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Patent 2139766 Summary

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(12) Patent Application: (11) CA 2139766
(54) English Title: METHOD FOR FILTERING A PRODUCT FORMED IN CAUSTICIZATION
(54) French Title: METHODE POUR LA FILTRATION D'UN PRODUIT FORME LORS DE LA CAUSTIFICATION
Status: Dead
Bibliographic Data
(51) International Patent Classification (IPC):
  • D21C 11/04 (2006.01)
  • D21C 11/00 (2006.01)
(72) Inventors :
  • HEITTO, PERTTI (Finland)
  • HELSTO, JAAKKO-JUHANI (Finland)
  • VARTIAINEN, NUUTTI (Finland)
  • VARTIAINEN, TIMO (Finland)
(73) Owners :
  • LAROX OY (Not Available)
(71) Applicants :
(74) Agent: MARKS & CLERK
(74) Associate agent:
(45) Issued:
(86) PCT Filing Date: 1993-07-06
(87) Open to Public Inspection: 1994-01-20
Examination requested: 1999-10-04
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/FI1993/000287
(87) International Publication Number: WO1994/001617
(85) National Entry: 1995-01-06

(30) Application Priority Data:
Application No. Country/Territory Date
923127 Finland 1992-07-07

Abstracts

English Abstract






The invention concerns a method for filtering a product
formed in a causticization process, in which filtration
process the product is subjected to separation of the
filtrate from the solids. The product received from a
causticization tank is routed to a filter, where the filtrate
is separated from the product to be filtered and the solids
content of the remaining solids cake is increased by drying
the cake, after which the cake is washed with water and
dried. The invention is characterized in that the filtrate
separated from the product in the filter is combined with the
washing filtrate obtained from the washing and drying steps
of the filtration process, and the primary liquor this
obtained is routed into a digester for use as cooking liquor.


Claims

Note: Claims are shown in the official language in which they were submitted.




Claims:

1. A method for filtering a product formed in a
causticization process, in which filtration process the
product is subjected to separation of the filtrate from
the solids in a manner in which the product received from
a causticization tank (11) is routed to a filter (12),
where the filtrate is separated from the product to be
filtered and the solids content of the remaining solids
cake increased by drying the cake, after which the
cake is washed with water and dried, c h a r a c t e r -
i z e d in that the filtrate separated in the filter
(12) from the product is combined with the washing
filtrate obtained from the washing and drying steps of
the filtration process.

2. A method as defined in claim 1, c h a r a c t e r -
i z e d in that the filtrate removed from the product in
the filter (12) is white liquor and the washing filtrate
obtained from the washing and drying steps of the
filtration process is weak white liquor.

3. A method as defined in claim 1 or 2, c h a r a c -
t e r i z e d in that the filtrate proper and washing
filtrate are routed either separately or combined into a
storage tank (13) and therefrom further into a digester
for use as cooking liquor.

4. A method as defined in any foregoing claim,
c h a r a c t e r i z e d in that the amount of wash
water used in the filtration process is in the range of
0.8-1 m3 of wash water per ton of dry lime sludge.



5. A method as defined in any foregoing claim,
c h a r a c t e r i z e d in that the primary liquor
formed from the filtrate proper and the washing filtrate
has a concentration in the range of 90-110 g/l (Na2O).

6. A method as defined in any foregoing claim,
c h a r a c t e r i z e d in that said filter (12) is
most advantageously a pressurized filter.

Description

Note: Descriptions are shown in the official language in which they were submitted.


D~c-20-1s94 12: 34 FROM OY HE I NRNEN RB TO 99016132308821 P .08/28
wo 94JOlGI7 2 1 3 9 7 6 ~



kSE~D FOR ~ILTERING A PRO~T FORII~ IN C~USTICIZ~TION

The pre~ent invention rel~tes to a me~od according ~o
the preauible of claim 1 for filteri~g a product ~o~med in
causticization.

