~ of about g5 percent of ~he l:heoretical d~nslty of ~he ~eramlc ma~erial u~ed. Xhe th~crQtical d~ o~ baw~te Yaria~
`' 80meWh~lt due to the ~omewhat di~~r~nt bn~ compo~itiol~s occurrlng ~n nature; howe~ver, th~ th~oretical den~lty of baux~Lte i8 us~lly abou~ 3.72 and th~ ~EPximum d~slty obtain~d a~ a re~ult of the proce~s of 'che l~v~ntion ., exc~eds 3.57 and u~ually 1~ beSw~en abou~ 3.60 and 3.S8.
Slnce ~ulbbling for 10 minu~e~ to 1 hour ~ub~t~ lly ~nhance~ suGh ~moothn~s, ~ flniohed p~ t~ c~n b~
tu~bled if de~ir~d.
Whsn the pelle~ are u~ed as ~ propping ~g~nt for ;. incr~asin~ pen~ea~lllty ~ a ~ubt~rrsne~n ~srth iEons~clo~
pQnetr~ted by a ~ell, the ~ph~rleal pellet~ ara ill~ro-duccd in~o a 1uid and the ~luld cont~Lnin~ th~ prop-ping ag~n~ i3 in'crodu~od in~o a ~rsctur~ whlc~ ha~ a `I compact~on pras~ure 3:~f at lea~t 4 000 p~i~ to d~posi~
l _ 9_ .
7~t~'7 a propp~ng di~trlbut:ion o ~che propplng agen~c ln ~
frag~ The propping d~str~ution i8 u~ually, b~t not neces~arily" ~ multllayer pack a~nd ~he o~erall p~rttcl~
., ~iz~ of the propping agent 1~ be~een 0.1 ~nd 2 a~llim~ter~.
ollawin~ ~ple~ serve to 111us~ra~e ~d ~ot llm~k the ~vention. Unless othe~r~e ~d~c~dJ par~s and p~rcen~ag~s are by weigh~.
P~LE 1.
About 135 kilogr&ms of Surlna~ b~ po~dor h~v-ing an averag;e pareicl~ ~ize o 14~198 tha~ 4 TDicro~ wer~
add~d wi~ aboult 1.35 kilo~r~ms of b~torllt~ clay p~sr to a~ E~r~ck mixer h~ving a pat~ d~meter of about 115 ceIl~imeters, an operatl~g c~paci~y of abs~ut 160 ~logr~
and an ~mpacting imp~ller di~ r of ~bout 27 ~ i~t~r~.
The pa~ ~7A~ ro~ed ~t about 35 rpm a~d t~
pell~r was rota~ced at ~bout 1090 rpDl a~d ~bo~t 82 k~
grams of wa~cer ~a~ ~dded. Ro~a~ o~ t~ pan ~nd ~m-. I pe~ r co~ti~ued for about 1 m~t¢ follo~d b~r incre~s-ing the ~mpeller ~p~d to about 2175 rpm ~nd a2~ addi tion~ll 8~ kilo~r~ms o~ wat~r w~ add~d. Th~ pan ~d iDI-i peller con~inue to rotate until ~eQd p~llets ar~ formæd wl lch contaln le~ 5 percen1: p~llets o a ~ e small~
er thar~ 35 ~ h~ (about 3 mIn~t~s~ Th2 ~ ller i~ th~n r~duc~d to ~bo~t 1090 rp~n and about 9 pou~nds o~ ~hs~ or~-~o~ng bau~cite powd~r co~taining 0.5 p~rc~ l~to~lt~ cl~r i~ ad~d. Ro~at~on o~ She pan and ~pell~r ~ cor~t~u~s for an add~tional 2 ml~utas to forEn ~pherieal p~llo~.
~hQ p~ t~ ~re eh~n dried ~3r ~bouc 30 ~uts~ st ; ! about 225~G in a rotati~g tra~ dryer and ~re the~ 1~od at abo~ 15GO~C: for about thr@~ ut~. The ~i~ld o~ u0ei~ul ;~, pell~ts ~ g a ~lz~ betw~n 14 and 60 ~rit 1~ Jator ~` :
- ' ~ 10-~
~.~
than 9O percQnt. r~e re~ul~cing p~llet~ ~ave ~ d~n~l~cy o~
about 3. 64 and ~ ~ph~ricl~y of sbout O . 9 .
