CA2136009A1 - Process and apparatus for producing granules from powdered material - Google Patents
Process and apparatus for producing granules from powdered materialInfo
- Publication number
- CA2136009A1 CA2136009A1 CA002136009A CA2136009A CA2136009A1 CA 2136009 A1 CA2136009 A1 CA 2136009A1 CA 002136009 A CA002136009 A CA 002136009A CA 2136009 A CA2136009 A CA 2136009A CA 2136009 A1 CA2136009 A1 CA 2136009A1
- Authority
- CA
- Canada
- Prior art keywords
- fluidised bed
- flat jet
- bed apparatus
- fluidised
- jet nozzles
- 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.)
- Abandoned
Links
Classifications
-
- 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
- B01J2/16—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
-
- 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
- B01J2/003—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic followed by coating of the granules
-
- 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
- B01J2/006—Coating of the granules without description of the process or the device by which the granules are obtained
Abstract
Abstract The specification describes a process for the build-up granulation of a powdered material in a fluidised bed apparatus, in which the granulating liquid containing a binder is sprayed into the fluidised bed of material to be granulated, the liquid being sprayed on to the fluidised bed from above, in counter-current to the gas producing the fluidised bed, by means of two-component flat jet nozzles. With batch sizes on an industrial scale, i.e. about 1000 kg, very uniform and dust-free granules can be produced in this way.
Description
1~1 N~V '94 1:3: 34 GOERTZPf~TENT P. 3/4 6 ~ (~ 9 ~.
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~ne in~ention r~te~ to a proce~ ~or build-up l~tlo~ or a powd~red ~uterial and~o;c the ~oat~ of granules in a fluidl~d b~ with a bin~r con~ained in a gru~ula~ing liq~ rhe~e~n the IQateriai io ~lU:IdlYH~ ~n a rluidl~ appA~tUS lDy ~lea~18 ot ~ g s cur~crlt ~ :
blowa ln ~ra~l 4elo~ thxough ~ at~d ba~ Qa~
ln part~ of th- ~ullc of t~ mat~rl~ he gras~ula~ln3 J.iquid :LB ~pr~yed into ~luidi~ os~e~ of th~ lal. ~ ention furth~r r~lat~ss to ~n ~pparatuu tor c;~r~ying out uueh a proce~
P~ eutical can~osition~, ~eed a~diti~ a~ ~th-3r : ~ :~
~r-~duct~ a~e rr~ tly obtain~d, at t~e end o~ the -aanu~cturi~g groc~ itsol~, a~ a ~wder or pocr~er :~
mlxture of a ~c~ecific ~rticl~ ~izc ~tril~utlon. ~n a produ~t w~ich i6 che~c2~llr or ln w~e oth~r way s2ecifically ~ulted ~!or a partl~ r use n~y occa6io~a11y fall to de~elop it~ u11 activity u~sder praetic2~1 ¢onditio~6 or ~ay be r~tri¢te~ in h~ndllng quali~ie6 i~ it i~ not p~eserlted in a ~uita~
ext~rnal ~nn. ~ne eolutlon to p~o~l~ of in~deguate ~ --ch~lcal rcs~lst~nc- ar ha~rdo~l8 h~llng ~t a powd~rad ~aterlal on t~e ~ou~ or dust ~onDaeion may ln certaln ca~ con~ifit ~ s~ ulat~g the po~dered mat~ar~al an~
:j optlon~lly ~1180 coati~ th~ ~ra~ula~e partic~ea w~th prote~ti~ stanco ~hich ha~ no lahe~rent d~A~ 5CkD.
13P-A-165 5`7~ ibeE, in t~ ca~e o~ a feed ~dditi~e ;1. cont~inl~ ~inc baoi~rao$n, ho~ tion c~n tantially i~pr~ he c~e~u~l ot~ility of a f~d s a~d~tive of ~hi~ klud ~ a feed ~turd~ ~o pr~f~rrad :
~ethod o g~a~ulstion ~ro~os~ad accordi~ eo R~A-1~5 577 the u~e o~ a ~luidi~e~l b~Kl gr~ul~tor in which the ~I po~dered atartlng ~terial i~ plAc~d ~sd, ~tar a di8ed be~ ha~ bec~ p~ duced by blo~issg a g~ curr~nt :
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~0 NOV '94 1~:34 GOEi~TZPRTEl`lT ~;J ~ 3 ~ ~ Q 9 P ~
throu~ ~ ~erf~r~eoa ba~e on which ~h~ ~t~rtirlg -;
t~ce r ~B, ~ yranulacirlg ~ ~r~ into e~se flu$diced b~d by meaI~u o~ ~pr~y ~le~, ehi~
contain~ 10~ by wel~t o~ a oult~le blndQr, isl :
solution or ~usp-n~ion, which wlll br~ng about lncrea~d aggla~r-tio~ o~ t~ po~red ~aterlal to ~orr~ gr~ les ~nd fi~Ally co~ tl~e g~a~ul-0 ~lt~ a ~rotectiv~ ~:
layer.
Wh~rea~, ln the ~ ect ~atter o~ ~SP-A-~ 6$ S77, the eseential a~acelve wa~ to i~nprove thc ch~lc~l ~ta~ y o~ a ~sod ~tdlel~ co~ta~lng z$nc ~cit~acin in a ~e~d ~ tu~e, BP-A-3~2 ~62 ~cribe~ pro~l-d graslulat~ng proc~D~ for ~-~d a~t~Yo~ 1~ g~2~0ral, wher~in a BlOtt~l ~yro dy~ uc filter granulating apya~atu~ l~ u~oa ~or tho g~ulat~o~. An ap~aratue o~
t~6 kln~ doecri~e~ ln Dl~-A-29 3a ~03, to which re~erence ie aleo made ln BP~ 02 462, ~, ln ~omewhat dl~ore~t e~bodimeAt~ in t~ late~
~p-~-331 lll. ~ i~ a ~luidlsed ~ed appar~tu~ ln whlch, unaer~eat~ t~e periorated ~a~-, ln tho ~in~
ahamber, th-ro i~ ~ rotor whleh only alloY~ the fluidi~ln~ ga~ to be ~lo~n ~n in certsin radlAlly ext-~ndlng ~on c ~1~ ~ce ~lorly a~ n re~ult of eho ~otati~ o~ th~t ro~or, ~o that fluidised bed ar~ can o~ly fc~nn in cert~ Hctor~ a a~oa~
~lowly th~ h ~he bulk o~ th~ ~aterial.
..
Wh~r~a~t, in the apparatus ae~ord~ng ta DB-A-29 32 hO3, thare i~ only a single ~pray no~zl~ arra~gel~ centrally abo~ th- p~rforate~ e to spra~ the coatlng o~
g~ulating liq~id into the ~lu~dls-ld hed ~ran ~el4w, lr th~ appas~tw aoao~i~g to ~P-A-33t 111 th~ro ar~ radial ar~6 pro~ ~e thes perfo2~at~d ba6~, hur$n~ n~lly direcCed ~pray no2zle6 ~-hiah rotat~ ~yncl~ronou~ ith the Ylo~cte~l gyro rotor, fiO that ~h~y ~gr~t~ r ~ith tho tlui~ e~ bed ~one8 ~ ~;~ray the grA~Iula~g ...
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';~. , 09 l~O~ '94 12:42 GOERTZP~TENT r 3~ 3 6 0 0 9 P.~/22 -- 4 - :
llquid into th~m f2~ b~low~
13P-~-30~ 4S2 describes, ~al~ ~aking the ex~le of a ~-fo~d addltlvo co~t~l~ln~ zlnc ~a~ltracin, ho ~ t~e gra~le~ ~oduc~ 1~ t~e ~lotte~ gyro f lu~ ~lse~ ba~
~p~ u~ ot only h~ re~ bo~ter c~e~ical ~td~illty Pu~ also a very narrow aA~ even p~rticle ~ize di~tr~ution of the g~ules, which conta~n ~art~ly any :~
o~or~izad partlGl~ and ax~ virtually ~reo ~ron~ du~t.
~o du~ producod ~ ~ abra~lon test, moroo~ror, contai~c h~rdly ~y o t~e uct~re ~ubst~e, ~lnc bac~tr~ci~ .
As i~ eleA~ ~r th4 e~odl~ents by vay o~ axan~le in EP-A-302 462, S~atche~ o~ ~tarting r~aterial Qf the order o~ 3 lcg w~ro proces~ed. P'c~ed ad~lti~ves ~re ~e~t 1~
t~e~. ~o e~blo eco~ ical pro~uction lt 1~ deslrable ~o ~rotluce g:c~nules iJ~ aloountl~ rang~ng ~rom 00~teral h~ndred l~llograT~ up to o~e to~, ~rhe alm o~ the inv~ntic~ to provl~e a proce~ for bull~-up granulaticn of powd~red ~c~rlal and a suitabl~ :
apparatus uhich 1111 pro~uce, mo~e particularly on an i~strial eeale, wi~orm ~nd ~ub~t-ntlally ~u~t-~ee g~:~ulo~ which ~orr~ o~d i~ t~eir propertie~ to th~3 reiaulw gl~ A-302 462.
It i~ ~ie~ll ks~own 'c~ ~ho~e ~klll~ the a~ i~e tho ~lo~r CharAC~eristlCs o~ tances d~ ignlitcantly on tl~e ex'ce~nal co~ditlon~ a~d al~o on th~ appi~r~tu~
uis~d. Tlliis ali~o i~pplies in ea~h C~ to gr~nulating ~roc~ss~ u6inSI ~luld~e~ bed æp~aratu~. The ~p~ri~nts ~ere c~rried ~ut ~ith a ~lul~lsed be~l a~paratu6 app~imately Z ~ in diamot~, tho ~tches of powelere~l mate~lal we$ghing abo~t 750 kg, 1~o~ 2r, it il~
as~umed that t~- re~ult~ sc~l~v~ can al~o b~ :
tra~ rred as~logou~ly to 4pparaeu~ o~ di~rent orders ~ .
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09 NO~ 'g4 12:43 GOERTZP~rENT ~ 1. 3 6 0 0 9 s~
of magnitude. ~e e~ri~snts were aloo ca~ d out in thi~ in~an~ ith ~ ~e~ ad~ti~ ont~ in~ zi~c bacltracir" th~ co~ ition and vt~er c~d~ tlon~ o~
whic~ casl be ~cund in l~P-A-165 577 asb~ l~P-A-302 462, to . :~
w~ich re~erence ~e ex~?re~ly ~e. Blres~ ~houg~ the ~xperln~t~ carrie~ out were inten~e~l prim~rlly fo~
granula~ln~ a f~d addit~e ~ontalning 2inc bacitr~c~n on an ln,~!lu~ial ~cale, with ~cl~lc gi~en prapor~$eo, ~e presenc l~lv~elon i~ not restricced to a fe~
additi~re o~ thi~ klna but 1~ s~en~rally sultablo ~or the gra~uldt~n o~ powde~ed mater~al, the ~r~i~g m;~t-ri~
and g~anulating liquids bel~S~ aa del~crlbed ~n ~P-A-302 ~.6a, to whlch re~erence ~ ~re~cly ~do ~or tbi~ rea~on.
Other s~tanc~- o~ partic~lar lntere~ a~e ~aterol, sputolyeille, bi~olvone, ~ lnia~cln, ~lo~ln, ~plr~mycln, no~ihe~tld~, p-nic~
chloroto~r~cycllrl~, ooyteeracycllns~, t~tracycl~ne6, e~thronyclr~, furazolidone, nitro~uran, thrl~etho~rir~, ~ull?honalnlde~, dlnultrid~zole, neo~yci~ base ~nd all vitamln~ w~ieh aro pk~rmacoueic~lly accol7ced or allowffi un~er ~cod r~yu~loDY, suth aJ ~ta~n A, a~, A~
B~ , B~ C ~a~corbie ~cld), aocor~ylpalmlt~te ~n~
ot~or ph~rs~colog~cally accept~ble dsrivatlv~
a~corb~e acid, D, D~ , D~, r~ , x, ~L~ Xa, ~ and - or act~vo ~ub~t~nc~6 6uoh a~ ~voparai~, flavopholtpol, ~on nsin, ~nensi~-~odiu~, salin~yci~, carbadox, nitrovln ~nd olaguinoox.
