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3.1 Experimental
1\cryiJc <Krd (GC Purity ()9%,), procured from Thomas Baker. India . dccyl
ak;(llwl ((i( Purity 08io) ubtamed from S D Fuw \ 'hcrmcals i ttL lnclra ->tvrenc
,Jhtamcd from Merck PrPdu~.:h. ( iennany and hydwqumone procured from S D. Fine
Chemicals Ltd, lndw, were used. 8enzuyl pero\.Jtk ( ( ,( Punty lJS"'o) procured from
r nha Chem1cais Pvi Ltd lmha. and was purified by ;;rystallization from methanol
~. 1.2. Esterification of den! anylate (l)A.I from a(.rylic acid and dccyl alcohol
De.. \ l acrvlat(' vv:b prcpan.d by reacting acryl1c acid with decyl alcohol ( l.ll
molar ralln rhc rca,twr; '"ii' Jrncd 11Ut m <1 nsm kc11le ll1 the presence of cataJytrc
,J!ll\Hll1t ,r ''rh:cntratcd -..ulphunc ac1d. ii ~~,)~;, hydroqun10ne (with respect to the
mon(Hnen as pulymcruatwn :nh1bttor t(,r lcryllc actd. and toluene a-; a solvt:nt under
1 slow stream nf deoxygenated nitrogen. The reactants. which were mixed with
toluene. were heated gradually tiom room wmp~;ratun: tu 403K using a well-
' on trolled thermostat. The progress or the reactwn was followed by monitoring the
amount of liberated water frnm the reaction mixture to g1ve the ester. decyl acrylate
139
pressure and was used m the polymerization process.
The polymerization was carried out in a four necked round bottom t1ask
-~qmpped with a stirreL condenser. thennometeL an inlet for the introduction of
:utrngen and a dropping tunnel tP add styrene drop w1se ln the t1ask was placed
des1rcd mass ,)1 DA and mmator iB/Pl fo!lmvcd hy the des1red mass of styrene wa~
added dropw ISL' f\n ) h m the prcs-.nc~. 'll. toluene as solvent The reaction temperature
was mamtamed at ~5~ K for 6 h. i\1 thL end ut the reactwn tnnc. the reactiPn mtxture
va..: poured mto methanol w1th ~tlrnng to terminate the polymenzat10n and to
preclpttalL lill P''i~ Tl l" \'.:l lurlh,r punt!ed npcated prcclpllalmn ,,j
140
Scheme I
Esterification:
Cone. H 2 S0 4
H 2C=CHCOOH Toluene, HQ inhibitor
Dean Stark
Apparatus
Scheme-l!
Homopolymen~a twn:
I nluene. fVP
.....
---
XO"< 6hr
Scheme-Ill
Copolymeri ..;;ation:
. CH=:::CH.
141
0.0 l K. Experimental determination was l:arriecl out by counting time flow at least six
ditterent concentrations uf the sample solutions. The time flow of the solution was
manually detern1ined by using a cbmnometer. ln a single measurement the lowest
value of solution concentration was chosen for the calculation. The viScometeJ was
calibrated frequently with distilled water. The viscosity results were checked against
viscosity of known solutions and uncertainty was found to be nearly 0. J 7 %.
Precautions regarding prevention of evaporation of the solvent were taken m all the
r\ll the hmary -:nlut10ns were prepared hy d1ssolving a measured we1ght of the
polymer tn chloroform and toluene and dilutmg to a measured volume. All the ternary
snlutwns were rrepared hy dissnlving ;l Int;':lS\lrerl weight of the polymers with a DA
'; IHHX' ell g and <1 P Tl:" !'-~! 461 were emploved m toluene and the unc.tanh K
!'he prepared addit1ves were evaluated as pour pomt depressant using two
di tTercnt hase \)lis collected from the ...;a me source. (Table 5) through the poll! pomt
te-.:1 accordmg tn the A ST!\11 !) .. )7 method usmg WI L -4 71 cloud and pour puml test
142
3.1.8. Evaluation of prepared additive as viscosity index improvers (VIIs) in base
oils
Different binary and ternary blends were prepared by using two ditTerent types
of base oil. Viscosities and the viscosity index (VI) of these oils were calculated
according to i\STM [)2'70 Different weight percentages of concentration from 0.25
hl ~.0 were used 1P ;.,tudv the effect nf concentration on V! of the additive-doped lube
.1tl The cxpenment \v<l'- dune f(n h\Jth binary and temary blends. In th1s respect. the
kinematic \'1'-'l'O'>ll~ , ,i Jh,: nd contammg different concentratiOns ,,f the prepared
polymers. ,:opolymers and polymer hlends ware detem1ined at 313K and 373KThe
experimentai data \\Trt" m>ted hv takmg an average of three expenmental results under
Jdenllca! ''
J.2. Referenct'\
depressants t0r l.ube Oil. Pet .)'o /ceiL. 2006, 24, 887-894
[4] Jukic. /\. I ornasek, L. J.; Janovic, Z.; Polyolefin and poly(alkyl
methacrylate) mixed additives as mineral lubricating oil rheology
modifiers. I uh. Sci, 2005, 17, 431-449.
143
[6J Gallucci, R. R.; Mullen, T~ Odie R. Sheth, C. K.; White, M. J.; Methods
of making polymer blends cumpl'il1Jons, l i S Patenr No 8.2nR. 934 H2
2012.
2008.
compositions usetul as rheology modi tiers and methods t(H making such
compositions,. Patcnt242-193Y .11 . Mar. 7, 2012.
144
ll4] Gravlin, CJ .; Swire . E. A.; and Jones, S P.; Pour pomt depression ot
139-46
VlSCPsltv mdl':x tmpwvers l\)r iubt: t.llL f'ei (,'t 1 lixh .. 2005 . .1 -;
; ~ 7 ."i.:l.()
64,2716.
[23] Garcia, R., Melad, 0.: Gomez, C. M.: Figucruclo, J. E.; Campos, A.:
145
Viscometnc study on the compatibility of polymer-polymer mixtures in
solution, Fur Polym J, 1999, 35, 47-55
l24] Sun, Z., Wang, W.; Feng, Z., Criterion of polymer-polymer miscibility
i.25j Yang. H, ZhtL P P.: Wang, S. Q.. Zeng, '{ M, Guo. Q. P. Viscomeln
study (\f pnlym~.T-pl)lyrncr mteractlons m ternary systems !I The
mfluence of -;nlvenr Cur Polvm ./ 1998. 34. 9, 1303 U08
penn\ depressant for Oil !nt .! Pulvm /Hater. 2011. 59. 1008--101
[31] Varnell, D. F.; Runt, J. P.; Coleman, M. M.; FT i.r. and thermal analysis
studies ofblends ofpoly(c:-caprolactone) with homo- and copolymers of
poly(vinylidene chloride), Polymer, 1983, 24, 37-42.
146
and Technolog~ 2009, 27, 20-32.
if I I! I l( 1989
147
ot ethylene-cyclic olefin copolymers, J>olpn lest .. 2002, 21(4),
411-41 'i
148