CA2024975A1

CA2024975A1 - Active sizing compositions

Info

Publication number: CA2024975A1
Application number: CA002024975A
Authority: CA
Inventors: Lawrence F. Watson
Original assignee: Individual
Current assignee: Solvay Solutions UK Ltd
Priority date: 1989-09-11
Filing date: 1990-09-10
Publication date: 1991-03-12
Also published as: BR9004518A; JPH03167391A; NO903926L; NO903926D0; ZA907216B; FI904444A0; AU6231790A; EP0418015A1; FI904444A7; GB8920456D0

Abstract

ABSTRACT
ACTIVE SIZING COMPOSITIONS
The compositions comprise an aqueous emulsion containing a ketone dimer reactive sizing agent and an anionic dispersant or emulsifier such as sodium lignosulphonate, calcium lignosulphonate or the sodium salt of naphthalene sulphonic acid. In addition an extender or modifier such as an anionic polyacrylamide, an anionic starch or colloid silica can be present to extend or modify the anionic charge density of the composition. The compositions are particularly effective in sizing systems containing cationically charged fillers, or cationic additives such as certain retention aids and fluorescent whitening agents.

Description

202~;37~

., ~
r AC~IVE 8I~ING COMPOSI~IONS
~ hlz lnv~nt~on rel~taz to actlv~ lze- cont~lnlng a r-~ctlv~ ~izlng Ag~nt and ~-'di~p-r-~nt.
For oonv~ nc-~ the t-rm "papor" i~ u~-d ln thl~
5 Jp~Ci~lo~t~on to mean ~ny fo~ o~ paper~ paporboard and r~lat-d produot~, tho manu~a~ture of w~lch lnvo~vs~ the ~ctlon o~ a ~ ~lng ag-nt upon c~llulo~lc or other f lbr-~, Tradltlonally, paper ha~ b--n ~lzed ~lth ro~ln in 10 co~unctlon w~th ~lum, whlch act- a~ a pr-clpltant More reo-ntly, r-actlv~ ~lzo~ ~av~ been lntroducod, in wh~ch a ~lzlng ag~nt reaot~ dlr~ctly wlth ~h~ c-llu108~
of th~ paper On~ cla~ o~ re~ctlv ~lze~ ln common u~ th- koten~ d1 m~r 61z~ Thece ~re typl~ally 15 u~-d an mul~lon~ ln wat~r in con~unotlon w~th dl~p~ nt~ ~nd omul~lfl~, whlch ~erve to ~t~bll~
tho o~ul~on Pr-vlou~ ket~no dlmer 81~e~ hAVe cont-ln-d, a~
dl~per-ant, o~tlonlc componant~ ~uch a- ~ta~ch~, 20 polyaDItne-~ polyamlde~ and polyacryl~mldo~. Th~s~
emul~ r~ and dl~pcr~nts aro ho~og-nl~od ln ~itu wlth the kotene dlmer to ~orm c~tlonlc~lly ~t~blllsed emul-lono Whll~t ~tloactory ln m-ny ~p~llcat~on~, ~h- known 2S cat~on~cally ~tnbll~ed k~ton- dl~er ~lzo~ ~lvo rl-~to pro~l-m- ln c~rtaln ~ppllcatlon~. Sn partlcular, co~ln g~d-- o~ p~p-r ~or ll~uld paok~glng and th~
manu~notur~ o~ photogr~phic p~p~r- 1AVO1~e, in th~ir manu~aotur~, th~ u-- of large quantltl-~ of catlonlc 30 poly~mlde amln~ ~pichlorohydrln ~ln, in ord-r to pro~uce ~vou~abl- we~-~tr-nqth propertl-- ln the ~lnlsh-d pap~r. Tn a wot-ond proco~s, tho reoln is no~lly ~dd~d to ~ho th~ok~tock. The r~ln ha~ a hlgh ~ub~t~ntlvlty to cell~lo~e, ~n ord-r to produce 3S ufflcient cover~ge Or th- flbr- Thc ~ntroductlon o~