~he ob~oc~ive o~ impro~g a ~oc4~a o~ th~ type de~cri~d ~Yelnbeforo i8 aChleved aaeo~di~ to the in~enti~ i~ th~t the granulati~g li~u~d i~ ~p~yed int~
fluidi~ed ~ane~ ~f ~he ~aterial by ~ea~s o~ fl~t ~et no~zle~ ~r~m ~bov~ th~ ~lui~i~ed bel, ~b~tantial.ly in co~nt~r-cur~ent to the ga~ cur~e~t which ~orm~ th~
~luidl~d bed. ~ ~luidi~ed ~e~ apparatu~ ~lch i~
}
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0~ NOV '94 12:4~ GOERTZPRTENT ~ O O ~ P.4 wi~a~le for per~ormlng the proces~ according to the ~ n~r~nt~ on i~ a~eortlingly cha~acteri~ed ~ ~ tbat t~ cpray nozzle~ ueo~ are ~lat ~t ~ot~le8 w~ arr~ng~d ln an upper part o~ the concal~ whic~ hen th~ a}~p~r~tu~
i6 operates~ a~ lnte~ ~ ve the flui~18ed bed ~o~d, ~ the~e ~lat ~et no~le- ~re Cl~rected ~o that ~ch~lr directlon of ~p~:aylns 1~ tant~ally dO~Ilw~B
tot~rd6 th~ idi~Cd bed, On an in~u~trial ~calo, ~ g a larger appa~atu~, lt ha~s ou~d that ~pr~ying the gra~ul~ting llquld in f rom below, i.e. ~rom the per~or~-ted b~ upwara~ ~nto tbe ~luid~ sod ~Lto~ial ~on~ riou~ly not ~h~ optlmum ~athc~d, ~rtlcula~ly i~ a ~l~ldi6~d X~ hno b-en l'ormod only in c~ in ~re~c, as ~ith '~he ~lott~d gy~o n~hod, the 1~id~1ng g~ ~ppo~r~ to c~ey up th~ granulati~ .
llqu~l whio~ ha~ be~ blawn in in ~arallel, ~o tllat lt doe~ not come ~nto optim~m Contact with the ~rial which 1~ to b~ agglos~erated. Ih~f4ro, it h~ pro~red more ef~ectlvR to spr~y the g~:~nul~tl~g liquld in ~rom :
abo~a, ~o tO 6pQak i~ counter-curre~t to ~ho fluid~ng ~as, into th~ ~uldls~d area~. ~o b~it r~eults were o~t~lned ~ith ~lat jet no~zles ~hic~, in ~ ca~o o~ a con'cainer of cirC111ar cro~6-Gectio~, aru p~eS-r~bly ali~d ~o th~t tho clongate ~u~ace co~ered b~ the j~
~ tlth ie~i 104g ~i~ ucis ~ tan~lally il~ t2~e di~ectiol~ o~ a radluY of the ~ppa~atu~.
The ~o~t e~octi~lr nozzl-~ ~avo ~r~re~ to b~ l:Wo-c~qpo~ent ~lat ~et lloz21e~ w~th ~xte~ lxing, whe~e~n, a~ter lea~g th~z nozzle, the liquid ~h~h i~
to b~ ~praye~ a~on~ced ~y a~ a7~ia~ e c~rrent ght ~r~to t~o desire~ jet ~o~m~ ~e s~e~iaoni~ for th advan~ageou~ e~ect o~ t~ese nozzle~ has no~
hitAer~o ~o~n expl~tnea i~ deta~l but 1~ i~ pre~
that, ln ~te o~ ~e ~ e3Wre o~ thc ;, at~i~lng g-s, a ~oft, ~ell di~ribut-d $et i~ produced :~ :
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09 ~IOV '94 12:44 G~)ERTZP~TENT ~ ~ ~3 6 0 0 9 P.5~2 wieh ~ t1 tlyna~ic ~hich produce~ a ~articula~ly even aSIglom~ratio~ e~ect i~ conjunctio~ with t~o fluidlsed po~ered mat~rl It ha~ been ~ nd tl~at, ~ uit~ble r~unber o~
~l~t ~et u~>~210~ are dl~rlbuted over ~ fluidl~ed Ped, it i8 ~10 lon~e~ ne¢e~a~y ln ge~eral to u~ th~ ro~atlrlg ~lott~d gs~ro, i~e. ~co produ~e llmited ~luidi~e~
~ea~ $eh rotat- ~lowly throu~h the ayparatu~. Gooc~
rosultE are Achiev d almo~t to the ~me extent with a perf~r~ted ~ hich i~ lly ac~ed upon by ~uidising gas. Mo~eov~r, lt i6 not absolutely e8~ntial to have thH ~l~t ~t nozzle~ ~l~atl1ag o~rer the rluldloed bo~, althou9h thl6 le ~I pre~erred e~odi~nt of tho pxoc~
according to ~h~ l~v~ntion. Whet~er t~AiB ~ea~ur~
nece~sary depend~ o~ the on~ han4 on the nun~er and diotr~butiorl o~ the ~c~z7cl~ n the t~th~r h~nd on the dyna~Dle6 ~ th ~lui~i~0d b~ t hals b~ aund ~bat, e~e-~ with ~cationa~y ilat ~ot ~0221es which ccnrer only a~o~t ~2~ of the surface ~ fl~lid4~od bed, ~ln~form g~:anule~ O~ o ac}~d. r~e dur~tlon of ~pr~ying and ~h~ recirc~lati~g ff~ct in ~he ~lui~i~ed b~d pre~ably cont~ibuto to th- ~e~ult- o~ tho proco~.
rhe choic~ o~ the nu~e~ o noz~eo i~ t~ot ~re~ ~ ac 7nu~h aH ~ ll~ted ~ounS o~ lating liquld ha~ to b~
~prayed i~to a ~tch of m~Co~ d the opray~ nwst ext~s~d over a cert~in l~gth o~ ti~ in o~der to achieve ~low a~lo~eratlo~ and gra~Ulatlon, w~llst tS~e ~luldis~ng ~as nsu~st al~o bo rl i~ pt~-itlon to ~ ~ove the ~olvene or 1;ll6pe~l6ion ~gen~C rrO~ the gr~nulating liquld.
Sln~ on the other h~nd the rLo~ s u~e~l r~8t have a ~pecl~c amount trarolliD3 t~rougb. ~chom~ lt il!~ no~
ble to ~pr~ ~h~ e~t4re ~rfa~e o~ t~ luld~ed bed. P~e~er~ly, ~ceos~ to the invelltion, ~t ~y ~ne :~
tim~, o~ly ~bou~ 2S~ oS cb,e ~ur~ace o~ ~h~ Sluidise~
b~d iB cov~r~d by tha ~pray ~et~ o~ the no3~1~8. T~i~
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09 NOB '94 12:45 GOE:~TZPPITE~T ~ ~ 3 6 o ~ ~ P ~/22 ---~ac~c may ~ke iC neoeli~ary to allo~ the s~ozzle~ to ~grato o~ver th~ ~ idl6ed bet or ~otato, tc~ achiev~ -~ett~r ~pray distribution.
Generally, ~.5-30~ ~y wel~ht, pre~erably 5-~0~ by we~ht, ba~ on t~e ~in~he~!l 0ra:t~ule~, o~ btn~er will b~ introd~o~d into the product, ~ho gr~ulating liquid beiny a 1-30~, pref~ly 2-10% and more e~peclally 5-7~.
~oluti~n or ~u6ponBio~ of the bindRr ln one pa~ticular nl~eer~ti~e enbod~ t o~ the prooet~
it iB po~61bl~ ~lr~t to rpray tne ~ure accl~ t~ce on ~co th-~ carrlor m~t~ial and to ooat it wlth ehe ~oating ~ater~al ~n a c~co~d ~tep. In t~iJ alternati~
emb~llm~nt the ~opo:ctloP. ~ w-ight or ac~ re sub~ta~o `19 ~s~eon 0.01 and 30~ ~y ~e$ght, b~oe4 on th~ ~lni~hed e~, d-~endlns~ on th~ p~nnacologlc~l act~rity o~
~he active sub~t~ce. Tho active o~tas~ce m-y b~
~p~ayed on i~ t~e ~o~ o~ ~ ~olut~o~, ~or ~le ~ o.o ~o 30~ ~y Yelg~t ~olution, o~ ln th c~e Or 1 colu~ ctl~e ~ubat~nce~, ~n t;he ~or~ o~ a Bu~pen~
Whe~n ~d~uctlng th~ concentr~tion of thll ~olutlon co~tainlng the ac~cive ~u~st~ce, o~viously the nature of th colven~ and th~ 80~ $ty 0~ the acti~e ~b~tanee ~ th~ ~olYe~t ~u~it be bon~e ~n minO
Ihl- altern~t~e e11ibodl~t 1~ o~ p~rtlcular inte~e~t -~
~rlt~ i~ly acti~e Bu~st~Ces 6~ch a~ cle~buterol o~
~putoly~lsle . 8xan~pl~ of carr~ er~ include ln~ Aic ~a~lar~ ~uc~ aB calcium car~onat~ or dicalcium pho~phat~ nt ~lef of org~lc car~l~s~ inclu~
9U9'E!ISB I~UCh ~1~ lacto~e, la~to~-cor~ ~tarch or ~accb.aroce~ but al~o ~or~itol.
In the ~rime~t~ c~ d out ~Ith tho ~ee~!l ad~el~ e, o~au~ 5~ o~ methyl c~llulo~o, l:~Ee~l or~ the fl~i~h~d :-~remul~, were used, the granulating liguid boins a 5 ,;
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"'~' ' . : ~, ., , ' El9 l`lOV '94 12:~5 GOERTZPflTE~T 2 ~ 6 0 ~) ~
aquaou~ ~olution o~ Che tnothyl clellulos~. Ot~r coat-lny ~a~erial~ a~e p~soible, a~ di~clo~ or exa~ n P-A ~65 s~7 E~nd 302 4~2, to whi~h re~e~ence i8 ~de.
o~ p~rticulAr ineorest, apart ~rc~ thyl cellulose, are ~ydroxypropyl call~lo~e, ~ydro~ypropyl~et~yl aellulose, polyethyle~ly~ol ant w~te~ oolubl~ 6taxch.
With a bi~d~r c~nton~ ~f 5~ ~ S~ 801utl0n, the total a~ount of gra~ t1ng liquid 1~ litre~ corro~pon4 ta~tlally to '~h~ weight in l~g o~ the po~red mataria~. ~peclf i~ . ~rl o~der to achleve good r~ul~6, thi~ quantlty of~ d wa~ pref erably ~prAy~d ~to the ~luidis6d ~d over a ~eriod of 3 to 4 hou~
ty o~ r U~Lit of tim~ ~oed n~ n6~e~sarily be kept Conatant throu51hout the e~tire ~pr~yi~g tl~.
Inaeed, rather more liqui~ may b~ ~p~ayed at th~
beginning o~ the proce~ d r~thsr le~ tow~r~l3 the en~. ~ith a ~ant~ ~y o~ about 1 litre o gr~nul-ting li~aUi~ per Iy~ o~ po~dero~ ~ter$~1 and a ~p~-ying ti~
o~ ju~t 3.S hour~ a~rerage ~pray gu~ntity ~r un~t tl~ of c~nly ~out 5 ~lJk~ of ~tartlny ~aterlal y~r m~ute i~ o~tain~ . It fOlloWC f ra~ tl~t the s~ray density on the to~ o t~e ~luidiBed bed casulot be mal~ta1ned at a v~ry high l~el.
rwo~ c~ ~lat ~et no~zl~ ~ult~lo ~or the proeeca w¢o~diny to th~ tion are 801~ OF ~ple, by t~e i~
compa~y 9pr~2~g Sy~te~. ~ te~t~, o~ ~o~zl~ ~de by thiw co~pa~y, ~ring tho name S'.JB 4S as~ ~a~ing a 3~ay angle o~ ~S^C prolred st~ltabl-, ~ ~. ~t:ord~ eo t~e ~eciricat~an o~ t~ ct~rer thiB no~zl~ ha~ a liquid through~ut of 4.7 l/~ ~o~ ope~ation ~itb w~ter a~ ~ ~lu~d pressu~ ~f 1.5 bar and an air pre~2re o~
a~out 6.0 ~ar. At a liquid i~let pres~ure o~ a.7 b~r ~nd an air ~res8u~e of S-6 bar, ~he wa~er t~ rough~ut ~all~ to 3.2 l/~in. ~:n the Ca~e of ~igl~er ~rlscs:~ity ' .".