The cooking lic~uor reqrlired in the dige~io~ proces-~ of a
Q~fate cellulo3e plant is mos~ generally prepa~e~
accord~ng to the following ~che~ne.

g~Qe~en~ to the cookang o~ the cellulos~ c raw m~terial
wit~h ~hite liquor, t~le pulp i-~ washed and the ~ookin~
liquor with waqh waters is recovered ~co~u~only called
weak hl ~çk lic~lor) . The weak b~ ack liquor i~ dewater~d by
~5 e~apora~ion ~d thus obt~i~eA he~y bla~ li~or is
bur~ed in ~ ~o~ recovery ~ n ~ ce . The molte~n ~melt
formed onto ~he -~oda I ~_ov~ry ~u~nn~oe ~ottom, consis~ing
p~nn~r~ly o~ sodi~m sutfide ~N~S) and ~odsum car~on~te
(~a2C03~, is taken out in a ~ontrolled m~r~ and di.q-
~ol~ed lnto wa5h wa~ters recovered ~rom s~sequent s~ages
of the proce~. The ~lution thu~ obtained is called
green or fresh liquor, also fre~h liquor. The green
liquor is clarified a~d the sludge ~hus o~tained iQ
~ e~ to re~over con~ained chemicals. The ~pent w~; ng
liquid i~ routed ~o the wea~ l~quor stora~e t~nk for use
ln the dissolut~on of the ~melt obtained ~rom the furna~e
ou~u~ .

The clarified green liquor is prep~red into white li~u~r
3~ for digestion through a ~wo-stage process.

~ir-~t, s1~kin~ of lime ls ~erforme~ in a unit ~alled ~ime
~laker w~ere lime (~aO1 is a~ded to the clarified gree~
liquor, whereby ~he lime rea~t~ wi~h th~ water contained
in the ~een liquor there~y ~orming slaked lime (Ca(0~)2)
a~ordin~ to ~he follow~ n~ reaction formula:

DEC-20-1994 12: 35 FROM OY HEIN~NEN R~ TO 990161~ 8821 P. 09/28
WO ~4~01617 2 1 3 9 7 6 ~ Pcr~93~002g~



C:aO + H20 ----> ~a ~OH~ 2

~rl the c~usticization pr~ce~s the calt:i~m hydroxide
(Ca (0~) 2~ fo~med as descri~ed abo~e i rea~ed ~ith
S sodium c~hon~te ~Na2C:03) con~in~ in t~e green li~or,
where~y 80~um hydroxide ~NaO~I) and calcium ca~ ~ona~e
~caCO3), al~o called slake lime, are formed al:cording t:o
thë following ~o~

C:a ~0~) 2 I Na2C:03 ~ 0~ I CaC03

~rhe Gausticization reac~-io~ starts irl the lime slaleer a~d
is con~ ci in mul~ple ~-3 pcs.~ causticiz~ion
c:ontA; ~r~ wherefrom the reaction products are routed to
15 a sock-type wh:~te liquor filter or arlother type of
clarifier. ~e filtra~e from the fil~er is the cooking
~ iquor (i . e ., white li ~uor) which is roul~ed to a s~orage
tan~, aLnd furth~r, to the cligester. The o}~tA~ ned white
liquor has a ca ~y o~er of ~ ~ 30 ~ of ~he a~ti~e
~odium in t~e form of ~a2S which, ho~e~er, h~-~ no
detri~ental e~fe~t on the -~u~equent reactions.

The filter ~otto~ di~char~e normRlly o~ n~rl as a
30-40 % solids cont~ning -~ludge i8 filtered in the lime
~S s~udge wns~i~g filter who~e filtrate is ~he weak ~hite
liquor tha~ is routed ~ia a storage ~ank to a dis~olution
tank. The l~e slud~e fonming the bot~o~ di~rharge is
routed via a storage tank to, e.g., a lime slu~ge ~ilter
o$ the crum ~ er type w~re ~he lime sludge is ~ashed
and r~ied. The filtrate proper and the was~ filtrate are
u~ed for, e.g., diluting the ~ludge entering the lime
sludge w~ch;ng ~ilter, whi~e the ~ried l~me sludge is
route~ to the rotary li~e kiln.