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~urth-r oatlonlc componQnt~, ~uch a~ ~tarch, dry-~tr~ngth ro~ln and cAtlonically sta}~ utene dlmer ~ze a~n lcad to poor retention of tbe component~ b~
th~ collulo-- and result ln ~low drainag~, poor 5 ~tr~ngth prop~rtlo~ ~nd low Jlz~ng ef~lolenoy. ~ ~
~robl-m~ c~n al~o arl~ u~aco slzlng ~ ~ ;
proc-~e~, partloul~rly becau~ trend in the ~ :
m~nuSactUrs o~ ~lnn ~peci~ y paper3 ls to apply th~
~ntionlc ~t~roh-~t~bil~sod k-t~n- dlm-r iz- to th~
10 su~ co o~ th- paper h--t ln con~ unctlon with a ~luoro~cont wh~t-nlng ag-nt ~FWA), Suoh ~g-nts ~re u~ually ~nionl~ in n~tur- nd thoir u~e ln oon~ un~tion wl~h c~ or~lo-llt~bllls~d slzo~ c~n l~d to ~ reductlon ln the ~-ctl~ne~ of the FWA ~nd c~u~- a ~uen~hing 15 ~S~at whloh qlve~ ri~o to a yollower p~p~r.
pr~vlll lnv~ lun pL-c~vld~ o.n ~c~ iDlng compo-lt~on whlch comprl~-~ an a~ueou~ omul~lon of a ~activ- ~lzln~ ag-nt and ~n anlo~lc dl~p~r~nt a~d/or L .
cmul~ er ~or~lng to ~t~bill~o th- mul~lon, th~
~0 ro~ctlvo ~lsln~ agont ao~prl~ln~ at lo~t one compound accord~ng to tho formula CE~ C - C~R2 O - C O ~ ','''',.
25 wh-roln ~1 and R2 a~e, ~ndopendently of oaeh other, _ - ;
hydroc~bon r~d~ cal~ bavlng at l-a~t ~lx c~rbon atom~
more prof-rably alkyl, alkenyl, cy~lo~lkyl, Aryl~
~ralkyl or alk~ryl radlcal~
Slzlng ag~nt~ of the lnventlon can o~f~r ~d~antag~
30 a~poclally ln ~y~tem~ wh~r- c~.tionlc charg-d fillor~
o.g.~ proc~pltatQd c~lclum o~r~on~te~ a~e pr-~-nt or ln ~y~t~ u~lng catlonlc compon-nt~ ~.g., r-t-neion alds o~ polyncrylam~d-, pol~amlno~ ~SI~ etc. in furni~h~ .! ;... -:
oon919tlny of gro~ndwood ~ thormom-ch~n~aal pulp~ or chemlcal th-rmomeohanlc~l pulp~ wh-ro llmlt-d hydroxyl j ..'.'., ":
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~O~ lt~s are avallabl~ for AXD'attach~nt and r~ct~vi~y, ~ o composltlon~ o~ tho lnv-ntion are partlcularly ~ultabl~ for U8- a~ an internal 3i~e ln 81zing 5 opor~tlon~ carrl-d out at the wet ond o~ a papor-making proc~
In p-rtlcul~rly proforred si~lng ~g~nt~, R1 and R2 ~re, indep~nd-nt~y o~ -~oh oth~r, C12 to C22 alkyl qroup-, C~4 to C1g alkyl gFOUp- being e~poclally 10 pr-f ~rrot. Tho oo~pouna~ ln whlch R1 and R2 aro each C14~29 or C16H33 ar- mo~t highly ~referr~d and are ror-rr-d to hereina~tor a~ "palmit~c~t-arlc dlmer".
~he l~tter co~pound~ can ~o r~gard~d a~ the cyoloaddltion pro~uct~ of on- koteno ~oloc~l~ of the 15 ~ormula R1-C~-C~O and on- koton- mol-oul- of the ~ormula R2-C~C-O~ wh-r-ln R1 And ~2 ar- o~ch C14H2g or C16H35 It h~ ~urp~l~ingly ~--n ~ound that, contrary to oxp-¢tatlono, actlve s~zlng compo~ltlonz ~acordlng to 20 ~h- tnventlon can b~ octlv~ ln th~lr olzlng prop rtle~, partlcularly when u~od in hl~hly-cationlc nvlronmonto, ~uch as tho-o encountor-d ln wot-on~
~izlng ln tb- m~nu~actur~ o~ llquld packaglng papers and photograph~c p~per~ en~on~d ~bov~, and thos~, 2S ~o m~ntionod ~bo~to, wh-n t~ ctl~ e ~ u~-d ~ n aonnection ~lth ~luoro~nt wh~ten~ng ag-nt~. In addltlon, papers u-ing c~tlonla ~ r- ~uch a~
precipltat~d calclum aarbonAte can b~ ~iz~d offlciently uB~ng ~n ~n~onlc~lly cb~rqed alkyl ket~n~ ~imo~ ~lz~ 0~
30 the P~o~ent lnvontlon. Th~t th~ oomposlt~on~ of th~
ln~n~lon a~n b- ffccl:lv- ~izlng ag-nt~ h~ mor~
~u~pri~ing booau~o lt h~- prevlou~ly b~n ~upposed ln th~ are that ~n anionlcally ~t~bll~ -d ~lzlng ~g-nt would laak th~ nQce~ary af ~lnlty wlth th- hydroxyl 35 group~ o~ tho c~llulo~ and th~t a ~tlonlcally .. . , - . .. -.. ~. .... . . . .. , .. .... . , - . :