~X~I.E 2 About 450 kllograms of Surina~ ~auxi~Q powdQr having a~ av~rag~ particle size o~ les~ th~ 4 micron~ w~r~ bl~nd-ed wlt~ about 4.$ kilograms o Be~conlte clag~ ~d ~out 164 kilograms of w~ter ln a ~ mulle~. The r~sulting putt~ ke material i~ then extruded ~chrou~h a~ ei8ht 1Inch extrud~r at room temperature with a water cool~d baQ~r~l. Th~ dle ~z~
cor~e~,ponds to the dlameter o a lO to 12 gr~ t p~tic10.
The resulting ex~ruded material i,~ dried for on~ hour at 260~C a~d granu~atlon iB ~ccomplished in a S~olce~ re-ciprocating f~ranula~or followad by a four minute pa83 through a Bllmger. Dust i~ r~ ed by sifting ~d rour~d-~d shap~s axe generated by t~ibling. The r~ult~g pell~t~
are s~nt~red a~ ~n ~ample 1.
The yield of ueeful pelle~a h~v:Lng ~ size be~woen 14 ansl 60 gr~t i8 1¢~1 than 80 p~reent. The resulti~g p~llet~
haYe a don~ity of about 3.64 and h~ve a ~ph~rlc~ty o~
than abo~t 0.8.
~D?Ll~ 3 ~ .
Bawc~te powde~ cont~lnlng 3 ~eigh~ p~rc~nt b~ onite w~ pelletized by rolllng ln ~ F~rro-Tach p~ tiz~r and fir~d in a ro~cary kiln ~ 1525-C for 3 mirlu~e0r 1525"C
in a ro~a~y ki}n wa,~ ln~,u~lcie~ ~or d~n~i~t~tlox ~ndicat~d by the whi~ce 4010r.
Pell~t~ w~re th6~n f~red a~ ~ g~l8 kll2l o~
at 1525C. Th~ irlng~t~at~mæn~ alt~d 1B appJlr~t Bp~Cii~lC ~raYlty of 3.30.
I~X~WLE 4.
Th~ permeab:Llity ln d~rcies o~ th~ pæll~, ~nu~
~actured ln ~ccor~anc~ ~ith Examplo 1 ~a,~ co~psr~sd ~th .
.~
.`
~he per~eabili~y in darci~ o th~ pell~ manufac~ur~d -, in ~ccord~c~3 wlth Example 2 in ~% KCl ~olution ~t 200~
at variou~ ~ppli~d pr~s~ures. ThQ re~ul~ ar~ sha~
TABLE: A.
T~BLE A
Pr~s~ur~ P~rmsa~lity Pe~ablll~y 2000 285 30~ -40~0 274 251 60~0 248 242 ~000 233 ~22 10000 2~2 213 example clearly ~h~w~ that th~ p~ t~ ccor-dsD~ce with ~che inv~ntion show be~7e~n above 4 ~nd abov~
9% bet~r 1s~w at p~e~sur~3~ o 4000 p~i ~o 10,000 p~i.
EXA~D?LE 5 .
Th~ p~ t~ of ~ample 1 ~;ere c~par~d for com~
pre~lbility with th~ pellets o~ ~ple 2 ~t 16,000 p~i lmd~r a pi~ton in a eo~flnod t~ . A b~d o~ about 0.25 lr~ch of th~ palle~s of ~he in~entlon iTI the te~t ~h~ed a compressibility o betwe~T~ 40 a~d 56 tbous~d~hs of ~ inch; where~, the pellet~ of Ex~pl~ 2 ~tbr ~he 88mQ conditio~s arld thicknes~ ~how~d a co~pres~l~iltty o~ bet~een 52 a~d 60 thoueandths of ~n i~ch.
1 .
'~
.
.
Claims (22)
1. A process for manufacturing spherical sintered ceramic pellets comprising:
a) Adding a sinterable ceramic powder composition having an average particle size of between 0 and about 5 microns to a rotatable table mixer pro-vided with a rotatable impacting impeller;
b) Rotating said table at from about 10 to about 60 rpm and rotating said impacting impeller to attain a tip speed of from about 25 to about 50 meters per second;
c) Adding sufficient water to cause spherical ceramic pellets to form;
d) Adding from about 5 to about 15 percent of addi-tional ceramic powder by weight of pellets;
e) Rotating said impeller at a tip speed of be-tween about 5 and about 20 meters per second for from about 1 to about 6 minutes while rotating said table at from about 10 to about 60 rpm;
f) Drying said pellets at between about 100 and about 300°C; and g) Furnacing said pellets at sintering temperature until maximum density is obtained.