~he l~me -~l~dge is incinerated wit~ the help of an
~ iary fuel ~oil, gas, et~.) in a xotary lime kiln,

DEC-20-1994 12:35 FROM OY HEIN~NEN RB TO 9g0161.~ 8W1 P.10/28
w~ ~u~1617 P~T/~3/00287
213~7~ S


whereby calcium oxide and carbon dioxide are fon~ed
according ~o the follow~ng formula:

C:a¢03 ~~~~ ¢~ + C2
s




The bur~t l~e (CaO~, ~ith makeup lime added to compen-
sa~e for ~ l lo8-~es~ ig u~ed in ~austic~zation.

In the above-de~cri~ed method the ~eak white li~or
0 rou~ed to t~e di~so}ution tank con~ains ~aO~ whi~h i5
there~rom c~ eyed to the caus~icizatio~ reaction. As
known in the art (~f. e.g. Sympo ium ~or ~eco~ery of
Pulping Ch~mical~; K. ~in~n~ Unter~l~rhl~n~en zur
Kaustizierung ~on Gr~nl~ en~, the in~oduc~ion of
1~ existing ~dium hydroxide into the caus~i~iza~on
rea~tion is detr; ent~l to the rea~ion.

It is an object of the present in~ention to simplify the
causticiza~ion proce~s in a m~n~_ in which the weak
20 cooking liquor, u~h resul~s from concurrent caus~ici-
zation proc:e . ses and i~ known ~o be detriment~l to the
cau~tic:iza~ion proc:ess, need not be returned ~o the dis-
so}ution tank of t~e soda reco~rery furnace cixcui~ for
weak alkali ,eco~,~ry, ~ut rather, ~he ~ ; ne .~olution
resulting from WA~h; ng wi~h a smal~ amount of warm water
in a f~ er can be c:om~ined with the main circulation o~
the coo3c~ng li~uor, i.e., the pr~mary li~id cont~
u~eful white li~uor at a ~oncen~r~tion o~ approx. g0-
110 ~Jl (Na~O~.
~o
The me~hod a~cor~ing to the prese~t in~en~ion aims at
o~er~oming the a~ove-described dr~w~acks and to sim~lift~
~he pro~ess in a m~nner whic:h pe~i~s omicsion of a
~ignifi~ant portion of equipment needed in conçurrent
pro~esses. Separation o~ white liquor, as wel~ as wasning




and ~ub~equent dry~ng of ~he lime sludge, take ~l~ce in a




~C-20-1~4 12:~ FRO~ OY HEIN~NEN ~ TO 9~161.~ 08R~1 P. 11/28
WO 94/01617 PCI~/FI93/l~
2139766


single pro~e-~s st~ye. The characteri~ing propertie~ o~
the method accor~i~g ~o the in~en~ion are di~clo-~ed in
the Anne~ed c~ c.

Accordi~g to the i~ention, the white liquor and l~me
sl~dge recei~red ~rom ~he causticization tank~ are ~outed
~ a filter, most adv~ntageo~sly a pr~surize~ filter~
wherefrom the ~hite liquo~ o~tA; n~ as ~iltrate is routed
to a sto age tank an~ fur~her to the digester. The solids
content of the lime slud~e cake -;n;ng in t~e ~ilter
is high, which means a low d~O~ o~ white liquor to be
washed away from the cake.

~ter filtering i5 completed, the lime ~udge c:ake still
15 rer-~n;n~ in the filter is w~ . Ow:~g to the high
-qoli~ co~tent ~f t~e l~e -~lu~ge cake, a good w~in~
re~ult c~n be at~ using or~ly ~ ~mall ~ -L of ~arm
water . Thus, the 3mall ~ou~t of filtrate from we~ ; n~,
that i_, of the weak w~ite liquor c:~ be rou~ed ~ nto the
20 stora~e tank of white liquor alre~dy sepàrated in the
riltration s~-a~e.

Ater f~lterin~ and w~-~hi~, the lime slud~ cake ~an ~e
~rther dried by, e.g., blowing co~preQQe~ air throu~h
2~ . it. Subse~uent to t~e-ee steps the lime sludge cakes are
~ ed from the ~i~ter and ~onveyed to ~n~ineration in
the rctary lime kiln.