2 ~ 7 ~ ~

stab~ ed emul3lon WaB neces~ary to provlde t~e n-c-~ary rotentlon o~ the slzlng agent by reactlon wlth th~ hydroxyl group~
The dl~par~ant andtor ~mul4lfler ~tablll81ng the n oan ba any ~ultable anionla d~sp-r~ant or omul~ , Soalum llvno-ulphonat~, calcium llgnooulphonat~ and th~ ~odlum ~alt of n~phthalene ~ulphonlc Aold, an~ m'xtura~ ~h-r-o~, ar- oxa~pl~ of ~ulta~lo dl4p-r~ant~. The dl~porsant an~/or omul~lfler 10 l~ pr-f-r~bly u--d ln a total amount o~ 0 5~ to 10~
ba-~d on tho w-lght o~ ~ho r~ctlvo slzing ag-nt, the 80tual amount u~ed ln any partlcular compo~lt~on b~lng ~h~t whlch lmpAr~ a do-~r-d an~onla char~ to th~
dl~per~ lzlng agont.
I~ d-~lr-~, th- anionlo charg- ~-n~lty ln the ~lzlng compo-~tlon- o~ th- ln~ntt on can be oxtondod or mod~lo~ u~ ng component~ such aJ anlon~c polyaorylAmldo-, anlonlc ~tarah or colloldal ~lllca as ~mul~ h- ~lzl~g agont 1~ pr-f~rably pr---nt ln 20 the sl8in~ compo~ltlon ln ~n amount o~ 5~ to 20~ by wolght, moro prof-rably 10~ to 15~ by woight, of th~
~lzlng compo~ltlon.
Th- ~lzlng compo~ltlon~ do~ d, may bo u~d ~n aoniunetion wlth offootl~- quantltlo~ of m~torlal uch 25 ~ ~ot-ntlon ~ido, dry ot~ength agont- and ~ralnag~
ai~o, for ox~mple alum ~lah aot~ both a~ a dralnage ~ld and a- a ~o-vong-~ for anlonla collo~dal dobri~
~ Th l~ln~ composltion~ o~ tho l~ventlo~ can ~-mado by ~ny con~enlent proceo~, but prafar~bly ar- madQ
30 by homogenl~i ng ~he r-activ- sl~lng agent ln llquld for~ ~f n~c~e~a~y ~fter ho~tlng to melt th~ materlal) with th~ dl~po~4~nt and/or emul-l~ler nd tho approprlato amount oi' water to ~o~m an aqueou~
emul~lon. For oxampl~, th- dl~p-r~nt ~nd/or 3S ~mul~fl~r 1~ di~-olv~d in wat-r at 65 to ~0C to which ~; ' .
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1~ added molten k~t~ne dlm-r prem-lted at 65 to 80C.
~h~ xe~ultant mlx i~ homogenlsoa at 2500 to 3500 psl to ~X
form a ~tAble emulslon.
~h- invention w~ 11 n~w be d~-crib~ ~urth-r by way i!
5 o~ ~x~r~pl~
EX~MPr E~ 1 to 4 and COMPARISON EXAMPT.~S 5 to 10 :~
In ~h- ~xp-rlmental work whloh 18 d-~crlbed h~re~:~t~ ing test~ w~-~ carrled out on a 50s50 dry w ight mlxture o~ bl~ach~d NN ~n~ SW kraf t pulp 10 which had ~o-n ~imultaneouJly be~ten to a 40SP
eQ~polnt ~n an oxperlm-ntal--cal~ v~lley ~ator. Th~ x ~1Z1Qg t--t ~mployod wa~ a 16 hour~ 1 0~ w/v lact~
aclt od~wlck t~t .~ .
15 Sa~ reDar~tlon wl~hQut r~c~r~ulatlon 1000cm3 of 1 0~ oon~l~t-ncy ~tock w~ plac~d ln a 1 500cm3 b~ak~r, to whlch th- n-c--~ary amount~ of c~emlcal~ (~ae T~bl- ~
2) w~- uad~d oqu~ntl~lly at 30-~econd lntorv~l6 u~ing ~ -p~tlo~ ~yrlng~ wlth an accuracy of ~0.1cm3, Th- 30-20 ooond ~ nt-r~ l w~ ~xt-naed to 60 ~con~s after ~ddltlon o~ the Xymene S57, ~h- pN o~E tho mlxtur~ wa~ n ad~u~t~d to 7 5 by additlon o~ oodlum blcarbonate lmmedlat-ly after addlt~ on o~ th~ ~ymon~ 557 M~xlng o~ tho co~ponent~ wao acco~pll~hed w~th a m-chanlcal ~, ~5 tlr~-r op~rat~t at 100 rp~ Sh~t- wore produoed ~rom the ~ln~l mlxture ~ n a 3rltl~h st~ndasd h~nd~h~t ~ -mould and pre~s~d ls~ ~ pn~umatlc~lly op~t~d Voith handsheet pre~ for S minutes at a pre--ure o~ 50 p~i~
( 3 ~S k ~ he sh~-t- wore t~en drl-d by pa--lng th~m 30 ~our tl~eo around a photo~raph~c drum dy~r op~r~t-d at t lOSC, givlng ~ re~id-nce ~ o o~ 3,3 mlnut~ ollowed ~
by S~0 m~nu~ ln a forc~d-draught o~ren ~t 1 05C t Aftor coolls~g ~o~ at lea~t 10 minut~, th~ she~t~ were ~ -rou~hly cut, lamln~t~d and fln~ly Ctlt to ~ flnal si~e t 35 o~ S 0 c~ x 12 5 cm i~' ' ~ ' ' 20~49 1~ ; ~