a) Adding a sinterable ceramic powder composition having an average particle size of between 0 and about 5 microns to a rotatable table mixer pro-vided with a rotatable impacting impeller;
b) Rotating said table at from about 10 to about 60 rpm and rotating said impacting impeller to attain a tip speed of from about 25 to about 50 meters per second;
c) Adding sufficient water to cause spherical ceramic pellets to form;
d) Adding from about 5 to about 15 percent of addi-tional ceramic powder by weight of pellets;
e) Rotating said impeller at a tip speed of be-tween about 5 and about 20 meters per second for from about 1 to about 6 minutes while rotating said table at from about 10 to about 60 rpm;
f) Drying said pellets at between about 100 and about 300°C; and g) Furnacing said pellets at sintering temperature until maximum density is obtained.
2. The process of Claim 1 wherein prior to drying the pellets, the rotation of the impeller is stopped while the table continues to rotate for between 1 and about 5 minutes.
3. The process of Claim 1 wherein said mixer is also provided with at least one deflector plate to deflect ceramic material from the mixer wall.
4. The process of Claim 1 wherein between about 0 and about 30 weight percent of a sintering aid is added to the ceramic material.
5. The process of Claim 1 wherein the sinterable ceramic powder is selected from bauxite, silicon carbide and aluminum silicate clay.
6. The process of Claim 1 wherein said table is ro-tated at from about 20 to 60 rpm and said ceramic ma-terial is bauxite.
7. The process of Claim 6 wherein said impeller is rotated at a tip speed of from about 25 to about 35 meters per second prior to the adding of said addi-tional ceramic powder and from about 10 to about 20 meters per second after the adding of said additional ceramic powder.
8. The process of Claim 7 wherein the diameter of said impeller is from about 10 to about 100 centimeters and prior to the adding of said additional ceramic powder, rotates at from about 500 to about 6500 rpm and sub-sequent to the adding of said additional ceramic powder rotates at from about 200 to about 3750 rpm.
9. The process of Claim 7 wherein from about 8 to about 10 percent of additional ceramic powder by weight of pellets is added.
10. The process of Claim 3 wherein subsequent to the addition of said additional ceramic powder, said impeller is rotated for from about 2 to about 4 minutes before the rotation of the impeller is stopped.
11. The process of Claim 10 wherein the pellets are dried at a temperature of between about 175 and about 275°C in a rotating tray dryer for from about 30 to about 60 minutes.
12. The process of Claim 1 wherein said ceramic com-position is bauxite and said furnacing temperature is from about 1485°C to about 1515°C and the time of furnacing is from about 2 to about 4 minutes.
13. The process of Claim 1 wherein the pellets are tumbled for 10 minutes to about one hour subsequent to firing.
14. A process for manufacturing spherical sintered bauxite pellets comprising:
a) Adding bauxite powder having an average par-ticle size of between 0 and about 4 microns to a rotatable inclined table mixer provided with a rotatable impacting impeller;
b) Rotating said table at from about 10 to about 60 rpm and rotating said impacting impeller at a tip speed from about 25 to about 50 meters per second;
c) Adding sufficient water to cause essentially spherical bauxite pellets to form;
d) Adding from about 5 to about 15 percent of additional bauxite powder by weight of pellets;
e) Rotating said impeller at a tip speed between about 5 and about 20 meters per second for from about 1 to about 6 minutes while rotating said table at from about 10 to about 60 rpm;
f) Drying said pellets at between about 100 and 300°C ; and g) Firing said pellets at sintering temperature until maximum density is obtained.
a) Adding bauxite powder having an average par-ticle size of between 0 and about 4 microns to a rotatable inclined table mixer provided with a rotatable impacting impeller;
b) Rotating said table at from about 10 to about 60 rpm and rotating said impacting impeller at a tip speed from about 25 to about 50 meters per second;
c) Adding sufficient water to cause essentially spherical bauxite pellets to form;
d) Adding from about 5 to about 15 percent of additional bauxite powder by weight of pellets;
e) Rotating said impeller at a tip speed between about 5 and about 20 meters per second for from about 1 to about 6 minutes while rotating said table at from about 10 to about 60 rpm;
f) Drying said pellets at between about 100 and 300°C ; and g) Firing said pellets at sintering temperature until maximum density is obtained.