By virt~e of the above-de~ribed method, the filterin~,
w~shing an~ dryin~ of the lime sludge can achieve
complete el~miA2tion of the pre-exi~ting sodium
hydroxide, which otherwi~e ~ould ~e c~rried over to ~he
~issolution of the smelt and subse~uent aetrime~tal
transfer i~to the cau~tirization pro~ess.
3~

DEC-20-1994 12:36 FROM OY HEINRNEN RB TO 990161.~ U8f2~1 P.1~/28
~ U~OI / PC~/~ JO~1287
~1397~


The ~ethod according to ~he inventio~ achie~es a simpler
and more e~fective causticization process o~r conven-
tional techniques, ~in~e unnece~axy circul~ions o~
liquids are ~im;n~ted and the number of re~ining ~ir-
S cula~ions is thus &~nifi~antly s~ller than tho-~e nee~ed
in pr~or art. Moreover, ~e abo~e-discusqed benefitQ also
o~fer essential ~pro~ements in the form of reA~C~A
en~ironment~

1~ T~e invention i~ next ~inO~ in sreater de ail with the
help of an excmp~ify~ng em~odiment ~y ~yking reference 'o
the attached draw~g (Fig . 1 ) ~howing ~he ~chematic
prin~iple of a plant acco~ding to t~e pre~ent in~ention.

Smelt recei~ecl ~rom a Qoda recovery furnace ~1 ) is routed
~o a di:3~olution tank ~2~ where it i~ cliRQol~red in wa~er
or any suitable rec:ycled proc~eQ~ wat-er o~ the f ac~o~ .
Therefrom the -~olution i5 routed via an ec~salizin~ ~a~k
(3) to a green liquor ~:larifier ~4). The slu~ge obtained
~o as t~le bottom disçharge of tb,e clarifier (4) is fil~erecl
ar~d washed in a green lic~uor filter (~)~ The liquid
~iltrate t.hus ob~inf~ can ~e u~ed from~ e g. ~ a ~uffer
storage ~ 6) for dis~solYin~ the Qmelt, while t:he ~olids
are removed 2g waste ( 7 )
2s
The ~:larii~ie~ green lit~u~r i routed toge~her with 1~ me
(8~ O~t~neA from the rotary l~me kiln, po-~2sibly
c:o~le~ented with makeup }ime ~9), ~n~o a l:Lme slakin~
tan3c (10 ) . The calc:ium hydroxide ~ormed in the lime
30 slaking rea~:tion reacts wit~ sodium c:ar~onate to forn
sodium hydroxide and ~alc~ arbonate, ~hat is, lime
sludge. The latter reaction takes place in causticization
tanks ~11) loc:ated after the lime sludge slaker (lO).

In the next pro~e~ ~teps accor~ing to the in~ention, the
calcium ~ar~onate and sodiu~ hydroxide recei~ed from the

DEC-20-1994 lZ:37 FROM OY HEINRNEN ~ TO 990161~ 8~1 P.13/28
W O 94/01617 2 1 3 9 7 ~ ~



cau~ticization t~ks are routed to a f~ t:er (1~), where
the solids cc~nten~ of ~he c~e ~o~med durin~ filtr2tion
is increa~ed ~y compre-~8ing the cake with the help of a
pressurizec} med~ act:Lng via a ~er membrane. The fil-
trate obtained from the filter is white liquor, which is
rollted ~ia a white liquor stora~7e tank (13) to t;he
dis~e~er ~

S~seque~t to the co~p~ession ~3~age, the calce 801id~ con-
10 tent i~ approX . 75 wt-S~ at the star~ of the W:~ ch; '''~ step .
Con~e~uen~ly, t~e wa~hing 8tep can ~e c~rried out usi~g a
very 8m~11 amOl~l't: of wash ~Tater whe~ comparecl to conven-
tional tech~iques. ~n the me~hod ac~ording to the inver~-
tion, the ~mount of wa--h water requi~ed is in the ra~s~e
of 0 . B-l m3 w~s~t ng water per ton of d~y llrne sludge .