Sam~l~ PreParation wlth reclrculat~on 3500cm3 of 2 79~ conol~tenoy stook was plAced ln a ~en-lltre pall Both Kym-n- 557 ~nd AKO ~lz~ were thon add~d to thi5 S ~u~pen~lon Th- pH WA~ ad~t~d to 7 5 by addltl~n of ~odlum blc-rbonAt-. Next, ~u~lclent of thls "thlok~tock" to cont~ln lOg o~ dry fibr~ wa~ dilut~d to a tot~l Yolum~ o~ 10qOem3 Th~s r-~ulted ln a "thinJtock" havlng a conslstency of 1 03~ Next, r :
lO alum, Acoo~tron~th B5 and Staklok 400 were added to the th~n~took. ~hl~ ~hinn~d ~u~p~nslon wa~ dralned throu~h ~ Mo~m~r con~l~t~ncy apparatu~. Th- retained r solld wa~ dl~aard~ and tha ~iltrate w~ then u~-d to dllute mor- o~ tho th~ ck~tock, ~o th~t ~urth-r ~ ;
15 ~tditlon~ o~ alum, Acco~tr~ngth 8S and Staklok 400 ~1 `
aould b~ mado Thlo cycl~ o~ dilutlon, dralnage and addltlon o~ ~lum, Acco~tron~tb ~S and Staklok 400 wa~
rap~ated untll 1~ had b-en carrl~d out nlno tlmos b~fore hand~heet manu~actur-, Ju~t prlor to ~ho-t 20 ~or~atlon~ the pH wa~ galn ad~u~t-d to 7 5 ~y ad~ltlon o2 further ~odlum blc~rbonate ~horough ml~lng o~ tho compon~nt~ wa~ ~ooompll~h~d m~nually Sheet~ wero produced ~ d--crlbed ~bo~e 2g s~mDle T~t~g All ~a~pl~ w-ro w~lgh~d and th-n pl~ced 2 Scm b-low t~o ~ur~ce o~ a 1,0~ w/v lactic ~cl~ ~oluelon ~t~r 16 hour~, tho JAmp~-s were r~moved, dried ~nd row~ighed ~h- r~ult~ ar~ ~hown ~n Table t i .
,, ~~~~'~~, , .. '.';.
-.
,, ~'' ' '' ~`` 2~497~ g ~AB~E 1 :-Samplo Fluld P~ck-up ~xam~l- Di~D-r-ant Pre~sation _ ~a) 1 K-y~m~ S~1 S1 0.3860 2 K-ydim~ S~1 S2 0.4013 ~ . .