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~ ~,36009 09 NO'~' '94 lZ: 46 GOERTZPhTE~T P. B/~Z
~- ~ O -- , ll~ui~ ah a~ th~ g~a~ulating liqui~ ln~rol~o~ h-r~, ~e llqu~d th~o~gh~ut of the n~zzl~ iG I~Ubet~t~ally le~e. ~q~e vi~c~ity ~ ~h0 li~ ay ;!113C~ be a~fecte~
by its t~peratu~. It ha~ bo~n ~o~d t~at the nozzle~
operate cati~factorily wit~ t~ granu~acis~ if the vi6co~i~y of the liq~d 1~ ~d~u~t0d So t~ult nc~2zleu ha~e a throuy~u~ wb,lch 1~ 0.1-0.3 tlm~, pre~!-ra~ly a . 12-O .111 tioU~E t~o ~anis-al chroughput with water~ Prefera~ly, the nozzle~ ax~ O~o~ted at ~
pr~s~ure of a'comiei~g gaE~ of ~etw~n 2 a~d 6 ~r. ~rhe tluld pr~ure 1B d~ten~ by th~ ~lred t~lro~gh~ut o~ tho 51O~ t lDay ~a~ t~ on 0.7 ant~ 3 bar ~n~ 10 fl~r~bly l:~et~e~ 1.2 ~nd l.t bar. ~t~th a 5~ hyl cellulo~e ~olutio~ h~ rlng ~ een~peratu~e o~ 30'C, the ~hr~u5~1?ut ~lth th~ ~ove-~tioned no2~1e t~pe ie a~out 0 . 6-1 . 4 l/~i~.
I)ependi~g on the ~pacing o~ suc~ A nozzle ~orn the sur~ace wh~ch 16 to ~ ~pray~d, ln thi~ caoe the theo~e~ical ~urfac~ of tl~ ~luid~3-1d ~ed, ehe noz~
oprayr ~ Crea o~ 15~-7~0 c~2, ~, ep;~zlyin~ a~-a o~ bet~een 500 ~nd 70D c~n' belng p~otorred, for ~hich t~ ~r~ge 6p~Ci~g Or the no~zle from ohe sur~ac~ to ~o ~;pr~,yed i~
~ou~ 70 c~. ~ha pre~erred ~pray d~ity, ba.~ed on the are~ ~ceually ~pra~ed, i~ preroral:~ly betwee~ d i 15 l/~.~.
~ha spr~ er ~ Q l~dl~rldu~ zzle~ l th~
;5~tl ty of gr~ulat~ liqui~ ~o b~ eprayed E~er u~
t~me will g~e th~ nu~r of s~ozzleæ r~quired, once a cific nozzl~ t~rpe has b~ o~e~, whil~t ~he ~rertic*l arr~ ement, iXI l?articul~r, wlll proauce t~e pr~orre~ ea to b~ sp~e~l. I~ the ca3e o~
;-~app~r~tu~ c~rclllar cro6æ-sestlon tl~e noz~ ar~
pre~er~ly arra~ged BO that thel~ op~aLy ~.rea~ exe~n~l radially ~nd are u~i~ormly ~paCe~ ov~r t~e p~riphQry the~eof. ~ the le~gth o~ t~e ~pray ~roa o~ a nozzle la J, .
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04 NGV ' 94 12: 46 GC~;~TZP8T~lT -- P . 4 'Z--more or 1~ t cie~t to Co~rer t~e rad~ u~ of a con~cainer, a ring o~ nozrles is ~refe~&bly u~e~, the r~o~zle~ b~ing ~p~eed f~e~ the centre ~ C roughly half th~ l~h of c~e ra~iu~. In ~;he ca~e o~ A cor,tainer it~ a dla~aeter o~ 2 m, for e~l¢, ~ood ~el~Ult6 were ac~ uith aix noz~lo~ a~ra~g-~l ~ ~io way a~d distribue-CI o~er ~h~ ciroumi~r~oe. Ft~r larger ~ontai~er di~ter~, a l~ger sstlnber o~ no~lac may 2:~a ~equtred, ~nd th~e ~oz~le~ t~ey do ~ot co~er ~ t the e~tlre le~s1th of t~o rad$u~ o~ a cos~t~iner, chould be ~ ltnrs~tely a~ ere~t ~pacin~ fra~ the c~nt~e of the Container i~ ~uc~ a ~y t~a~ ehe m4~t mlfonn ~pr~y d~it~ibution po~ible i~ a~i~ved over the ~luldi~ed ~atd.. Bao~ on the ~otal ~ur~ac0 ~rea o~ t2~o ~luidi~e~ bed a ~pr~y de~lty of betv~
~ne in~ention r~te~ to a proce~ ~or build-up l~tlo~ or a powd~red ~uterial and~o;c the ~oat~ of granules in a fluidl~d b~ with a bin~r con~ained in a gru~ula~ing liq~ rhe~e~n the IQateriai io ~lU:IdlYH~ ~n a rluidl~ appA~tUS lDy ~lea~18 ot ~ g s cur~crlt ~ :
blowa ln ~ra~l 4elo~ thxough ~ at~d ba~ Qa~
ln part~ of th- ~ullc of t~ mat~rl~ he gras~ula~ln3 J.iquid :LB ~pr~yed into ~luidi~ os~e~ of th~ lal. ~ ention furth~r r~lat~ss to ~n ~pparatuu tor c;~r~ying out uueh a proce~
P~ eutical can~osition~, ~eed a~diti~ a~ ~th-3r : ~ :~
~r-~duct~ a~e rr~ tly obtain~d, at t~e end o~ the -aanu~cturi~g groc~ itsol~, a~ a ~wder or pocr~er :~
mlxture of a ~c~ecific ~rticl~ ~izc ~tril~utlon. ~n a produ~t w~ich i6 che~c2~llr or ln w~e oth~r way s2ecifically ~ulted ~!or a partl~ r use n~y occa6io~a11y fall to de~elop it~ u11 activity u~sder praetic2~1 ¢onditio~6 or ~ay be r~tri¢te~ in h~ndllng quali~ie6 i~ it i~ not p~eserlted in a ~uita~
ext~rnal ~nn. ~ne eolutlon to p~o~l~ of in~deguate ~ --ch~lcal rcs~lst~nc- ar ha~rdo~l8 h~llng ~t a powd~rad ~aterlal on t~e ~ou~ or dust ~onDaeion may ln certaln ca~ con~ifit ~ s~ ulat~g the po~dered mat~ar~al an~
:j optlon~lly ~1180 coati~ th~ ~ra~ula~e partic~ea w~th prote~ti~ stanco ~hich ha~ no lahe~rent d~A~ 5CkD.
13P-A-165 5`7~ ibeE, in t~ ca~e o~ a feed ~dditi~e ;1. cont~inl~ ~inc baoi~rao$n, ho~ tion c~n tantially i~pr~ he c~e~u~l ot~ility of a f~d s a~d~tive of ~hi~ klud ~ a feed ~turd~ ~o pr~f~rrad :
~ethod o g~a~ulstion ~ro~os~ad accordi~ eo R~A-1~5 577 the u~e o~ a ~luidi~e~l b~Kl gr~ul~tor in which the ~I po~dered atartlng ~terial i~ plAc~d ~sd, ~tar a di8ed be~ ha~ bec~ p~ duced by blo~issg a g~ curr~nt :
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~0 NOV '94 1~:34 GOEi~TZPRTEl`lT ~;J ~ 3 ~ ~ Q 9 P ~
throu~ ~ ~erf~r~eoa ba~e on which ~h~ ~t~rtirlg -;
t~ce r ~B, ~ yranulacirlg ~ ~r~ into e~se flu$diced b~d by meaI~u o~ ~pr~y ~le~, ehi~
contain~ 10~ by wel~t o~ a oult~le blndQr, isl :
solution or ~usp-n~ion, which wlll br~ng about lncrea~d aggla~r-tio~ o~ t~ po~red ~aterlal to ~orr~ gr~ les ~nd fi~Ally co~ tl~e g~a~ul-0 ~lt~ a ~rotectiv~ ~:
layer.
Wh~rea~, ln the ~ ect ~atter o~ ~SP-A-~ 6$ S77, the eseential a~acelve wa~ to i~nprove thc ch~lc~l ~ta~ y o~ a ~sod ~tdlel~ co~ta~lng z$nc ~cit~acin in a ~e~d ~ tu~e, BP-A-3~2 ~62 ~cribe~ pro~l-d graslulat~ng proc~D~ for ~-~d a~t~Yo~ 1~ g~2~0ral, wher~in a BlOtt~l ~yro dy~ uc filter granulating apya~atu~ l~ u~oa ~or tho g~ulat~o~. An ap~aratue o~
t~6 kln~ doecri~e~ ln Dl~-A-29 3a ~03, to which re~erence ie aleo made ln BP~ 02 462, ~, ln ~omewhat dl~ore~t e~bodimeAt~ in t~ late~
~p-~-331 lll. ~ i~ a ~luidlsed ~ed appar~tu~ ln whlch, unaer~eat~ t~e periorated ~a~-, ln tho ~in~
ahamber, th-ro i~ ~ rotor whleh only alloY~ the fluidi~ln~ ga~ to be ~lo~n ~n in certsin radlAlly ext-~ndlng ~on c ~1~ ~ce ~lorly a~ n re~ult of eho ~otati~ o~ th~t ro~or, ~o that fluidised bed ar~ can o~ly fc~nn in cert~ Hctor~ a a~oa~
~lowly th~ h ~he bulk o~ th~ ~aterial.
..
Wh~r~a~t, in the apparatus ae~ord~ng ta DB-A-29 32 hO3, thare i~ only a single ~pray no~zl~ arra~gel~ centrally abo~ th- p~rforate~ e to spra~ the coatlng o~
g~ulating liq~id into the ~lu~dls-ld hed ~ran ~el4w, lr th~ appas~tw aoao~i~g to ~P-A-33t 111 th~ro ar~ radial ar~6 pro~ ~e thes perfo2~at~d ba6~, hur$n~ n~lly direcCed ~pray no2zle6 ~-hiah rotat~ ~yncl~ronou~ ith the Ylo~cte~l gyro rotor, fiO that ~h~y ~gr~t~ r ~ith tho tlui~ e~ bed ~one8 ~ ~;~ray the grA~Iula~g ...
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';~. , 09 l~O~ '94 12:42 GOERTZP~TENT r 3~ 3 6 0 0 9 P.~/22 -- 4 - :
llquid into th~m f2~ b~low~
13P-~-30~ 4S2 describes, ~al~ ~aking the ex~le of a ~-fo~d addltlvo co~t~l~ln~ zlnc ~a~ltracin, ho ~ t~e gra~le~ ~oduc~ 1~ t~e ~lotte~ gyro f lu~ ~lse~ ba~
~p~ u~ ot only h~ re~ bo~ter c~e~ical ~td~illty Pu~ also a very narrow aA~ even p~rticle ~ize di~tr~ution of the g~ules, which conta~n ~art~ly any :~
o~or~izad partlGl~ and ax~ virtually ~reo ~ron~ du~t.
~o du~ producod ~ ~ abra~lon test, moroo~ror, contai~c h~rdly ~y o t~e uct~re ~ubst~e, ~lnc bac~tr~ci~ .