15. The process of Claim 14 wherein prior to drying the pellets, the rotation of the impeller is stopped while the table continues to rotate for between 1 and about 5 minutes.
16. The process of Claim 14 wherein between about 0.2 and 1 percent of bentonite clay by weight of bauxite is blended with the dry bauxite prior to forming approx-imately spherical bauxite pellets.
17. The process of Claim 14 wherein said sufficient water comprises from about 17 to about 20 weight per-cent by weight of bauxite.
18. The process of Claim 14 wherein said rotatable impacting impeller is located at a position other than at the center of the table.
19. The process of Claim14 wherein the surface of said table is inclined at an angle of from 10 to 35° from the horizontal.
20. Spherical sintered bauxite pellets having a den-sity in excess of about 3.57 grams per cubic centimeter wherein repeated random samples of such pellets in-dicate an average sphericity of greater than 0.82 with 95% confidence limits.
21. Spherical sintered bauxite pellets in accordance with Claim 20 wherein repeated random samples of such pellets indicates an average sphericity of greater than 0.85 with 95% confidence limits.
22. A method for increasing permeability in a sub-terranean earth formation penetrated by a well where-in a fluid is pumped into the well to create a fracture therein, the improvement which comprises introducing a spherical sintered bauxite propping agent having an average sphericity greater than 0.82 and a density in excess of 3.57 grams per cubic centimeter into a fluid;
introducing said propping agent containing fluid into a fracture, the compaction pressure of which is at least 4,000 psi, to deposit a propping distribution of said propping agent, said propping agent having an average particle size between 0.1 and 2 millimeters.
introducing said propping agent containing fluid into a fracture, the compaction pressure of which is at least 4,000 psi, to deposit a propping distribution of said propping agent, said propping agent having an average particle size between 0.1 and 2 millimeters.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US96912278A | 1978-12-13 | 1978-12-13 | |
| US969,122 | 1978-12-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1117987A true CA1117987A (en) | 1982-02-09 |
Family
ID=25515210
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000339222A Expired CA1117987A (en) | 1978-12-13 | 1979-11-06 | Sintered high density spherical ceramic pellets for gas and oil well proppants and their process of manufacture |
Country Status (4)
| Country | Link |
|---|---|
| CA (1) | CA1117987A (en) |
| DE (1) | DE2948584A1 (en) |
| FR (1) | FR2450245A1 (en) |
| GB (2) | GB2092561B (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4632876A (en) * | 1985-06-12 | 1986-12-30 | Minnesota Mining And Manufacturing Company | Ceramic spheroids having low density and high crush resistance |
| US4680230A (en) * | 1984-01-18 | 1987-07-14 | Minnesota Mining And Manufacturing Company | Particulate ceramic useful as a proppant |
| US4944905A (en) * | 1984-01-18 | 1990-07-31 | Minnesota Mining And Manufacturing Company | Particulate ceramic useful as a proppant |
| US7036591B2 (en) | 2002-10-10 | 2006-05-02 | Carbo Ceramics Inc. | Low density proppant |
| US7654323B2 (en) | 2005-09-21 | 2010-02-02 | Imerys | Electrofused proppant, method of manufacture, and method of use |
| US7678723B2 (en) | 2004-09-14 | 2010-03-16 | Carbo Ceramics, Inc. | Sintered spherical pellets |
| US7721804B2 (en) | 2007-07-06 | 2010-05-25 | Carbo Ceramics Inc. | Proppants for gel clean-up |
| US7828998B2 (en) | 2006-07-11 | 2010-11-09 | Carbo Ceramics, Inc. | Material having a controlled microstructure, core-shell macrostructure, and method for its fabrication |
| US8063000B2 (en) | 2006-08-30 | 2011-11-22 | Carbo Ceramics Inc. | Low bulk density proppant and methods for producing the same |
| US8216675B2 (en) | 2005-03-01 | 2012-07-10 | Carbo Ceramics Inc. | Methods for producing sintered particles from a slurry of an alumina-containing raw material |
| US8562900B2 (en) | 2006-09-01 | 2013-10-22 | Imerys | Method of manufacturing and using rod-shaped proppants and anti-flowback additives |