3 x.ya- m~ S~1 S3 0.4299 4 ~-ydlm- SP1 S1-~ 0.32 ~ .
Xoydlm~ D10 31 0.3612 ~ .
6 X~ydl~- D10 S2 0.40a8 ~ .
7 Roydlm- D10 S3 0.4330 a XoydLm~ D10 S1 -R 0 . 3 2 9 X ydl~o D125 S2 0.4102 Xaydlm~ D12S S3 0.4191 15 Exampl~ 5 to 10 ar- co~parlzon xa~pl~o omploying c~tionlcally-~tablli--d AR~ ~lzin~ a~nt~. ~
, ' ~ha cod-~ S1, S2, g3 and S1-R d~-cr~b~ th~ ~amp~e prapar~lon t~chn~qu-~ u~od~
Xoydl~o SPl 19 a ~loper~ant contalnlng ~odlu~ ~
llgno~ulphonat~ and th~ sodium ~alt o~ naphthalone .~ :
~ulphonl¢ acld. It l~ avallablo ~ro~ Albrlght ~ W~lson c ~lmlt~d. l~-ydl~o ~10 and Xaydlmo Dl 25 ~r- cationioally 2S tablll~d AXD ~lzing a~onto oont~lning, on a dry w-l~ht ba-l-, 10~ AXD ~h~ palmitlo-~t~rlc compound ~ ~ ~
m~n~loned abo~) and, r--poctlv~ly, 2.5~ and 1.25~ ~E ~ `
aationlc poly~-r. Xeydlm- D10 and ~y~lm~ D125 are aloo ~vallable ~r3m Albr~g~t ~ on ~lmitad~

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TA3~E 2 Addl~ion ~eau~nce S1 ~1) 8~01b/~ ~4.0 ~g/t) Xymen~ 557 ~polyam~d~ am~ne epl~hlorohydrin, .
a~aila~le ~rom ~erculo~ 20wder Co.) :~
~2) 7.01bt~ ~3.5 kg/t~ AXD ~p~lmitlc-~tea~lc dlm~r) .
t3~ 1,01b/T ~0.5 lcc/~) ~lum ~4) 4.01b/~ ~2.0 k~/t) Acooot~onyth 85 . :
1~ ~an anlo~lc dry ~treng~h agent .~
c~mpri~lng polyacrylamld~ dry polym-r on dry ~ibrc) (S) 10.0lb/~ (5.0 k~/t) Staklok 400 ~o~tlonla corn ~tarcb, avallablo from 9tal~y Man~acturlng Co.) S2 ~ .OlbJ~ ~4.0 kg/t) Xymen~ 557 : :~
(~) 7,01b/~ ~3.5 k~/t) AXD ~a~ abovo) ~ ::
~3~ 1.Olb/T ~0.5 ~g/t) alum ;
~4) 10.01b/~ ~5.~ k~/t) Sta~lok 400 . :-tS) 4,01b/~ ~2.0 kg/t) ~aao~trongth 8~
. ;.
S3 ~ S1 ~2~ 7.01b/~ (3.5 k~/~)AXD ~a~ ~bov-) and 10.101~/T ~5,Q kglt) Sta~lok 40~, :
promlxed -. ~.
~3) 1.01b/~ (0.5 kg/t) alum :.:
~4) 4.01b/T t2.0 kg/t) Accostronqth 85 ,, . ,:
S1-R an S1 but with r~clrculatlon In ~ac~ additlon ~equ~no~, the AXD w-~ ~dded tog~th~r~ ; .:
with t~o xoyd~me SPl tin ex~mpl~a 1 to ~) and as A
compon-ne o~ th~ K~ydlm~ D10 or D125 ~n cxa~plo~ 5 to 35 1~), an AXD-X~ydime SP1 ~mul~ion ha~lng boen o~med by --` . 2~2~7~ : -.

