Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
1~1 N~V '94 1:3: 34 GOERTZPf~TENT P. 3/4
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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
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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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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$u~ o~ a cos~t~iner, chould
be ~ ltnrs~tely a~ ere~t ~pacin~ fra~ the
c~nt~e of the Container i~ ~uc~ a ~y t~a~ ehe m4~t
mlfonn ~pr~y d~it~ibution po~ible i~ a~i~ved over the
~luldi~ed ~atd.. Bao~ on the ~otal ~ur~ac0 ~rea o~ t2~o
~luidi~e~ bed a ~pr~y de~lty of betv~
3 l/m2.min, l?Fefer~ly ~etween 1.2 auld l.S l/ma.m~n ha~
pro~od ~ultd~lo.
To produ~e the ~luldl6~d ~d, quanti~ ~ of gao ~angin~
rran 10-60 n~ o~ ~er$orated ~a~e ~atte prov~
suitablo. The proceH~ ~ccor~ing to the $nv~n~ ha~
th~rerore p~ov~d partlcu~arly econc~acal i~ th~6
re~ ct. I~like ~y lcno~n ~th~e, t~e proc~s~
according to th~ invention i~ not ~arelcula~ly af~ected
by wheth~r e~e cu~ent o~ ~luidl~ny ~a~ tl~rough ~he
per~orated ba~- 1B generaeed by ov rpres~ure belo~ the
p~rfor~ted b~e or by ~de~-pre~;su~ above ~he.
or~t~d b~-. 'rher~o~, ior generat~g t~e ga~
currc~t, elt~r ~ pr-~cur0-generAting bl4 -~r may b~ :
~ro~ided in the Sl~ ch~er ~ w the per~or~t~d ~se or
a ~uctlon blow ay se pro~do~ ln the pr~u~t op~ce
a~o~re the ~luiaised ~ed,.
~a~; prcc~a~irg the ~eed add~tlv~ ~u~d ln t~e
ex~er~luents, good re~ults were ol~ined by ope~atin~
with a ~peeific pe~ora~s~?l ba~e lo~l o~ 200-300 kg o~
pow~er~d o~rting ~terial ~ n? o p~oro.ted ~a~e. In
~'
:
,;: . ~ . - :
~1 f3 6 ~
~19 NOV '94 lZ: 47 GOERT~PRTENT P. 10~2
- 12 -
t~lo par~loul,ar ~n~tance, the ~luidi~l~g gas u~ed ~as
nitrogen, whieh ~a~ at a ee~erature in the range fronn
90 to ll~-C, pre~ably 104~C, on ~t~ing t~
5~anulating ap~ tu~ d~r~d m~t~rlal wae be~t~d
~o a ~e~p~ tu~e alx~ve 70-C, p~t~ral~ly BD-C, ~or~ tho
~tart o~ ~prayin~. ~e ~ollo~ring i6 a ~e~cription Of
t~e ba~lo c~-~ructio~ o~ ~ etnbodi~ent Or a fluldioo~ -
bed app~r~tu~ accordlng t~ th~ ln~r~ntlon, r~orrinS~ to
the accon~anyirlg ~raw~ng~, vher6~in:
~ig. 1 ~8 ~ diagran~atic ~rertlcal ~ection th~:ough the
inlportant c~ponent~ ~ the apparatu~
~1~. 2 i~ a diagrammatlc }~ori~onta~, sec~o~ through
' ~pp~AtU~s~ ~ the di9t~$~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
- 13 -
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 :
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