As i~ eleA~ ~r th4 e~odl~ents by vay o~ axan~le in EP-A-302 462, S~atche~ o~ ~tarting r~aterial Qf the order o~ 3 lcg w~ro proces~ed. P'c~ed ad~lti~ves ~re ~e~t 1~
t~e~. ~o e~blo eco~ ical pro~uction lt 1~ deslrable ~o ~rotluce g:c~nules iJ~ aloountl~ rang~ng ~rom 00~teral h~ndred l~llograT~ up to o~e to~, ~rhe alm o~ the inv~ntic~ to provl~e a proce~ for bull~-up granulaticn of powd~red ~c~rlal and a suitabl~ :
apparatus uhich 1111 pro~uce, mo~e particularly on an i~strial eeale, wi~orm ~nd ~ub~t-ntlally ~u~t-~ee g~:~ulo~ which ~orr~ o~d i~ t~eir propertie~ to th~3 reiaulw gl~ A-302 462.
It i~ ~ie~ll ks~own 'c~ ~ho~e ~klll~ the a~ i~e tho ~lo~r CharAC~eristlCs o~ tances d~ ignlitcantly on tl~e ex'ce~nal co~ditlon~ a~d al~o on th~ appi~r~tu~
uis~d. Tlliis ali~o i~pplies in ea~h C~ to gr~nulating ~roc~ss~ u6inSI ~luld~e~ bed æp~aratu~. The ~p~ri~nts ~ere c~rried ~ut ~ith a ~lul~lsed be~l a~paratu6 app~imately Z ~ in diamot~, tho ~tches of powelere~l mate~lal we$ghing abo~t 750 kg, 1~o~ 2r, it il~
as~umed that t~- re~ult~ sc~l~v~ can al~o b~ :
tra~ rred as~logou~ly to 4pparaeu~ o~ di~rent orders ~ .
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09 NO~ 'g4 12:43 GOERTZP~rENT ~ 1. 3 6 0 0 9 s~
of magnitude. ~e e~ri~snts were aloo ca~ d out in thi~ in~an~ ith ~ ~e~ ad~ti~ ont~ in~ zi~c bacltracir" th~ co~ ition and vt~er c~d~ tlon~ o~
whic~ casl be ~cund in l~P-A-165 577 asb~ l~P-A-302 462, to . :~
w~ich re~erence ~e ex~?re~ly ~e. Blres~ ~houg~ the ~xperln~t~ carrie~ out were inten~e~l prim~rlly fo~
granula~ln~ a f~d addit~e ~ontalning 2inc bacitr~c~n on an ln,~!lu~ial ~cale, with ~cl~lc gi~en prapor~$eo, ~e presenc l~lv~elon i~ not restricced to a fe~
additi~re o~ thi~ klna but 1~ s~en~rally sultablo ~or the gra~uldt~n o~ powde~ed mater~al, the ~r~i~g m;~t-ri~
and g~anulating liquids bel~S~ aa del~crlbed ~n ~P-A-302 ~.6a, to whlch re~erence ~ ~re~cly ~do ~or tbi~ rea~on.
Other s~tanc~- o~ partic~lar lntere~ a~e ~aterol, sputolyeille, bi~olvone, ~ lnia~cln, ~lo~ln, ~plr~mycln, no~ihe~tld~, p-nic~
chloroto~r~cycllrl~, ooyteeracycllns~, t~tracycl~ne6, e~thronyclr~, furazolidone, nitro~uran, thrl~etho~rir~, ~ull?honalnlde~, dlnultrid~zole, neo~yci~ base ~nd all vitamln~ w~ieh aro pk~rmacoueic~lly accol7ced or allowffi un~er ~cod r~yu~loDY, suth aJ ~ta~n A, a~, A~
B~ , B~ C ~a~corbie ~cld), aocor~ylpalmlt~te ~n~
ot~or ph~rs~colog~cally accept~ble dsrivatlv~
a~corb~e acid, D, D~ , D~, r~ , x, ~L~ Xa, ~ and - or act~vo ~ub~t~nc~6 6uoh a~ ~voparai~, flavopholtpol, ~on nsin, ~nensi~-~odiu~, salin~yci~, carbadox, nitrovln ~nd olaguinoox.
~he ob~oc~ive o~ impro~g a ~oc4~a o~ th~ type de~cri~d ~Yelnbeforo i8 aChleved aaeo~di~ to the in~enti~ i~ th~t the granulati~g li~u~d i~ ~p~yed int~
fluidi~ed ~ane~ ~f ~he ~aterial by ~ea~s o~ fl~t ~et no~zle~ ~r~m ~bov~ th~ ~lui~i~ed bel, ~b~tantial.ly in co~nt~r-cur~ent to the ga~ cur~e~t which ~orm~ th~
~luidl~d bed. ~ ~luidi~ed ~e~ apparatu~ ~lch i~
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0~ NOV '94 12:4~ GOERTZPRTENT ~ O O ~ P.4 wi~a~le for per~ormlng the proces~ according to the ~ n~r~nt~ on i~ a~eortlingly cha~acteri~ed ~ ~ tbat t~ cpray nozzle~ ueo~ are ~lat ~t ~ot~le8 w~ arr~ng~d ln an upper part o~ the concal~ whic~ hen th~ a}~p~r~tu~
i6 operates~ a~ lnte~ ~ ve the flui~18ed bed ~o~d, ~ the~e ~lat ~et no~le- ~re Cl~rected ~o that ~ch~lr directlon of ~p~:aylns 1~ tant~ally dO~Ilw~B
tot~rd6 th~ idi~Cd bed, On an in~u~trial ~calo, ~ g a larger appa~atu~, lt ha~s ou~d that ~pr~ying the gra~ul~ting llquld in f rom below, i.e. ~rom the per~or~-ted b~ upwara~ ~nto tbe ~luid~ sod ~Lto~ial ~on~ riou~ly not ~h~ optlmum ~athc~d, ~rtlcula~ly i~ a ~l~ldi6~d X~ hno b-en l'ormod only in c~ in ~re~c, as ~ith '~he ~lott~d gy~o n~hod, the 1~id~1ng g~ ~ppo~r~ to c~ey up th~ granulati~ .
llqu~l whio~ ha~ be~ blawn in in ~arallel, ~o tllat lt doe~ not come ~nto optim~m Contact with the ~rial which 1~ to b~ agglos~erated. Ih~f4ro, it h~ pro~red more ef~ectlvR to spr~y the g~:~nul~tl~g liquld in ~rom :
abo~a, ~o tO 6pQak i~ counter-curre~t to ~ho fluid~ng ~as, into th~ ~uldls~d area~. ~o b~it r~eults were o~t~lned ~ith ~lat jet no~zles ~hic~, in ~ ca~o o~ a con'cainer of cirC111ar cro~6-Gectio~, aru p~eS-r~bly ali~d ~o th~t tho clongate ~u~ace co~ered b~ the j~
~ tlth ie~i 104g ~i~ ucis ~ tan~lally il~ t2~e di~ectiol~ o~ a radluY of the ~ppa~atu~.
The ~o~t e~octi~lr nozzl-~ ~avo ~r~re~ to b~ l:Wo-c~qpo~ent ~lat ~et lloz21e~ w~th ~xte~ lxing, whe~e~n, a~ter lea~g th~z nozzle, the liquid ~h~h i~
to b~ ~praye~ a~on~ced ~y a~ a7~ia~ e c~rrent ght ~r~to t~o desire~ jet ~o~m~ ~e s~e~iaoni~ for th advan~ageou~ e~ect o~ t~ese nozzle~ has no~
hitAer~o ~o~n expl~tnea i~ deta~l but 1~ i~ pre~
that, ln ~te o~ ~e ~ e3Wre o~ thc ;, at~i~lng g-s, a ~oft, ~ell di~ribut-d $et i~ produced :~ :
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09 ~IOV '94 12:44 G~)ERTZP~TENT ~ ~ ~3 6 0 0 9 P.5~2 wieh ~ t1 tlyna~ic ~hich produce~ a ~articula~ly even aSIglom~ratio~ e~ect i~ conjunctio~ with t~o fluidlsed po~ered mat~rl It ha~ been ~ nd tl~at, ~ uit~ble r~unber o~
~l~t ~et u~>~210~ are dl~rlbuted over ~ fluidl~ed Ped, it i8 ~10 lon~e~ ne¢e~a~y ln ge~eral to u~ th~ ro~atlrlg ~lott~d gs~ro, i~e. ~co produ~e llmited ~luidi~e~
~ea~ $eh rotat- ~lowly throu~h the ayparatu~. Gooc~
rosultE are Achiev d almo~t to the ~me extent with a perf~r~ted ~ hich i~ lly ac~ed upon by ~uidising gas. Mo~eov~r, lt i6 not absolutely e8~ntial to have thH ~l~t ~t nozzle~ ~l~atl1ag o~rer the rluldloed bo~, althou9h thl6 le ~I pre~erred e~odi~nt of tho pxoc~
according to ~h~ l~v~ntion. Whet~er t~AiB ~ea~ur~
nece~sary depend~ o~ the on~ han4 on the nun~er and diotr~butiorl o~ the ~c~z7cl~ n the t~th~r h~nd on the dyna~Dle6 ~ th ~lui~i~0d b~ t hals b~ aund ~bat, e~e-~ with ~cationa~y ilat ~ot ~0221es which ccnrer only a~o~t ~2~ of the surface ~ fl~lid4~od bed, ~ln~form g~:anule~ O~ o ac}~d. r~e dur~tlon of ~pr~ying and ~h~ recirc~lati~g ff~ct in ~he ~lui~i~ed b~d pre~ably cont~ibuto to th- ~e~ult- o~ tho proco~.
rhe choic~ o~ the nu~e~ o noz~eo i~ t~ot ~re~ ~ ac 7nu~h aH ~ ll~ted ~ounS o~ lating liquld ha~ to b~
~prayed i~to a ~tch of m~Co~ d the opray~ nwst ext~s~d over a cert~in l~gth o~ ti~ in o~der to achieve ~low a~lo~eratlo~ and gra~Ulatlon, w~llst tS~e ~luldis~ng ~as nsu~st al~o bo rl i~ pt~-itlon to ~ ~ove the ~olvene or 1;ll6pe~l6ion ~gen~C rrO~ the gr~nulating liquld.
Sln~ on the other h~nd the rLo~ s u~e~l r~8t have a ~pecl~c amount trarolliD3 t~rougb. ~chom~ lt il!~ no~
ble to ~pr~ ~h~ e~t4re ~rfa~e o~ t~ luld~ed bed. P~e~er~ly, ~ceos~ to the invelltion, ~t ~y ~ne :~
tim~, o~ly ~bou~ 2S~ oS cb,e ~ur~ace o~ ~h~ Sluidise~
b~d iB cov~r~d by tha ~pray ~et~ o~ the no3~1~8. T~i~
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09 NOB '94 12:45 GOE:~TZPPITE~T ~ ~ 3 6 o ~ ~ P ~/22 ---~ac~c may ~ke iC neoeli~ary to allo~ the s~ozzle~ to ~grato o~ver th~ ~ idl6ed bet or ~otato, tc~ achiev~ -~ett~r ~pray distribution.
Generally, ~.5-30~ ~y wel~ht, pre~erably 5-~0~ by we~ht, ba~ on t~e ~in~he~!l 0ra:t~ule~, o~ btn~er will b~ introd~o~d into the product, ~ho gr~ulating liquid beiny a 1-30~, pref~ly 2-10% and more e~peclally 5-7~.
~oluti~n or ~u6ponBio~ of the bindRr ln one pa~ticular nl~eer~ti~e enbod~ t o~ the prooet~
it iB po~61bl~ ~lr~t to rpray tne ~ure accl~ t~ce on ~co th-~ carrlor m~t~ial and to ooat it wlth ehe ~oating ~ater~al ~n a c~co~d ~tep. In t~iJ alternati~
emb~llm~nt the ~opo:ctloP. ~ w-ight or ac~ re sub~ta~o `19 ~s~eon 0.01 and 30~ ~y ~e$ght, b~oe4 on th~ ~lni~hed e~, d-~endlns~ on th~ p~nnacologlc~l act~rity o~
~he active sub~t~ce. Tho active o~tas~ce m-y b~
~p~ayed on i~ t~e ~o~ o~ ~ ~olut~o~, ~or ~le ~ o.o ~o 30~ ~y Yelg~t ~olution, o~ ln th c~e Or 1 colu~ ctl~e ~ubat~nce~, ~n t;he ~or~ o~ a Bu~pen~
Whe~n ~d~uctlng th~ concentr~tion of thll ~olutlon co~tainlng the ac~cive ~u~st~ce, o~viously the nature of th colven~ and th~ 80~ $ty 0~ the acti~e ~b~tanee ~ th~ ~olYe~t ~u~it be bon~e ~n minO
Ihl- altern~t~e e11ibodl~t 1~ o~ p~rtlcular inte~e~t -~
~rlt~ i~ly acti~e Bu~st~Ces 6~ch a~ cle~buterol o~
~putoly~lsle . 8xan~pl~ of carr~ er~ include ln~ Aic ~a~lar~ ~uc~ aB calcium car~onat~ or dicalcium pho~phat~ nt ~lef of org~lc car~l~s~ inclu~
9U9'E!ISB I~UCh ~1~ lacto~e, la~to~-cor~ ~tarch or ~accb.aroce~ but al~o ~or~itol.