g ~ .
meltln~ the ~XD at 6S to 80C, dl~olving the molten AKD in wster at 65 to 803C and ho~ogenlsing the mixture wlth Reydlme SP1 at 2500 to 3000 p91~

S Example~ 1 to 4, when compared with Ex~mples 5 to 10, ~how fluld plck-up~ (odgewlck) w~th anlonlc agents compar~bl- to or botter than thos~ o~ c~tlonlc agents 3xampl-~ 4 and 8 show Lh~L b~tter :~sult~ can be atta~n~d with reclrculation wh~ch mo~t reallstlcally 10 ~i~ul~tes the paperma~ng proce~s EXAMPL~S 11 to 15 and ~OM~ARI9ON EXAMP~ 16 Ed~wlok o~alu~tlon tests oon~l~tin~ of two parto ~ ormation oi' sh~-t~, and ~2) Co~tlng And lactlc aald t-zt~ ;' wore ~a~rlod out on ~ urth-r ~zlng composltlons ~he re~ults aro cloarly lndicative o~ the ~act that Anlonlc ~atlv~ ~lzing aompo~eLons porSorm w~ll in the to~t~ and ar~ ~ultablo ~o~ UJ- ln ~lz~ng p~pors ~or ~0 th- liquld paoka~lng lnduotry, Proc~d~r-Stook u-e~ w~ 50/S0 h~rdwood/~oStwood bo~t~n to a Schopp-r ~olqlar of 40.
~hemi~L ~ddlt~on~
2S ~hlckztock: 3.2~ A/R ~-t ~trongth ro~ln (Kymene 557) 0,35~ ~XD/Flbre ~lzlng oompo~ltion ThlnJtoc~ 0,05~ Dry Alum/Fibre 2 kg/t Accostr~ngth 85 1~ Dry St~lok 400 30 The proc~ur~ wa~ follow~d for oaoh o~ flv~ ~izing compo~ltlono ha~lng the follow$ng con~tltu~t~
Exampl~ 11 100g Ket-n~ Dimar ~palmitlc-~t-arlc) 1 25g Orotan ~ur~ctant) 4 5g W~nin t~urfaatant) ~5 aoog Wat~r I ~ ~
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2 ~ 7 ~ ~ :
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Ex~ple 12 1~0g ~eten~ Dl~or ~palmi~lo-st-~rlc) 1~25g Orotan :.
.Sg Wanin l.~g ~ercol lS5 ~50~ ~olid Aniontc Polyacryl~mld-) 800g Wator .
EX-~pl- 13 100g X~t~n~ Dlm-~ ~palmitlc-~t~ariC1 1.2S~ Orot~
4.5g Wanln ~6g BMA (cont~lns anionlc ~lllca) :.
~15~ ol~
133~ Water ~ ~ :
~x~pl~ 14 100g Xet~n~ Dl~or ~palmitic-~te~lc) 1.25g Orotan 7 lS ~.5~ W~nln 333g 1/2 BMA
166g W~ter , ~l :
Ex~mpl~ 15 100~ ~-tene ~im~r ~palmltic~4~aric) 1.25g orotAn :. .
4.5g Wanln ' ' ~ :
a.s~ ~ab 99~ ~x ~o~u~tt-) Anlonio Starcb ~ .
~25~ Wat~r A~ter aomblnAtion oi' th~ ~bov~ matorial~, i'urth~r w~t~r was add~d to ad~ust th~ eo~po~itlon~ to ~n AXD ~olld~
~5 oontont of 10~ by wolght.
....
Tho to~t~ aon~lotod of two part~: 1 , ~ .
Part 1t : ;
250 gsm sheets werla pro~uc~d on labo~atory sheet~
form~ng appa2~tu~ and the oon91~'cency of the tl~ln~tock w~ 0.5~.
The ~b~ots wor~ drl~d a~ 10~0C for 8 mlnut~ then oven ¢urQd fox 5 mlnut~s, 35 ~
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Pa~ 2 L~ctlc acla lmmer~lon teBt~ ~re c~rrled out on the ~
~hoet~. ~h- ~h-ets we~ oo~t~d wl~h t~po and cut to jj 12.5cm x 5cm otrlp~. Tho~o ~t~lp~ w~re w~ighed bo~or~
S lmm~r41On ln 2.Som o~ 1~ lactlo aald ~or 15 hours. Th~
strip- wero th-n r-w ~ghed ~nd t~o plckup c~lc~lated ln ~4 grAm~. ~h~ av~rage o~ 3 r~ult~ WA~ takon for eaah ~l~lng ~ompo~ltlon, ,¦
~ho edgowlo~ to~ts ga~o th- followlng results~ Jl;, ~xa~le Ed~ewiok (~) ~ Picku ,~
11 0.2~7 6.B
12 0.174 7.2 i~
1~ 0.316 12,7 14 0,317 t2,~ "' 0.185 7.6 ~
16 0.181 7,9 Examplo 16 i4 a oomparlson ex~mplo u~lng ~oydim- D10. ~
~he9e ro~ult~ o~-rall lndlcato th~t anlonlo AXD ~izing '!~
co~o~ltlon~ p-rform a- woll i~ not ~llgh~ly bettor ao th~n compo~ltlon~ ln sltuationa wh-re hl~b lo~elJ of c~tlonlclty ar- pro~ent. ~h~ co~po~ltlon~ aro '~
th~rofore ~ultable for u-- ln th~ liquid p~ck~glng t indu~try. . i~
: .
25 EXANP~ES 17 to 19 A ~rl~- of anlonlo ~lzo compo~ltlon~ wore propA~ed and :.
to~t~d: t Com~o~ltion 1 2 3 A~t tl~/Dl~-r~n~
Naphth~l~n~ Su~phorlla Aald 1,25 1.2S 1.25 -:
Na ~i~no~ulphos~at~ ~.5 4,5 4,5 l~
As~onla ~oly~oryl~.mld~ - l.a Collol~l Silica - - 37.S
A~yl Xoton~ Pim~r 100 100 100 `Jt ,"~
35 li~lmlelc/Sto~ric 7 ~ ~
!