| US9227874B2 (en) | 2011-01-25 | 2016-01-05 | Halliburton Energy Services, Inc. | Extrusion process for proppant production |
Families Citing this family (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2079261B (en) * | 1980-07-07 | 1983-06-08 | Niro Atomizer As | Process for the production of sintered bauxite spheres |
| US4440866A (en) * | 1980-07-07 | 1984-04-03 | A/S Niro Atomizer | Process for the production of sintered bauxite spheres |
| US4518039A (en) * | 1981-08-20 | 1985-05-21 | Graham John W | Method for treating subterranean formations |
| CH667223A5 (en) * | 1981-12-23 | 1988-09-30 | Alusuisse | METHOD AND DEVICE FOR ROUNDING DOWN GRANULAR SOLID PARTICLES. |
| US4522731A (en) * | 1982-10-28 | 1985-06-11 | Dresser Industries, Inc. | Hydraulic fracturing propping agent |
| US4658899A (en) * | 1982-02-09 | 1987-04-21 | Standard Oil Proppants Company, L.P. | Use of uncalcined/partially calcined ingredients in the manufacture of sintered pellets useful for gas and oil well proppants |
| US4623630A (en) | 1982-02-09 | 1986-11-18 | Standard Oil Proppants Company | Use of uncalcined/partially calcined ingredients in the manufacture of sintered pellets useful for gas and oil well proppants |
| US4427068A (en) | 1982-02-09 | 1984-01-24 | Kennecott Corporation | Sintered spherical pellets containing clay as a major component useful for gas and oil well proppants |
| DE3223024A1 (en) * | 1982-06-19 | 1983-12-22 | Battelle-Institut E.V., 6000 Frankfurt | METHOD FOR PRODUCING A SUPPORT |
| US5120455A (en) * | 1982-10-28 | 1992-06-09 | Carbo Ceramics Inc. | Hydraulic fracturing propping agent |
| US4548269A (en) * | 1983-01-03 | 1985-10-22 | Chevron Research Company | Steam injection well gravel prepack material of sintered bauxite |
| US4537254A (en) * | 1983-01-03 | 1985-08-27 | Chevron Research Company | Steam injection well gravel pack material of sintered bauxite |
| CA1217319A (en) * | 1983-02-07 | 1987-02-03 | Arup K. Khaund | Low density proppant |
| US4555493A (en) * | 1983-12-07 | 1985-11-26 | Reynolds Metals Company | Aluminosilicate ceramic proppant for gas and oil well fracturing and method of forming same |
| CA1228226A (en) * | 1984-07-05 | 1987-10-20 | Arup K. Khaund | Sintered low density gas and oil well proppants from a low cost unblended clay material of selected compositions |
| US4668645A (en) * | 1984-07-05 | 1987-05-26 | Arup Khaund | Sintered low density gas and oil well proppants from a low cost unblended clay material of selected composition |
| US4713203A (en) * | 1985-05-23 | 1987-12-15 | Comalco Aluminium Limited | Bauxite proppant |
| AU628700B2 (en) * | 1989-12-22 | 1992-09-17 | Comalco Aluminium Limited | Ceramic microspheres |
| BR0301036B1 (en) | 2003-04-29 | 2013-09-10 | suitable for hydraulic fracturing of oil or gas wells as well as method for reducing or eliminating the flow reversal phenomenon in oil or gas wells | |
| RU2344156C2 (en) * | 2007-02-28 | 2009-01-20 | Шлюмбергер Текнолоджи Б.В. | Proppant and method of well efficiency increase |
| DE102010007176A1 (en) * | 2010-02-08 | 2011-08-11 | Polysius AG, 59269 | Method for producing a refractory material from bauxite |
| EP3155064A4 (en) * | 2014-06-13 | 2018-03-07 | Imerys Oilfield Minerals, Inc. | Method of making proppants and anti-flowback additives using gear pelletizers |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3437148A (en) * | 1967-01-06 | 1969-04-08 | Union Carbide Corp | Method and article for increasing the permeability of earth formations |
| DE1592088A1 (en) * | 1967-06-01 | 1970-12-03 | Dynamit Nobel Ag | Process for the production of pressure- and abrasion-resistant balls |
| US3890072A (en) * | 1973-09-04 | 1975-06-17 | Norton Co | Apparatus for forming solid spherical pellets |
| CA1045027A (en) * | 1975-09-26 | 1978-12-26 | Walter A. Hedden | Hydraulic fracturing method using sintered bauxite propping agent |
-
1979
- 1979-11-06 CA CA000339222A patent/CA1117987A/en not_active Expired
- 1979-11-22 GB GB8205575A patent/GB2092561B/en not_active Expired
- 1979-11-22 GB GB7940365A patent/GB2037727B/en not_active Expired