In the ~rime~t~ c~ d out ~Ith tho ~ee~!l ad~el~ e, o~au~ 5~ o~ methyl c~llulo~o, l:~Ee~l or~ the fl~i~h~d :-~remul~, were used, the granulating liguid boins a 5 ,;
d :' : :
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"'~' ' . : ~, ., , ' El9 l`lOV '94 12:~5 GOERTZPflTE~T 2 ~ 6 0 ~) ~
aquaou~ ~olution o~ Che tnothyl clellulos~. Ot~r coat-lny ~a~erial~ a~e p~soible, a~ di~clo~ or exa~ n P-A ~65 s~7 E~nd 302 4~2, to whi~h re~e~ence i8 ~de.
o~ p~rticulAr ineorest, apart ~rc~ thyl cellulose, are ~ydroxypropyl call~lo~e, ~ydro~ypropyl~et~yl aellulose, polyethyle~ly~ol ant w~te~ oolubl~ 6taxch.
With a bi~d~r c~nton~ ~f 5~ ~ S~ 801utl0n, the total a~ount of gra~ t1ng liquid 1~ litre~ corro~pon4 ta~tlally to '~h~ weight in l~g o~ the po~red mataria~. ~peclf i~ . ~rl o~der to achleve good r~ul~6, thi~ quantlty of~ d wa~ pref erably ~prAy~d ~to the ~luidis6d ~d over a ~eriod of 3 to 4 hou~
ty o~ r U~Lit of tim~ ~oed n~ n6~e~sarily be kept Conatant throu51hout the e~tire ~pr~yi~g tl~.
Inaeed, rather more liqui~ may b~ ~p~ayed at th~
beginning o~ the proce~ d r~thsr le~ tow~r~l3 the en~. ~ith a ~ant~ ~y o~ about 1 litre o gr~nul-ting li~aUi~ per Iy~ o~ po~dero~ ~ter$~1 and a ~p~-ying ti~
o~ ju~t 3.S hour~ a~rerage ~pray gu~ntity ~r un~t tl~ of c~nly ~out 5 ~lJk~ of ~tartlny ~aterlal y~r m~ute i~ o~tain~ . It fOlloWC f ra~ tl~t the s~ray density on the to~ o t~e ~luidiBed bed casulot be mal~ta1ned at a v~ry high l~el.
rwo~ c~ ~lat ~et no~zl~ ~ult~lo ~or the proeeca w¢o~diny to th~ tion are 801~ OF ~ple, by t~e i~
compa~y 9pr~2~g Sy~te~. ~ te~t~, o~ ~o~zl~ ~de by thiw co~pa~y, ~ring tho name S'.JB 4S as~ ~a~ing a 3~ay angle o~ ~S^C prolred st~ltabl-, ~ ~. ~t:ord~ eo t~e ~eciricat~an o~ t~ ct~rer thiB no~zl~ ha~ a liquid through~ut of 4.7 l/~ ~o~ ope~ation ~itb w~ter a~ ~ ~lu~d pressu~ ~f 1.5 bar and an air pre~2re o~
a~out 6.0 ~ar. At a liquid i~let pres~ure o~ a.7 b~r ~nd an air ~res8u~e of S-6 bar, ~he wa~er t~ rough~ut ~all~ to 3.2 l/~in. ~:n the Ca~e of ~igl~er ~rlscs:~ity ' .".
^. . .
,............................................................ :
.
~ ~,36009 09 NO'~' '94 lZ: 46 GOERTZPhTE~T P. B/~Z
~- ~ O -- , ll~ui~ ah a~ th~ g~a~ulating liqui~ ln~rol~o~ h-r~, ~e llqu~d th~o~gh~ut of the n~zzl~ iG I~Ubet~t~ally le~e. ~q~e vi~c~ity ~ ~h0 li~ ay ;!113C~ be a~fecte~
by its t~peratu~. It ha~ bo~n ~o~d t~at the nozzle~
operate cati~factorily wit~ t~ granu~acis~ if the vi6co~i~y of the liq~d 1~ ~d~u~t0d So t~ult nc~2zleu ha~e a throuy~u~ wb,lch 1~ 0.1-0.3 tlm~, pre~!-ra~ly a . 12-O .111 tioU~E t~o ~anis-al chroughput with water~ Prefera~ly, the nozzle~ ax~ O~o~ted at ~
pr~s~ure of a'comiei~g gaE~ of ~etw~n 2 a~d 6 ~r. ~rhe tluld pr~ure 1B d~ten~ by th~ ~lred t~lro~gh~ut o~ tho 51O~ t lDay ~a~ t~ on 0.7 ant~ 3 bar ~n~ 10 fl~r~bly l:~et~e~ 1.2 ~nd l.t bar. ~t~th a 5~ hyl cellulo~e ~olutio~ h~ rlng ~ een~peratu~e o~ 30'C, the ~hr~u5~1?ut ~lth th~ ~ove-~tioned no2~1e t~pe ie a~out 0 . 6-1 . 4 l/~i~.
I)ependi~g on the ~pacing o~ suc~ A nozzle ~orn the sur~ace wh~ch 16 to ~ ~pray~d, ln thi~ caoe the theo~e~ical ~urfac~ of tl~ ~luid~3-1d ~ed, ehe noz~
oprayr ~ Crea o~ 15~-7~0 c~2, ~, ep;~zlyin~ a~-a o~ bet~een 500 ~nd 70D c~n' belng p~otorred, for ~hich t~ ~r~ge 6p~Ci~g Or the no~zle from ohe sur~ac~ to ~o ~;pr~,yed i~
~ou~ 70 c~. ~ha pre~erred ~pray d~ity, ba.~ed on the are~ ~ceually ~pra~ed, i~ preroral:~ly betwee~ d i 15 l/~.~.
~ha spr~ er ~ Q l~dl~rldu~ zzle~ l th~
;5~tl ty of gr~ulat~ liqui~ ~o b~ eprayed E~er u~
t~me will g~e th~ nu~r of s~ozzleæ r~quired, once a cific nozzl~ t~rpe has b~ o~e~, whil~t ~he ~rertic*l arr~ ement, iXI l?articul~r, wlll proauce t~e pr~orre~ ea to b~ sp~e~l. I~ the ca3e o~
;-~app~r~tu~ c~rclllar cro6æ-sestlon tl~e noz~ ar~
pre~er~ly arra~ged BO that thel~ op~aLy ~.rea~ exe~n~l radially ~nd are u~i~ormly ~paCe~ ov~r t~e p~riphQry the~eof. ~ the le~gth o~ t~e ~pray ~roa o~ a nozzle la J, .
` ` .
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s~
04 NGV ' 94 12: 46 GC~;~TZP8T~lT -- P . 4 'Z--more or 1~ t cie~t to Co~rer t~e rad~ u~ of a con~cainer, a ring o~ nozrles is ~refe~&bly u~e~, the r~o~zle~ b~ing ~p~eed f~e~ the centre ~ C roughly half th~ l~h of c~e ra~iu~. In ~;he ca~e o~ A cor,tainer it~ a dla~aeter o~ 2 m, for e~l¢, ~ood ~el~Ult6 were ac~ uith aix noz~lo~ a~ra~g-~l ~ ~io way a~d distribue-CI o~er ~h~ ciroumi~r~oe. Ft~r larger ~ontai~er di~ter~, a l~ger sstlnber o~ no~lac may 2:~a ~equtred, ~nd th~e ~oz~le~ t~ey do ~ot co~er ~ t the e~tlre le~s1th of t~o rad$u~ o~ a cos~t~iner, chould be ~ ltnrs~tely a~ ere~t ~pacin~ fra~ the c~nt~e of the Container i~ ~uc~ a ~y t~a~ ehe m4~t mlfonn ~pr~y d~it~ibution po~ible i~ a~i~ved over the ~luldi~ed ~atd.. Bao~ on the ~otal ~ur~ac0 ~rea o~ t2~o ~luidi~e~ bed a ~pr~y de~lty of betv~
3 l/m2.min, l?Fefer~ly ~etween 1.2 auld l.S l/ma.m~n ha~
pro~od ~ultd~lo.
To produ~e the ~luldl6~d ~d, quanti~ ~ of gao ~angin~
rran 10-60 n~ o~ ~er$orated ~a~e ~atte prov~
suitablo. The proceH~ ~ccor~ing to the $nv~n~ ha~
th~rerore p~ov~d partlcu~arly econc~acal i~ th~6 re~ ct. I~like ~y lcno~n ~th~e, t~e proc~s~
according to th~ invention i~ not ~arelcula~ly af~ected by wheth~r e~e cu~ent o~ ~luidl~ny ~a~ tl~rough ~he per~orated ba~- 1B generaeed by ov rpres~ure belo~ the p~rfor~ted b~e or by ~de~-pre~;su~ above ~he.
or~t~d b~-. 'rher~o~, ior generat~g t~e ga~
currc~t, elt~r ~ pr-~cur0-generAting bl4 -~r may b~ :
~ro~ided in the Sl~ ch~er ~ w the per~or~t~d ~se or a ~uctlon blow ay se pro~do~ ln the pr~u~t op~ce a~o~re the ~luiaised ~ed,.
~a~; prcc~a~irg the ~eed add~tlv~ ~u~d ln t~e ex~er~luents, good re~ults were ol~ined by ope~atin~
with a ~peeific pe~ora~s~?l ba~e lo~l o~ 200-300 kg o~
pow~er~d o~rting ~terial ~ n? o p~oro.ted ~a~e. In ~' :
,;: . ~ . - :
~1 f3 6 ~
~19 NOV '94 lZ: 47 GOERT~PRTENT P. 10~2 t~lo par~loul,ar ~n~tance, the ~luidi~l~g gas u~ed ~as nitrogen, whieh ~a~ at a ee~erature in the range fronn 90 to ll~-C, pre~ably 104~C, on ~t~ing t~
5~anulating ap~ tu~ d~r~d m~t~rlal wae be~t~d ~o a ~e~p~ tu~e alx~ve 70-C, p~t~ral~ly BD-C, ~or~ tho ~tart o~ ~prayin~. ~e ~ollo~ring i6 a ~e~cription Of t~e ba~lo c~-~ructio~ o~ ~ etnbodi~ent Or a fluldioo~ -bed app~r~tu~ accordlng t~ th~ ln~r~ntlon, r~orrinS~ to the accon~anyirlg ~raw~ng~, vher6~in:
~ig. 1 ~8 ~ diagran~atic ~rertlcal ~ection th~:ough the inlportant c~ponent~ ~ the apparatu~
~1~. 2 i~ a diagrammatlc }~ori~onta~, sec~o~ through ' ~pp~AtU~s~ ~ the di9t~$~ution o~ the ~pray ~o~sl~
l~he ~luidi6~d bed gr~llator ~how3 i~ diagran~tic c~o~s- section in Fig . l co~prl~eY a prod~ct ~ontaine~ 2 for ~he po rdere~ n~aterial which i~ to b~ granul~e~l, g~alod o~f ~t its lo~r end by a fi~e ~ c~rated the ~gree ot ~ o~ which i~ ~u~ t~at th~
p~wderod ~utorlal wh~ch it l9 lnterldet to ~u~ort euY~Iot Fao~ through the pe~forat~ e i~ any 6~ ta~tlal :~ .
amsunt . A2wv~ the ~ro~uct cont~lner ~ a~d on an upw~ra :
~o~ti~a~on ther~of is provlded an ~pper ~ect~on 6 of the ~r~wlator. q~ upp r 6ec~ aG a cylin~rlcal -out~ casing 8 whlch i~ lo~ o~f ~t the top b~
upper wall 10. Bela~ t~ product cosltai~er 2 or ~he p~rforatod ba~e 4 th~2reof i~ a wind ch~mber 12 pro~ ed ~th ga~ inlet po~tc 14 which ar~ ca~e~ted to a blo~r t~Lot sh~n). In the uppe~ section 6 Df tho app~ratu~ i~
a g~ outl-e por~ 16 ehrough which th~ 1uidi~i~g gao cAn ltave ~h app~ratu~ ~g~in. The broX~n lin~ la ~n the top part o~ the apparatu6 ~iagru~atlcally ln~icace~ :~
a ~uat ~ilce~ whiCh 1~ inte~de~ to catch aEIy du ~areicle6 fro~ the po~derc~l mater~l carri~ by the ., . ~....