12 il All amounto ars ~xpressed a~ dry grams of ~aterial. 3 '11 ':
~mulsion Manu~actu~e Proceduro ~n ~ach c~- th~ proc~- water wa~ acld~lod prlor to S th~ addltion o~ dl~po~ants. Tho ~xturo wa~ ~ated to 70C bo~oro add~ion ~o a laboratory homogenlzer wblch wa~ ~roh-at-d to the 9~e tempe~atur~. Homogonizatlon pr-~-ur~ wa~ ad~u3te~ to 350Q polg t24 M Pa) ~ideally 2500 to 5000 p~lg (17 to 34 M Pa)). Molten alkyl 10 k~ton- dl~-r wax was added at ~0C and allowed three theor~tlcal pas~o~ plu~ one to dlocharq-. Upon dl~c~arg~, th~ product wa~ pa~d through a 200 me~h '~
~tlt~r and the t~mperatur- rapldly reduced to below 2~C. . . .

5 r~boratorY P~ocduro~ "
a~ ~tock Prop~,~atlon ~ -All wo~k WA8 ~o~or~d on a SO:S0 mlxture of q -hardwood and ~o~twood bo~ten ~ n a Valley Beater to .;
~OOSR ~300 CSF) .
20 b) Ch-mlc~l Addltlvo~
Cb~mlcal addltlon~ wor- mad- u-ing ~yring ~ havln~ j~
An acouraay o~ ~ 0 1 cm3, All chomlcal addltlv~
oxcop~ praoipltatod calclum carbonato w-ro dlluted , pr~or to u~ for aoouraoy o~ ~ddlt~on. ~' ~5 Tl~c proolp~t~tod o~lclum carbonate used ~or thls woxk w~ ~ oommoro~lly ~v~ grado Alb~car HO t ~:
mado at 20~ sollds wlth no dlsper~ant ~dded.
Partlclo ~lze avQrag~d 2.7 mlcron- wlth a Zota pot-ntlal o~ ~5 mv 30 c) Sl~ -t~
~h~ ~z~ t~t ~mploy~d ~n thls work was a 2-mlnut~
Cob~ t--t und-r ~t~nd~r~

35 ---~~'~~~ ,. , ~

.. .