After w:~3h ~ng, the -~olids calce i~ dxied by repea~ l;he
compre~Qion st~p via ~he r~be~ mç~ra~e in the ~o~re-
deQcri~ed ~ n~er, complemented ~ith add~ tional d~y:~g by
20 blowing com~resQed gas ~ypicall~ cG~r e-~-Qed air) through
the cake. The ~ma11 amount of riltrate o~tained from the
w:~qhin~ ~tage and ~3ub~equent drying !3t;a~s, c:om~rised of
w~ite liquor~ is routed into t.~e ~hite liquor cirCul atio~
( 13 ) and the~e~rom ~urther into the di~ester .
After drying, the 1ime sluclge cak~s are r ~ov~d from the
~i~ter into a !3torage tank ~14), wherefrom t~ey are
further conveyed into a rotary l ime kiln (15) . In ~he
rotary lime ~ciln (15) the c:al~ m carbonate ~ s in~::iner-
30 a~ed a~d ~he ca1cium oxide ~-b,~s formed is routed to a
lime storage t~nk (8) for u~e in the cauctici~ation
rea~tior~ ~

In practice, the a}~ove-de~cri~ed method entirely prevents
35 pre-exis1~ing sodium hydroxide ~rom reach~ ng the c;austici-
zation reaction, thus si~nificantly impro~ring the

DEC~ 1994 12:37 FROM OY HEINRNEN RB TO 990161 ~;~.sl~8~3~1 P. 14/28
WO g4/01617 2 13 9 7 ~ ~ ~C~/F1~3/00~87



reaction conditions. Owing tc: t~e e~iciency of th~
er empl oyed, most advan~ageouLly a pressurized
fi}ter, re~uc~e-i water cor~ tion is at Pine~ and wAshing
can be per~o~ed using proce~ waters obt~ ~A from,
e . g ., ~he e~aporatio~ stage .

For those ver ed in th~ art it i~ e~icleslt that the dif~e-
rent ~le~entations oi~ the invent~ c~n are no~ ted by
~he exem~lifying em}~otiment descri~ed a~ove, bu~ instead,
10 it can be varied within the c:ope of the ~n- r~ed cla~ms .

Representative Drawing
A single figure which represents the drawing illustrating the invention.
Administrative Status

For a clearer understanding of the status of the application/patent presented on this page, the site Disclaimer , as well as the definitions for Patent , Administrative Status , Maintenance Fee  and Payment History  should be consulted.

Administrative Status

Title Date
Forecasted Issue Date Unavailable
(86) PCT Filing Date 1993-07-06
(87) PCT Publication Date 1994-01-20
(85) National Entry 1995-01-06
Examination Requested 1999-10-04
Dead Application 2003-10-20

Abandonment History

Abandonment Date Reason Reinstatement Date
2002-10-21 R30(2) - Failure to Respond
2003-07-07 FAILURE TO PAY APPLICATION MAINTENANCE FEE

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1995-01-06
Maintenance Fee - Application - New Act 2 1995-07-06 $100.00 1995-05-10
Registration of a document - section 124 $0.00 1995-08-10
Maintenance Fee - Application - New Act 3 1996-07-08 $100.00 1996-05-29
Maintenance Fee - Application - New Act 4 1997-07-07 $100.00 1997-06-02
Maintenance Fee - Application - New Act 5 1998-07-06 $150.00 1998-06-10
Maintenance Fee - Application - New Act 6 1999-07-06 $150.00 1999-06-30
Request for Examination $400.00 1999-10-04
Maintenance Fee - Application - New Act 7 2000-07-06 $150.00 2000-05-31
Maintenance Fee - Application - New Act 8 2001-07-06 $150.00 2001-05-24
Maintenance Fee - Application - New Act 9 2002-07-08 $150.00 2002-06-20
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
LAROX OY
Past Owners on Record
HEITTO, PERTTI
HELSTO, JAAKKO-JUHANI
VARTIAINEN, NUUTTI
VARTIAINEN, TIMO
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Representative Drawing 1999-04-14 1 8
Cover Page 1995-09-13 1 16
Abstract 1994-01-20 1 22
Description 1994-01-20 7 268
Claims 1994-01-20 2 46
Drawings 1994-01-20 1 14
Assignment 1995-01-06 9 324
PCT 1995-01-06 20 683
Prosecution-Amendment 1999-10-04 1 32
Prosecution-Amendment 2000-04-03 1 27
Prosecution-Amendment 2002-06-20 3 132
Fees 1996-05-29 1 54
Fees 1995-05-10 1 62