~ l 3 ~ 9 09 NO`~f '94 12:47 GOERTZPflTENT P. ll/Z2 fluidl~3ing ga~ d elthor reeu~n thesl~ pa~tlcle~ eo ehe product contalner f.ecm abo~r~e l~r coll~ct ~chem for ~urth~r treat~ent, de~tln~ on ~c pnzticula~
Alonsl the ce~tral aXi~ o~ th~ app~ratus ~d ln ~he lower pa~t ther~o ili ~r~ded ~ shaft Z2 which ~ o~ca~ly dri~ n by a mo~or 20. this ~ pl~scing throug~ the perroratl b~s~ fron~ b lo~ g providea, a~o~e the per~orated ba~e, with ~pra~ ann~ 24 ~acb of wb,ic~
pra~rid~d ~t lt~ ~nd ~ith a t~o~ ~c~ fl~t ~et s~ozzlo 2~ lgurR 2 ~o~ that tho shaft 2Z i~ Slt~ed ~ith ~ix l~pr~y an~ arrangea at egual ~n~ular s~Cing~ around the circu~f erenc~ o~ ~e ap~aratu~, ~he~e s~ray togethe~ carryin~ ~x spray nozzle~ ~I lch are po~tlon~d ~ubstantially ~al~way along the r~ al ~pac$Pg of t~e t ~2 ~rom t~e o~tor wall Or the appa~atu8. ~he Rha~t ~2 aJ~a th-~ ~pray ~ 24 l~re of hollo~
eOn8t~:u0ti~1 i~ ord~s to b~ to ~upply ~p~y ll~uld ~o ~he nos~1~6 26 by m~ o~ ply ~ (not ~ho~
In t~le dra~ngs, th~ ~rod~ct oont~n~r 2 i~ not proui,de~
with a cha~ging po~t fo~ th~ powd~r~ sial; ralt~er, the ~hol- thln~ lnclu~ll~ th~ 0z~t~tl b~ , c~n ~e noveld l~terally a~t of the f lul~ d ~ppar~tut ~ n ord-r to lo~!l and unlo~d it, as indicat~d by ~2 break 2a isl the out-~ w~ll o~ ~hf~ apparat~. ~e apparatu~
inten~ed~ ~o~ batch o~ atio~.
In ~a e~ll~nt of the ~lu~dl~ed b*~ appat~atu~ U~d ~or acperimental pur~ , the ~lametos 0~ t~ pro~UCt ~ontainer ~ of the u~per ~ction wzls a}~o~t 2 m, which, ~ter ~e~uctio~ or the cro~6-~ection o~ the ~ t ~2 a~ the per~c~r~t~l ba~e, g~ p~orated ~a~e ere~
o~ ut 3.1 m2. T~e ~ray ~02zlee use~ were t~o-canponen~c 21at ~et no~zles ~udo by tb- in~ ~prhyir~g .:
i Sy~'~em~, of the t~ SU~ ~5. S~e ~oz~e8 wero axr~e~
about 145 cm a~ovo ~he per~orate~ ~ase 4. ~lth , :
., O~ NO~ ~94 lZ:48 ~OERTZP~TE~T ~ 1 3 6 0 ~ 9 P lZ/zz rluldised t~ed height abo~e the E~Qrforatecl ~a8e O~ abtu~t ..
75 cm, t~i~ yave a ~p~Cins o~ the nozzle~ ~rom ~he fl~lidi~ed be~ o~ a~aut 70 cm. ~ha noz~le~ ~ere ope~a~ed und~r a gas pr~6ure o~ a~out 4 ~ar. ~na~r a ~luld ~re~gu~ Of a~ Ur 1.5 b~r, a no~le o~ t~l~ kl~d ha~ a wate~r: thro~ghp~ o~ about 4 . 7 l/~a~ . ~en ~pr~y~ 2~g a 5%
ac~ t~yl oQllulo~Q ~ol~ the th~oughput p-r nozzle i~ about 0.6~ l/mln, aepen~ çr on the rluld pre~ur- .
5he d~v~ foz t~e o~ft z2 ~ d co ~e rogulatabl~ ~or ~eed~ betwoo~ 0.2 a~ 10 r~m.
The ~luidi~ed bo~ appar~t~ d~cribc~d ~bov~ was u~ o gra~ulst~! ~ po~arod ~t addlti~ cont~lning zin~ ::
b~citracl~. A typi¢~1 e~odimOEnt ~y wi~y O~ ~?le i~ .
glve~ here~naft~r: :
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~36~0~
09 NOV '94 12:48 GOERTZP~TENT P. 13,'22 . .. __.
- 15 - i O
71Z.~ kg ~f a po~ldere~ ~o~ additiv~l: cont~iD~ng rinc bacltraoin were ~1AC~d in ~e pr~duct co~taine~ o~ the ~lu~ ~a bea aFpar~tW de~cr~b~d ~bove. rrhe powder hAd a particle ~izo ~l~tr~buelon o~ 0 ~m, the ~a~orlty Of t~e ~artlcle ~lze di~t~ibutl~ being in t~e ran~o ~rotn 10-1~ ~. In ad~lt~on ~o 5-30~ by weiyht of ~lnc bacitrwi~ a pa~r or thi~ kind al~o contalns ~r~neat~on reoldu~ ~r~ ehe ~act~rln~ ~roc~ and C~leiUlD c~rbonate.
Nl~rog~n W~B u~ed a~ ~h~ ~luld~ing ~. At th~ t~rt o~ proeo~, th powd~red ~t~tiny ~aterial ~
h~atod to 80-C ~or ~out 2~ ~lnut0~ by ~nB O~ nltro~en ga~ at ~ t~mper~tu~e o~ 95~C.
For the opr~ying oS t~e gra~ulaeln~ liquld whic~ take~
~lace next, BiX flat jet no2zle6 we~e u~ed, ~ith thelr jets dl~ecte~ downwar~ on to ~ uiai6e4 be~, ~he~e noz~le~ ~otatin~ at a ~p~et of 6 rp~ thrcu~ the appar~tus. A total o~ ~0 1 o~ m~hyl ~llulo~
~olution at A t~mæ~ratur~ ~ 30'C ~ prayed o~.
In order to prGduce the ~lul~i~ed b-d, ni~oge~ ga6 at ~ :
approximat~ly 100~ ~Q8 blown into the a~3raeu~ ~n in~rea~in~ amount~, initially at a rang~ of 40 m3/min and, to~ard6 t~c end, at ~ rate o~ lB7 ~fmlu. ~he ~pray rate o~ the granulat~ng liguid w~s 4 lJ~l~ ae thO .
be~inning ana ~as ~ncrea~ed by 1 l/~1~ artox 20 lltre~
had bee~ spray~d in, ~d ~ lly to 8 lJ~n. A~ the ~pray sat~ wa~ $n~rea6ed t~e ~a~ti~y o~ ~lui~is~ng gac was al~o ~c~ased by 10 ~31~in Up to gO o~lmin. ~fter ~ :
~0 litres oY gr~sulat~ng liquid haâ ~eon ~pr~ , the spray rate was reducYd to 4 l/~dn a~ X~pt constant. :`
The ~o~al ~prayi~B tlme ~a~ ~bout 3 h4ur~
09 NOV '94 lZ:49 GOERT~PRTENT ~ ~ 3 6 ~ ~ ~ P 14/ZZ -----Aft~ praying had ~inlshed a~d t~e ~oz~le6 ~ad boen waRhed with a cer~ain quantity oY wator, ~h~ granul~a p~duc~d ~ero d~ roduct ~empor~tu~e ant th~
~pent air ~ture o~ the ~y air were ~itored.
~he particl~ size d~str~bution o~ the gr~nule~ l,ra~ v~
even, the propo~tion o~ partlcle~ bet~ 190 an4 710 ~m in e~e gr~nule~ was more tban 20%, wh~ch s~ti~iod the :
~peclfiGationB. More tha~ 98S o~ t~e granule~ ell wlthln t~e r~ of 1~5 to lOOO ~ rhe ~xo~7ort 10n o~
V~ ino ~ticle~ ~6uring le~ t~an 45 llm ~a~ 0.01~, which wa~ ~g~ w~thiD. t~ peci~iCAeion.
~ore~or~ nule~ 1ch ar- totally ~tlJ~actory c~n be produced ~lng th~ ~tho~ accorCli~s to the lnventinn an~ the ~luidi~ed b~d apparatu~ according to th~ !
in~rent ion . I :
A~alogou~ly ~o ~cho ~x~le do~cribeat te6t~ ~rt al~o c~rried out o~ an ln~u~lal 5C~lc wit~ c~lcium carbonate ~a la~tose a~ ca~rlers an~l furt~er : -~i~ent6 lr~re carrled oUt u~i~g Rol~la ~t~ch ~ ehe C05Cs,zg ~t-ri~
;l :
d ~:
,`,-' ' ~
pro~od ~ultd~lo.
To produ~e the ~luldl6~d ~d, quanti~ ~ of gao ~angin~
rran 10-60 n~ o~ ~er$orated ~a~e ~atte prov~
suitablo. The proceH~ ~ccor~ing to the $nv~n~ ha~
th~rerore p~ov~d partlcu~arly econc~acal i~ th~6 re~ ct. I~like ~y lcno~n ~th~e, t~e proc~s~
according to th~ invention i~ not ~arelcula~ly af~ected by wheth~r e~e cu~ent o~ ~luidl~ny ~a~ tl~rough ~he per~orated ba~- 1B generaeed by ov rpres~ure belo~ the p~rfor~ted b~e or by ~de~-pre~;su~ above ~he.
or~t~d b~-. 'rher~o~, ior generat~g t~e ga~
currc~t, elt~r ~ pr-~cur0-generAting bl4 -~r may b~ :
~ro~ided in the Sl~ ch~er ~ w the per~or~t~d ~se or a ~uctlon blow ay se pro~do~ ln the pr~u~t op~ce a~o~re the ~luiaised ~ed,.
~a~; prcc~a~irg the ~eed add~tlv~ ~u~d ln t~e ex~er~luents, good re~ults were ol~ined by ope~atin~
with a ~peeific pe~ora~s~?l ba~e lo~l o~ 200-300 kg o~
pow~er~d o~rting ~terial ~ n? o p~oro.ted ~a~e. In ~' :
,;: . ~ . - :
~1 f3 6 ~
~19 NOV '94 lZ: 47 GOERT~PRTENT P. 10~2 t~lo par~loul,ar ~n~tance, the ~luidi~l~g gas u~ed ~as nitrogen, whieh ~a~ at a ee~erature in the range fronn 90 to ll~-C, pre~ably 104~C, on ~t~ing t~
5~anulating ap~ tu~ d~r~d m~t~rlal wae be~t~d ~o a ~e~p~ tu~e alx~ve 70-C, p~t~ral~ly BD-C, ~or~ tho ~tart o~ ~prayin~. ~e ~ollo~ring i6 a ~e~cription Of t~e ba~lo c~-~ructio~ o~ ~ etnbodi~ent Or a fluldioo~ -bed app~r~tu~ accordlng t~ th~ ln~r~ntlon, r~orrinS~ to the accon~anyirlg ~raw~ng~, vher6~in:
~ig. 1 ~8 ~ diagran~atic ~rertlcal ~ection th~:ough the inlportant c~ponent~ ~ the apparatu~
~1~. 2 i~ a diagrammatlc }~ori~onta~, sec~o~ through ' ~pp~AtU~s~ ~ the di9t~$~ution o~ the ~pray ~o~sl~
l~he ~luidi6~d bed gr~llator ~how3 i~ diagran~tic c~o~s- section in Fig . l co~prl~eY a prod~ct ~ontaine~ 2 for ~he po rdere~ n~aterial which i~ to b~ granul~e~l, g~alod o~f ~t its lo~r end by a fi~e ~ c~rated the ~gree ot ~ o~ which i~ ~u~ t~at th~
p~wderod ~utorlal wh~ch it l9 lnterldet to ~u~ort euY~Iot Fao~ through the pe~forat~ e i~ any 6~ ta~tlal :~ .
amsunt . A2wv~ the ~ro~uct cont~lner ~ a~d on an upw~ra :
~o~ti~a~on ther~of is provlded an ~pper ~ect~on 6 of the ~r~wlator. q~ upp r 6ec~ aG a cylin~rlcal -out~ casing 8 whlch i~ lo~ o~f ~t the top b~
upper wall 10. Bela~ t~ product cosltai~er 2 or ~he p~rforatod ba~e 4 th~2reof i~ a wind ch~mber 12 pro~ ed ~th ga~ inlet po~tc 14 which ar~ ca~e~ted to a blo~r t~Lot sh~n). In the uppe~ section 6 Df tho app~ratu~ i~
a g~ outl-e por~ 16 ehrough which th~ 1uidi~i~g gao cAn ltave ~h app~ratu~ ~g~in. The broX~n lin~ la ~n the top part o~ the apparatu6 ~iagru~atlcally ln~icace~ :~
a ~uat ~ilce~ whiCh 1~ inte~de~ to catch aEIy du ~areicle6 fro~ the po~derc~l mater~l carri~ by the ., . ~....
~ l 3 ~ 9 09 NO`~f '94 12:47 GOERTZPflTENT P. ll/Z2 fluidl~3ing ga~ d elthor reeu~n thesl~ pa~tlcle~ eo ehe product contalner f.ecm abo~r~e l~r coll~ct ~chem for ~urth~r treat~ent, de~tln~ on ~c pnzticula~
Alonsl the ce~tral aXi~ o~ th~ app~ratus ~d ln ~he lower pa~t ther~o ili ~r~ded ~ shaft Z2 which ~ o~ca~ly dri~ n by a mo~or 20. this ~ pl~scing throug~ the perroratl b~s~ fron~ b lo~ g providea, a~o~e the per~orated ba~e, with ~pra~ ann~ 24 ~acb of wb,ic~
pra~rid~d ~t lt~ ~nd ~ith a t~o~ ~c~ fl~t ~et s~ozzlo 2~ lgurR 2 ~o~ that tho shaft 2Z i~ Slt~ed ~ith ~ix l~pr~y an~ arrangea at egual ~n~ular s~Cing~ around the circu~f erenc~ o~ ~e ap~aratu~, ~he~e s~ray togethe~ carryin~ ~x spray nozzle~ ~I lch are po~tlon~d ~ubstantially ~al~way along the r~ al ~pac$Pg of t~e t ~2 ~rom t~e o~tor wall Or the appa~atu8. ~he Rha~t ~2 aJ~a th-~ ~pray ~ 24 l~re of hollo~
eOn8t~:u0ti~1 i~ ord~s to b~ to ~upply ~p~y ll~uld ~o ~he nos~1~6 26 by m~ o~ ply ~ (not ~ho~
In t~le dra~ngs, th~ ~rod~ct oont~n~r 2 i~ not proui,de~
with a cha~ging po~t fo~ th~ powd~r~ sial; ralt~er, the ~hol- thln~ lnclu~ll~ th~ 0z~t~tl b~ , c~n ~e noveld l~terally a~t of the f lul~ d ~ppar~tut ~ n ord-r to lo~!l and unlo~d it, as indicat~d by ~2 break 2a isl the out-~ w~ll o~ ~hf~ apparat~. ~e apparatu~
inten~ed~ ~o~ batch o~ atio~.
In ~a e~ll~nt of the ~lu~dl~ed b*~ appat~atu~ U~d ~or acperimental pur~ , the ~lametos 0~ t~ pro~UCt ~ontainer ~ of the u~per ~ction wzls a}~o~t 2 m, which, ~ter ~e~uctio~ or the cro~6-~ection o~ the ~ t ~2 a~ the per~c~r~t~l ba~e, g~ p~orated ~a~e ere~
o~ ut 3.1 m2. T~e ~ray ~02zlee use~ were t~o-canponen~c 21at ~et no~zles ~udo by tb- in~ ~prhyir~g .:
i Sy~'~em~, of the t~ SU~ ~5. S~e ~oz~e8 wero axr~e~
about 145 cm a~ovo ~he per~orate~ ~ase 4. ~lth , :
., O~ NO~ ~94 lZ:48 ~OERTZP~TE~T ~ 1 3 6 0 ~ 9 P lZ/zz rluldised t~ed height abo~e the E~Qrforatecl ~a8e O~ abtu~t ..
75 cm, t~i~ yave a ~p~Cins o~ the nozzle~ ~rom ~he fl~lidi~ed be~ o~ a~aut 70 cm. ~ha noz~le~ ~ere ope~a~ed und~r a gas pr~6ure o~ a~out 4 ~ar. ~na~r a ~luld ~re~gu~ Of a~ Ur 1.5 b~r, a no~le o~ t~l~ kl~d ha~ a wate~r: thro~ghp~ o~ about 4 . 7 l/~a~ . ~en ~pr~y~ 2~g a 5%
ac~ t~yl oQllulo~Q ~ol~ the th~oughput p-r nozzle i~ about 0.6~ l/mln, aepen~ çr on the rluld pre~ur- .
5he d~v~ foz t~e o~ft z2 ~ d co ~e rogulatabl~ ~or ~eed~ betwoo~ 0.2 a~ 10 r~m.
The ~luidi~ed bo~ appar~t~ d~cribc~d ~bov~ was u~ o gra~ulst~! ~ po~arod ~t addlti~ cont~lning zin~ ::
b~citracl~. A typi¢~1 e~odimOEnt ~y wi~y O~ ~?le i~ .
glve~ here~naft~r: :
,, ~ , . .. . .
~36~0~
09 NOV '94 12:48 GOERTZP~TENT P. 13,'22 . .. __.
- 15 - i O
71Z.~ kg ~f a po~ldere~ ~o~ additiv~l: cont~iD~ng rinc bacltraoin were ~1AC~d in ~e pr~duct co~taine~ o~ the ~lu~ ~a bea aFpar~tW de~cr~b~d ~bove. rrhe powder hAd a particle ~izo ~l~tr~buelon o~ 0 ~m, the ~a~orlty Of t~e ~artlcle ~lze di~t~ibutl~ being in t~e ran~o ~rotn 10-1~ ~. In ad~lt~on ~o 5-30~ by weiyht of ~lnc bacitrwi~ a pa~r or thi~ kind al~o contalns ~r~neat~on reoldu~ ~r~ ehe ~act~rln~ ~roc~ and C~leiUlD c~rbonate.
Nl~rog~n W~B u~ed a~ ~h~ ~luld~ing ~. At th~ t~rt o~ proeo~, th powd~red ~t~tiny ~aterial ~
h~atod to 80-C ~or ~out 2~ ~lnut0~ by ~nB O~ nltro~en ga~ at ~ t~mper~tu~e o~ 95~C.
For the opr~ying oS t~e gra~ulaeln~ liquld whic~ take~
~lace next, BiX flat jet no2zle6 we~e u~ed, ~ith thelr jets dl~ecte~ downwar~ on to ~ uiai6e4 be~, ~he~e noz~le~ ~otatin~ at a ~p~et of 6 rp~ thrcu~ the appar~tus. A total o~ ~0 1 o~ m~hyl ~llulo~
~olution at A t~mæ~ratur~ ~ 30'C ~ prayed o~.
In order to prGduce the ~lul~i~ed b-d, ni~oge~ ga6 at ~ :
approximat~ly 100~ ~Q8 blown into the a~3raeu~ ~n in~rea~in~ amount~, initially at a rang~ of 40 m3/min and, to~ard6 t~c end, at ~ rate o~ lB7 ~fmlu. ~he ~pray rate o~ the granulat~ng liguid w~s 4 lJ~l~ ae thO .
be~inning ana ~as ~ncrea~ed by 1 l/~1~ artox 20 lltre~
had bee~ spray~d in, ~d ~ lly to 8 lJ~n. A~ the ~pray sat~ wa~ $n~rea6ed t~e ~a~ti~y o~ ~lui~is~ng gac was al~o ~c~ased by 10 ~31~in Up to gO o~lmin. ~fter ~ :
~0 litres oY gr~sulat~ng liquid haâ ~eon ~pr~ , the spray rate was reducYd to 4 l/~dn a~ X~pt constant. :`
The ~o~al ~prayi~B tlme ~a~ ~bout 3 h4ur~
09 NOV '94 lZ:49 GOERT~PRTENT ~ ~ 3 6 ~ ~ ~ P 14/ZZ -----Aft~ praying had ~inlshed a~d t~e ~oz~le6 ~ad boen waRhed with a cer~ain quantity oY wator, ~h~ granul~a p~duc~d ~ero d~ roduct ~empor~tu~e ant th~
~pent air ~ture o~ the ~y air were ~itored.
~he particl~ size d~str~bution o~ the gr~nule~ l,ra~ v~
even, the propo~tion o~ partlcle~ bet~ 190 an4 710 ~m in e~e gr~nule~ was more tban 20%, wh~ch s~ti~iod the :
~peclfiGationB. More tha~ 98S o~ t~e granule~ ell wlthln t~e r~ of 1~5 to lOOO ~ rhe ~xo~7ort 10n o~
V~ ino ~ticle~ ~6uring le~ t~an 45 llm ~a~ 0.01~, which wa~ ~g~ w~thiD. t~ peci~iCAeion.
~ore~or~ nule~ 1ch ar- totally ~tlJ~actory c~n be produced ~lng th~ ~tho~ accorCli~s to the lnventinn an~ the ~luidi~ed b~d apparatu~ according to th~ !
in~rent ion . I :
A~alogou~ly ~o ~cho ~x~le do~cribeat te6t~ ~rt al~o c~rried out o~ an ln~u~lal 5C~lc wit~ c~lcium carbonate ~a la~tose a~ ca~rlers an~l furt~er : -~i~ent6 lr~re carrled oUt u~i~g Rol~la ~t~ch ~ ehe C05Cs,zg ~t-ri~
;l :
d ~:
,`,-' ' ~
Claims (20)
1. Process for build-up granulation of a powdered material and/or the coating of granules in a fluidised bed with a binder contained in a granulating liquid, wherein the powdered material is fluidised, at least in parts of its bulk, in a fluidised bed apparatus by means of a has current introduced from below through a perforated base and the granulating liquid is sprayed into fluidised zones of the material, characterised in that the granulating liquid is sprayed by means of flat jet nozzle(s) into fluidised zones of the material from above the fluidised bed, substantially in counter-current to the gas current which forms the fluidised bed.
2. Process according to claim 1, characterised in that two-component overpressure flat jet nozzles are used for external mixing, which are operated at a pressure of atomising gas of 2 to 6 bar.
3. Process according to claim 1 or 2, characterised in that a plurality of flat jet nozzles are used which are distributed as evenly as possible over the surface of the fluidised bed.
4. Process according to at least one of claims 1 to 3, characterised in that the bulk of the material is fluidised only in parts and these parts and, together with them, the flat jet nozzles are allowed to migrate through the fluidised bed apparatus.
5. Process according to at least one of claims 1 to 3, characterised in that substantially all the bulk material is fluidised in the fluidised bed and the flat jet nozzles are allowed to migrate over the fluidised bed.
6. Process according to at least one of claims 1 to 5 for processing a feed additive containing zinc bacitracin, characterised in that, in the fluidised bed apparatus, a specific bulk of 200-300 kg of starting material is processed per m2 of perforated base, and the granulating liquid used is a 4 to 6% by weight aqueous solution of methyl cellulose.
7. Fluidised bed apparatus having a container (2, 6), a perforated base (4) arranged in the container (2) for carrying powdered material, a device (12, 14) arranged underneath the perforated base (4) for introducing fluidising gas through the perforated base into the material and at least one spray nozzle (26) arranged above the perforated base (4) for spraying granulating liquid, as well as means for conveying the granulating liquid to the or each spray nozzle (26), characterised in that the or each spray nozzle (26) is a flat jet nozzle which is arranged in an upper part of the container (6), which is located above the fluidised bed formed when the apparatus is operated as intended, and which is arranged so that its direction of spraying is substantially downwards towards the fluidised bed.
8. Fluidised bed apparatus according to claim 7, characterised in that the or each spray nozzle (26) is a two-component overpressure flat jet nozzle with external mixing.
9. Fluidised bed apparatus according to claim 8, characterised in that the or each flat jet nozzle (26) is designed for a pressure of atomising gas of 2 to 7 bar and for a pressure of 0.2 to 3.0 bar in the granulating liquid which is to be atomised.
10. Fluidised bed apparatus according to claim 8 or 9, characterised in that the or each flat jet nozzle (26) is designed for a liquid throughput, based on water, of 1.5 to 5.0 l/min.
11. Fluidised bed apparatus according to at least one of claims 7 to 10, with a container (2, 6) of substantially circular cross-section, characterised in that the or each flat jet nozzle (26) is arranged with its spraying area directed substantially radially, the spraying area, based on the vertical central axis (22) of the container extending only on one side of said axis substantially along a radius, and the spray nozzle (26) being rotatable about the central axis of the container.
12. Fluidised bed apparatus according to claim 11, characterised in that a plurality of flat jet nozzles (26), preferably 6-12 flat jet nozzles, are uniformly distributed over the circumference of the container (2, 6).
13. Fluidised bed apparatus according to claim 11 or 12, characterised in that the flat jet nozzles (26) are mounted by means of arms (24) on a central rotation shaft (22) and optionally the supply of granulating liquid to the flat jet nozzles (26) is provided through the hollow rotation shaft (22) and the arms (24).
14. Fluidised bed apparatus according to at least one of claims 11 to 13, characterised in that, under the perforated base, there is a rotatable plate having substantially radial air passage slots which are rotatable in registry with the flat jet nozzles.
15. Fluidised bed apparatus according to at least one of claims 7 to 10 with a container of substantially circular cross-section, characterised in that a plurality of flat jet nozzles are arranged with their spray areas substantially radially aligned at approximately equal spacings over the circumference of the container.
16. Fluidised bed apparatus according to claim 15, characterised in that 6 to 12 flat jet nozzles are provided.
17. Fluidised bed apparatus according to at least one of claims 12 to 16, characterised in that the area of the fluidised bed covered by the flat jet nozzles at any time is about 10 to 25% of the total area of the fluidised bed.
18. Fluidised bed apparatus according to at least one of claims 12 to 17, characterised in that the surface of the fluidised bed covered by a flat jet nozzle is 150 to 750 cm2, preferably 600-700 cm2.
19. Use of a fluidised bed apparatus according to one of claims 7 to 18 for the build-up granulation of a powdered material and/or the coating of granules with a binder contained in a granulating liquid.
20. Use of a fluidised bed apparatus according to one of claims 7 to 18 for the build-up granulation of a powdered feed additive containing zinc bacitracin.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP4217971.8 | 1992-05-30 | ||
| DE4217971A DE4217971C1 (en) | 1992-05-30 | 1992-05-30 | Process and fluid bed apparatus for granulating and / or wrapping |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2136009A1 true CA2136009A1 (en) | 1993-12-09 |
Family
ID=6460109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002136009A Abandoned CA2136009A1 (en) | 1992-05-30 | 1993-05-27 | Process and apparatus for producing granules from powdered material |
Country Status (17)
| Country | Link |
|---|---|
| EP (1) | EP0642383B1 (en) |
| JP (1) | JPH07507230A (en) |
| KR (1) | KR950701837A (en) |
| AT (1) | ATE177343T1 (en) |
| AU (1) | AU673675B2 (en) |
| CA (1) | CA2136009A1 (en) |
| CZ (1) | CZ292794A3 (en) |
| DE (2) | DE4217971C1 (en) |
| DK (1) | DK0642383T3 (en) |
| ES (1) | ES2130270T3 (en) |
| FI (1) | FI945618A0 (en) |
| GR (1) | GR3030318T3 (en) |
| HU (1) | HUT68286A (en) |
| NO (1) | NO944581D0 (en) |
| NZ (1) | NZ253083A (en) |
| RU (1) | RU2131295C1 (en) |
| WO (1) | WO1993024215A1 (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19531782A1 (en) * | 1995-08-30 | 1997-03-06 | Basf Ag | Free-flowing granules based on organic acids, process for their preparation and their use |
| FR2748393B1 (en) * | 1996-05-10 | 1998-09-11 | Sogeval Lab | PROCESS FOR THE TREATMENT OF PULVERULENT ACTIVE PRINCIPLES AND MIXTURE, IN PARTICULAR ANIMAL FEED CONTAINING ACTIVE PRINCIPLES THUS PROCESSED |
| DE19621930C1 (en) * | 1996-05-31 | 1997-12-11 | Degussa | Process for the preparation of an animal feed additive based on fermentation broth |
| FR2791905B1 (en) * | 1999-04-09 | 2001-09-14 | Toulouse Inst Nat Polytech | PROCESS FOR COATING AND FILMING OF FINE POWDERS IN A FLUIDIZED BED COVER |
| US20020035107A1 (en) | 2000-06-20 | 2002-03-21 | Stefan Henke | Highly concentrated stable meloxicam solutions |
| DE10161077A1 (en) | 2001-12-12 | 2003-06-18 | Boehringer Ingelheim Vetmed | Highly concentrated stable meloxicam solutions for needleless injection |
| US8992980B2 (en) | 2002-10-25 | 2015-03-31 | Boehringer Ingelheim Vetmedica Gmbh | Water-soluble meloxicam granules |
| EP1568369A1 (en) | 2004-02-23 | 2005-08-31 | Boehringer Ingelheim Vetmedica Gmbh | Use of meloxicam for the treatment of respiratory diseases in pigs |
| JP2009510007A (en) * | 2005-09-30 | 2009-03-12 | ベーリンガー インゲルハイム フェトメディカ ゲゼルシャフト ミット ベシュレンクテル ハフツング | Pharmaceutical preparation containing meloxicam |
| DE102007025442B4 (en) * | 2007-05-31 | 2023-03-02 | Clariant International Ltd. | Use of a device for producing a coated catalyst and coated catalyst |
| CN102647971B (en) | 2009-10-12 | 2016-03-16 | 贝林格尔.英格海姆维特梅迪卡有限公司 | For comprising the container of the compositions of meloxicam |
| AU2010347598B2 (en) | 2010-03-03 | 2014-11-27 | Boehringer Ingelheim Vetmedica Gmbh | Use of meloxicam for the long-term treatment of musculoskeletal disorders in cats |
| US9795568B2 (en) | 2010-05-05 | 2017-10-24 | Boehringer Ingelheim Vetmedica Gmbh | Low concentration meloxicam tablets |
| JP5950533B2 (en) * | 2010-11-12 | 2016-07-13 | 大日本住友製薬株式会社 | Fluidized bed equipment |
| CN107048450A (en) * | 2017-06-10 | 2017-08-18 | 文松 | A kind of improved fodder granulating machine |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3382093A (en) * | 1965-11-22 | 1968-05-07 | Battelle Development Corp | Fluidized bed coating of fragile bodies |
| EP0331111B1 (en) * | 1974-05-17 | 1991-01-23 | Herbert Hüttlin | Fluidised-bed apparatus, particularly for granulating pulverulent material |
| DE2932803C2 (en) * | 1979-08-13 | 1986-12-04 | Herbert 7853 Steinen Hüttlin | Fluidized bed apparatus |
| DE3422782A1 (en) * | 1984-06-20 | 1986-01-02 | Boehringer Ingelheim Vetmedica GmbH, 6507 Ingelheim | ZINKBACITRACIN CONTAINING FEED ADDITIVE |
| SE8501365L (en) * | 1985-03-20 | 1986-09-21 | Lejus Medical Ab | PROCEDURE FOR GRANULAR TRANSFER; PILLS AND TABLETS |
| DE3725946A1 (en) * | 1987-08-05 | 1989-02-16 | Boehringer Ingelheim Vetmed | STABILIZED FEED ADDITIVE AND METHOD FOR THE PRODUCTION THEREOF |
| US4875435A (en) * | 1988-02-24 | 1989-10-24 | Warner-Lambert Company | Fluidized bed dryer/granulator |
| DK161743C (en) * | 1989-07-03 | 1992-02-17 | Niro Atomizer As | PROCEDURE AND APPARATUS FOR AGGLOMERATION OF A POWDER-SHAPED MATERIAL |
-
1992
- 1992-05-30 DE DE4217971A patent/DE4217971C1/en not_active Expired - Fee Related
-
1993
- 1993-05-27 KR KR1019940704408A patent/KR950701837A/en not_active Application Discontinuation
- 1993-05-27 HU HU9403418A patent/HUT68286A/en unknown
- 1993-05-27 JP JP6500192A patent/JPH07507230A/en active Pending
- 1993-05-27 RU RU94046213A patent/RU2131295C1/en active
- 1993-05-27 AT AT93912801T patent/ATE177343T1/en not_active IP Right Cessation
- 1993-05-27 WO PCT/EP1993/001328 patent/WO1993024215A1/en not_active Application Discontinuation
- 1993-05-27 AU AU43183/93A patent/AU673675B2/en not_active Ceased
- 1993-05-27 CZ CZ942927A patent/CZ292794A3/en unknown
- 1993-05-27 CA CA002136009A patent/CA2136009A1/en not_active Abandoned
- 1993-05-27 NZ NZ253083A patent/NZ253083A/en unknown
- 1993-05-27 ES ES93912801T patent/ES2130270T3/en not_active Expired - Lifetime
- 1993-05-27 EP EP93912801A patent/EP0642383B1/en not_active Expired - Lifetime
- 1993-05-27 DE DE59309436T patent/DE59309436D1/en not_active Expired - Fee Related
- 1993-05-27 DK DK93912801T patent/DK0642383T3/en active
-
1994
- 1994-11-29 FI FI945618A patent/FI945618A0/en unknown
- 1994-11-29 NO NO944581A patent/NO944581D0/en unknown
-
1999
- 1999-05-27 GR GR990401405T patent/GR3030318T3/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| NO944581L (en) | 1994-11-29 |
| EP0642383A1 (en) | 1995-03-15 |
| KR950701837A (en) | 1995-05-17 |
| JPH07507230A (en) | 1995-08-10 |
| RU94046213A (en) | 1996-10-27 |
| NZ253083A (en) | 1996-11-26 |
| HUT68286A (en) | 1995-06-28 |
| ATE177343T1 (en) | 1999-03-15 |
| ES2130270T3 (en) | 1999-07-01 |
| FI945618A (en) | 1994-11-29 |
| NO944581D0 (en) | 1994-11-29 |
| GR3030318T3 (en) | 1999-09-30 |
| DK0642383T3 (en) | 1999-09-27 |
| WO1993024215A1 (en) | 1993-12-09 |
| EP0642383B1 (en) | 1999-03-10 |
| DE4217971C1 (en) | 1993-10-21 |
| FI945618A0 (en) | 1994-11-29 |
| RU2131295C1 (en) | 1999-06-10 |
| AU4318393A (en) | 1993-12-30 |
| DE59309436D1 (en) | 1999-04-15 |
| CZ292794A3 (en) | 1995-04-12 |
| AU673675B2 (en) | 1996-11-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FZDE | Discontinued |