.4;g~ I

R ~ult~
Ch-mio~l Ad~itlon- - lb~/~on dry b~ls on ~lbre ~ x~ Z~n. ~b Si2ing g/m2 ck~x~ tlon 0~ 0~ Nhtur~l Eu~le S~xh Flll-r S~ze/~p A1~ r Cw~d CNred 17 lO.O 300 3.0~1 ) a.s 4040 q1 18 lO.O 3~0 3,~(2) 0~5 3C36 37 l9 10.0 300 3.0(3) 0.; 4441 38 1 0 , ,;, ' St~roh-~t~lok 400 CatLon~c Pota~o St~roh oomm~rcially.
available ~rom ~taley StArch Products ~td. ~ :
r ~ olpltated calclum oarbonat~ - 8e~ abov~
81S- - Compo~ltlon 1, 2 or 3 ~ above.
1~ Retentlon Ald--Hydraid ~RP-95~. Cattonic polyacryla~lde aommorcl~lly a~allabl- ~om Calgon ~td.
. ~ .:., ... ~:
M~cblne T~l~l Data Anlonlc ~lz- compo~l~lon (l) o~ Exampl- 11, wa- te~ted : .. ~.
20 ~g-ln-t a co~pctltl~, oa~lonlcally ~tab~l~zed ~Z. : ~.
A~uapal C348 ~uppll-~ com~orc~ally by ~orcul~ Powd~r Co. 8lsing w~ ~-a~urod to A ~ndard 1-~ln. Cobb :
t-~t. .
.: ,: .
2S Maahln~ Furnl~h on 60q/m~ Wovo ~udc Fl~rouo - Cb-mlthormal mochanloal pulp SO~ .
Whl~ Offcut~ 17 hlt~ Lot~r Wa~t~ 17~ l .
~hlt~ N~t~ Ro~oot~ 8 o~n Brok- 8 Ch~lo~l~
R~ontlon Ald - Cationlc Polya~ryla~ Nal~loc 4662 oom~ol-lly avallablo ~rom Naloo ~td.
Flll-r~ - Calclum carbonat~ add~tlon to A ~pocl~i~d 35 Jhoot a~b o~ 23~ w,o,f, r ~=

~ } ~ S~

~2~

~3 1 4 : ~3 Size A~itio~ Retention Sizing/srln C~
~ as Aci~ on Oven Cur~d Slze ~ype Rece~ed gJtcnne ' ~; Sheet Ash 3 min at 105C
A~el 3.7 ~57 2~.4 17.7 5 C34B ~.
~cn~ 1,6 257 22.g 16.9 9~
~.'' The8e r-~ult~ aro avet~a~ed ovor a poxio~. o~ 5 hours d o~ oontlnuou~ machino oporation. ~ .
.~
~'' , j ,~
~!

:1; ' . :

Claims

1. An active sizing composition comprising an aqueous emulsion of a reactive sizing agent and an anionic dispersant and/or emulsifier serving to stabilize the emulsion, the reactive sizing agent comprising at least one compound according to the formula wherein R1 and R2, which may be the same or different, are hydrocarbon radicals each having at least six carbon atoms.

2. A sizing composition according to claim 1, in which R1 and R2 are, independently of each other, alkyl, alkenyl, cycloalkyl, aryl, aralkyl or alkaryl radicals.

3. A sizing composition according to claim 2, in which R1 and R2 are, independently of each other, C12 to C22 alkyl groups.

4. A sizing composition according to any preceding claim, in which te anionic dispersant or emulsifier comprises one or more of sodium lignosulphonate, calcium lignosulphonate and the sodium salt of the naphthalene sulphonic acid.

5. A sizing composition according to any preceding claim, in which the dispersant or emulsifier is present in an amount of 0.5% to 10% based on the weight of the reactive sizing agent.

6. A sizing composition according to any preceding claim, including at least one substance wich extends or modifies the anionic charge density of the composition.

7. A sizing composition according to claim 6, in which the extender or modifier comprises one or more anionic polyacrylamides, anionic starch or colloidal silica.

8. A sizing composition according to any preceding claim, containing reactive sizing agent in an amount of 5% to 20% by weight of the composition.

9. A sizing composition according to claim 8, in which the amount is 10% to 15% by weight of the composition.

10. A method of sizing paper, using a composition according to any preceding claim.

11. A method according to claim 10, in which the sizing is carried out in the presence of a cationically charged substance.

12. A method according to claim 11, in which the cationically charged substance is a filler or a retention aid.

13. A method according to claim 10, in which the sizing is carried out in the presence of a fluorescent whitening agent.

14. A method according to any of claims 10 to 13, which is carried out at the wet end of a paper making process.

15. Sized paper made by a method according to any of claims 10 to 14.