- 1979-11-23 FR FR7928939A patent/FR2450245A1/en active Pending
- 1979-12-03 DE DE19792948584 patent/DE2948584A1/en not_active Withdrawn
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4680230A (en) * | 1984-01-18 | 1987-07-14 | Minnesota Mining And Manufacturing Company | Particulate ceramic useful as a proppant |
| US4944905A (en) * | 1984-01-18 | 1990-07-31 | Minnesota Mining And Manufacturing Company | Particulate ceramic useful as a proppant |
| US4632876A (en) * | 1985-06-12 | 1986-12-30 | Minnesota Mining And Manufacturing Company | Ceramic spheroids having low density and high crush resistance |
| US7036591B2 (en) | 2002-10-10 | 2006-05-02 | Carbo Ceramics Inc. | Low density proppant |
| US7678723B2 (en) | 2004-09-14 | 2010-03-16 | Carbo Ceramics, Inc. | Sintered spherical pellets |
| US7825053B2 (en) | 2004-09-14 | 2010-11-02 | Carbo Ceramics Inc. | Sintered spherical pellets |
| US8216675B2 (en) | 2005-03-01 | 2012-07-10 | Carbo Ceramics Inc. | Methods for producing sintered particles from a slurry of an alumina-containing raw material |
| US7654323B2 (en) | 2005-09-21 | 2010-02-02 | Imerys | Electrofused proppant, method of manufacture, and method of use |
| US7828998B2 (en) | 2006-07-11 | 2010-11-09 | Carbo Ceramics, Inc. | Material having a controlled microstructure, core-shell macrostructure, and method for its fabrication |
| US8063000B2 (en) | 2006-08-30 | 2011-11-22 | Carbo Ceramics Inc. | Low bulk density proppant and methods for producing the same |
| US8562900B2 (en) | 2006-09-01 | 2013-10-22 | Imerys | Method of manufacturing and using rod-shaped proppants and anti-flowback additives |
| US7721804B2 (en) | 2007-07-06 | 2010-05-25 | Carbo Ceramics Inc. | Proppants for gel clean-up |
| US9227874B2 (en) | 2011-01-25 | 2016-01-05 | Halliburton Energy Services, Inc. | Extrusion process for proppant production |
| US9862879B2 (en) | 2011-01-25 | 2018-01-09 | Halliburton Energy Services, Inc. | Extrusion process for proppant production |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2450245A1 (en) | 1980-09-26 |
| GB2092561B (en) | 1983-10-05 |
| DE2948584A1 (en) | 1980-06-26 |
| GB2037727A (en) | 1980-07-16 |
| GB2092561A (en) | 1982-08-18 |
| GB2037727B (en) | 1983-05-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA1117987A (en) | Sintered high density spherical ceramic pellets for gas and oil well proppants and their process of manufacture | |
| CA1232921A (en) | Particulate ceramic useful as a proppant | |
| US4658899A (en) | Use of uncalcined/partially calcined ingredients in the manufacture of sintered pellets useful for gas and oil well proppants | |
| KR101501293B1 (en) | A composition and method for making a proppant | |
| US4944905A (en) | Particulate ceramic useful as a proppant | |
| US4879181A (en) | Sintered spherical pellets containing clay as a major component useful for gas and oil well proppants | |
| US4623630A (en) | Use of uncalcined/partially calcined ingredients in the manufacture of sintered pellets useful for gas and oil well proppants | |
| US4427068A (en) | Sintered spherical pellets containing clay as a major component useful for gas and oil well proppants | |
| US4894285A (en) | Sintered spherical pellets containing clay as a major component useful for gas and oil well proppants | |
| US7067445B2 (en) | Extended particle size distribution ceramic fracturing proppant | |
| US20070023187A1 (en) | Sintered spherical pellets useful for gas and oil well proppants | |
| US8420578B2 (en) | Low-density ceramic proppant and its production method | |
| US8603578B2 (en) | Composition and method for making a proppant | |
| CN104031632A (en) | High strength ceramic elements and methods for making and using the same | |
| US8283271B2 (en) | High strength proppants | |
| EA012634B1 (en) | A composition and method for making a proppant | |
| MX2014004760A (en) | Porous proppants. | |
| WO2016149133A1 (en) | Methods of making proppant particles from slurry droplets and methods of use | |
| CN107109919A (en) | The proppant particles and its application method formed by slurry drop |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry |