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Journal of Petroleum Science and Engineering 58 (2007) 111 –118www.elsevier.comlocate!etrol

"nfluence of !ol#mer $ases on t%e s#nergistic effects o$tainedfrom mi&tures of additives in t%e !etroleum industr#'

Performance and residue formation

uciana S. S!inelli a *line S. *+uino a ,enata -. Pires a Elaine . /ar$oa a*na aria . ouvisse $ Elia$ete . ucas a

a "nstitute of acromoleculesederal 3niversit# of ,io de Janeiro "*3,J 4idade 3niversitria4entro de ecnologia /loco J "l%a do und6o 215970 ,io de Janeiro /rail

$ Petro$ras ,esearc% 4enter4E:PES — ;. 7 — 4idade 3niversitria "l%a do und6o 21900 ,io de Janeiro /rail

,eceived 2 June 200cto$er 200

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com!onent also ?nown as $ase. :ormall# eac% $ase %as a

!articular effect on eac% ?ind of oil to $e treated and solvents

are added to t%e formulation suc% as aromatic com!ounds and

alco%ols wor?ing as co9

additives andor to render t%e

formulation less viscous and

!um!a$le so as to allow

inFection in line ( race

12).

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112 .S. S!inelli et al. Journal of Petroleum Science and Engineering 58 (2007) 111 –118

Since usuall# !etroleum is !roducedtoget%er wit% water and gas so9calleddemulsifiers are added to desta$ilie t%ewater9in9oil (K>) emulsions. Suc%emulsions can form de!ending on t%e

!etroleum com!osition and on t%etur$ulent flow regimen associated wit%t%e !roduction tec%ni+ue. Suc% !roductsaim at !romoting t%e se!aration andremoval of water from t%e oil and at t%esame time !reventing t%e se!aratedwater from containing a %ig% residual oilcontent w%ic% could cause t%e formation

of oil9in9water (>K) emulsion ( Pauliset al. 1D).

Buring oil !roduction it is usual to co9

!roduce a !ortion of t%e water em!lo#edfor inFection. *s a conse+uence %ugevolumes of water are generated w%ic% inoffs%ore o!erations %ave to $e discarded int%e sea. Suc% water called !roduced wateris an oil9in9water (>K) emulsionnormall# treated using floccu9lating agentst%at can $e adsor$ed on t%e interface of t%eoil dro!s so as to !romote t%eneutraliation of c%arges andor t%e

formation of inter9!article $ridges ( eder

et al. 200= ernandes et al. 2005).%e !resence of water in !etroleum

!roduction leads to corrosion and formation

of salt de!osits (scales). K%en t%is occurscorrosion and scale in%i$itors are used in

order to !revent corrosion of !i!es as well as

scale formation eit%er t%roug% de!osits on

surfaces or t%roug% formation of scaling

cr#stals suc% as calcium car$onates and

$arium strontium and calcium sulfates (

Iasson et al. 17= Brela et al. 18= Ie et

al. 1= B#er and ra%am 2002).S#nergistic effects can occur w%en

c%emical additives are used in admi&turesin t%e !etroleum industr#. Suc% effects canen%ance or diminis% t%e !erformance of eac% additive andor can cause undesira$leresidue. %e ?nowledge of t%ese ?inds of effects !ermits (1) o!timiing t%e amountof eac% additive added (2) !reventingdam9ages and (D) reducing residuedis!osal.

%e identification of t%e constituentsof t%e formula9tions res!onsi$le for t%es#nergistic effects leads to reformulation

of suc% additivesaiming at minimiingan# undesira$le effect.

%e aim of t%iswor? is to evaluate t%einfluence of t%e

!ol#meric9$ases ont%e s#nergistic effectst%at occur w%en someadditives(demulsifiersflocculating agentsand scale in%i$itors)are used in admi&turesin t%e !etroleumindustr#.

2. Experimental

section

2.1. aterials

4ommercialdemulsifierflocculating agent andscale in%i$itor additives su!!lied $#PE,>/,*S as well

as t%eir res!ective !ol#mer $ases $loc? co!ol#mer of

!ol#(et%#lene o&ide9 $9!ro!#lene o&ide)—4>P1 (Bow ;uLmica

/rail) cationic !ol#acr#lamide –P*4 (4ME4) and

!ol#(sodiumacr#late) –P*S(>&iteno /rail) wereused. *not%er $loc? co!ol#mer of !ol#(et%#lene o&ide9$9

!ro!#lene o&ide) —4>P2 (Bow ;uLmica/rail) was used in

order to com!are itsefficienc# to t%e4>P1= t%ese two

!ol#o&ides differ interms of arrangementof t%eir $loc?s.Petroleum of medium*P" grade and oil#water from t%e4am!os /asin werealso used in t%e stud#.

2.2. et%ods

Ke c%aracteried t%ecommercial additives $#ourier ransform"nfrared s!ectrometr#(",) and t%e !ol#mer9ic $ases $# siee&clusionc%romatogra!%# (SE4)%#drogen nuclear

magnetic resonance (1I9,:) $esides ",.or eac% additive we rans!ecific !erformancetests t%at isdemulsificationflocculation and scalein%i$ition tests. Keconducted t%ese testswit% t%e commercialadditives individuall#and in $inar# and ternar#mi&tures and also wit%t%e !ol#meric $ases

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individuall# and in $inar# and ternar#mi&tures. /esides t%is we !erformed residueformation tests for t%ese same s#stems.

2.2.1. 4%aracteriation

2.2.1.1. ourier transform infrared

s!ectrosco!# (",). Ke !erformed", on a Per?in Elmer1720& s!ectrometer ta?ing

measurements from 000 to 00 cm− 1

wit% 2 cm− 1 resolution. Eac% measure9ment was an average of 20 scans. or commercial additives (demulsifierflocculant and scale in%i$itor) and

!ol#meric $ases (4>P1 4>P2 andP*S) w%ic% are li+uid sam!les we

!erformed +ualitative anal#ses on *g/r cell. or !ol#meric $ase P*4 w%ic%

is a solid sam!le wemi&ed it wit% A/r

!owder.

2.2.1.2. Siee&clusionc%romatogra!%#

(SE4). Ke used SE4to determine t%eaverage molar mass of t%e !ol#meric $ases4>P1 and 4>P2. %ee&!erimentswere !erformed onst#rene9divin#l$eneneco!ol#mer columns

(10 –10D –500 –100N) using

tetra%#drofuran as a

solvent and !ol#st#rene asstandards in a Katers

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.S. S!inelli et al. Journal of Petroleum Science and Engineering 58 (2007) 111 –118 11D

-arian 3:"M D00 instrument wor?ingat D00 I at D0 O 0.1 4 usingdeuterated c%loroform as a solvent. Ke

!erformed +uantitative anal#ses for

co!ol#mers 4>P1 and 4>P2 todetermine t%e et%#lene o&ide !ro!#leneo&ide ratio.

2.2.2. Performance tests

2.2.2.1. Bemulsification test. Ke evaluatedt%e !er9formances of t%e commercialdemulsifier and of t%e demulsif#ing

!ol#mer $ases in t%e la$orator# $# !re!aring a s#nt%etic water9in9oil (K>)

emulsion using !etroleum and $rine at aconcentration of 55 000 mg sodiumc%loride and calcium c%loride

(:a4l'4a4l2Q2I2> — 10'1). %isemulsion was !re!ared at 5050R vvoilwater wit% t%e aid of an 3ltra urra&

$lender at a rotation of

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nm. *lt%oug% t%e ma&imum a$sor!tionsare at a$out 250 nm we c%ose 00 nm inorder to minimie t%e interference of t%e

solvent as s%own in ig. 1. Kecalculated t%e flocculation efficienc#

!ercentage of t%e sam!les anal#ed int%e Far test $# t%e difference of t%e >

value of $lan? oil# water and > valueof oil# water containing additivesdivided $# t%e > value of $lan? oil#water.

2.2.2.D. Scale in%i$ition test. Ke em!lo#edt%is test to evaluate t%e a$ilit# of t%e scalein%i$itor to !revent t%e !reci!itation of solids ad%ering to t%e surface mainl#

resulting from $rinewit% large amounts of calcium salts.

%is test consists of t%e !re!aration of twos#nt%etic $rines one of t%em containing

calcium ions and t%eot%er containing $icar$onate ions. %econcentrations of ig. 1. ra!%ic of

a$sor!tions of oil inc%loroform at aconcentration (mg) of' (a)0.0= ($) 10.0= (c) 20.0= (d)D0.0= (e) 75.0= (f ) 125.0=

(g) 150.0= (%) 4I4lD.

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cations and anions !resent in t%ese $rines

are !resented in a$le 1. /ot% $rines were

saturated $# $u$$ling wit% 4>2 at ana!!ro&imate flow rate of D00 mmin.

%ese $rines were t%en admi&ed at5050Rvv in an a!!ro!riate flas? w%ic%contained a sufficient volume of concentrated solution so t%at t%e finalconcentration of t%e !roducts %aving ascale in%i$ition c%aracter was 10 and 50mg. Ke !laced t%ese flas?s in atem!erature9controlled $at% at 70 4 for 2% and t%en carried out com!le&ometrictitrations using a 0.01 EB* solution asa titrating solution and erioc%rome $lac? as indicator. %e value of t%e !roducts

in%i$ition !ercentage was assessed $asedon t%e o$tained data using E+. (1)

R "n%i$ition ¼½ð-a−-cÞ=ð-$−-cÞ 100 ð1Þ

"n order to evaluate t%e influence of t%e ot%er additives on t%e !erformance of t%e scale in%i$itor we added a flocculantandor demulsifier solution toget%er wit%t%e scale in%i$itor sufficient to reac% 10

mg. Ke ran t%ese tests for commercialadditives as well as for t%e !ol#mer $ases.

2.2.2.. ,esidue formation test. Sincesolu$ilit# is a relevant !ro!ert# for evaluating t%e com!ati$ilit# among

!ol#mer additives we evaluated t%eformation of a de!osit resulting from t%eadmi&ture of commercial additives andt%e admi&ture of !ol#mer $ases in $rineand in oil# water.

Ke !laced flocculant solutions at 100 200and 500 mg in t%e oven at a tem!erature of

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related to t%e eac% !ol#meric $ase wereo$served.

%e main a$sor!tions o$served for t%edemulsifier formulation are relative to' (i)

–>I a&ial stretc%ing (at D cm− 1)= (ii) –4 –> –4 – s#mmetric and as#mmetric a&ialstretc%ing (at 1111 and 1015 cm− 1)= (iii)— 4I2 and –4I a&ial stretc%ing (at 287D

cm− 1)= and (iv) –4I2 angular stretc%ing(at 8P1 and4>P2.

Ke o$served t%e following maina$sor!tion $ands at t%e s!ectrum of t%ecommercial flocculant' 4 # > a&ialstretc%ing related to amide grou!overla!!ed wit% – :I2 stretc%ing (at

1

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.S. S!inelli et al. Journal of Petroleum Science and Engineering 58 (2007) 111 –118 115

a$le 2ain c%aracteristics of !ol#meric $ases

Pol#meric Pro!erties $ases

n w nw

4>P1 P2 7800 8000 1.02P*4 Iig%

aIig%

a –

P*S Iig%a

Iig%a

–

a olecular weig%t in a range of 1.10

< and 1.10

7

gmol.

D.2. Bemulsification

%e $est !erformance among t%et%ree demulsifier concentrations wass%own $# 100 mg. Positive s#nergisticeffects were o$served $# adding t%escale in%i$itor and t%e mi&ture of t%isconcentration wit% t%e flocculant to t%edemulsifier in $inar# and ternar#

mi&tures as s%own in ig. D.Ke first o$served w%ic% one of t%ese

$ases !erforms $etter as a demulsifier .ig. s%ows t%at 4>P1 !romotes water –oil se!aration w%ile 4>P2 does not s%owt%e same efficienc# as a demulsifier. 4>P1is t%e $ase of commercial demulsifier and

4>P2 is anot%er $loc? co!ol#mer of PE>9PP>. %us t%is difference in !erformanceis due to t%e fact t%at 4>P1 and 4>P2

%ave different structures ( ig. 2) in s!iteof t%e fact t%at $ot% are PE>9PP> $loc? co!ol#mers %aving similar molecular weig%t and t%e E>9P> ratio of 4>P2leads to an I/ value t%at favors t%edesta$iliation of K> emulsions $etter t%an 4>P1 I/. %e 4>P1 structureinvolves %#dro!%ilic adFacent grou!s (>I

grou! $eside t%e et%#lene o&ide segment)w%ile 4>P2 %as an alternate structure (ansur et al. 18 200). %e adFacentstructure !romotes t%e desta$iliation of K> emulsions so as to facilitate t%e

!ositioning at t%e interface of t%e oil andwater dro!s dis!lacing t%eir naturalsta$ilier agents and !romoting !%asese!aration.

%us we carried out t%e stud# of t%es#nergistic effects among t%e mi&tures of

!ol#meric $ases using 4>P1. ig. s%ows a !ositive significant s#nergistic

effect for all t%e $inar# and ternar#mi&tures $ased on t%e

!erformance of 4>P1alone. %is means t%at

t%e

ig. D. Besta$iliation ofK> emulsions $#commercial additives.

!ositive s#nergisticeffects o$served for t%e commercialadditives stem at leastin !art from t%e

$e%avior of t%eir !ol#meric $ases.

D.D. locculation

%e o!timum

concentration for t%ecommercial flocculantwas 50 mg t%eefficienc# of w%ic%was 7R. %eaddition of commercialdemulsifier did notcause an# s#nergisticeffect w%ile t%eaddition of com9mercial scale in%i$itor

!romoted a negatives#nergistic effect.a$le D s%ows t%e

!erformance data for t%e flocculation of commercial additives

!ol#meric $ases andt%eir mi&tures.

>n c%ec?ing t%eeffect of t%e Foint useof t%e !ol#9meric

$ases on t%e P*4efficienc# a negatives#nergistic effect can

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$e o$served for $ot% t%e $inar# andternar# mi&tures containing t%e

!ol#meric demulsi9fier $ase. %eaddition of 4>P1 w%ic% desta$iliesK> emulsion and tends to sta$ilie>K emulsion causes com!etition wit%t%e flocculant action of t%e P*4 so t%e

total effect $ecomes nil.

>n t%e ot%er %andt%e P*S !ol#meric $asestrongl# aids in t%eflocculation of s#nt%etic oil# water w%en added to P*4t%at is t%e Foint use of

P*4 and P*S #ieldsa !ositive s#nergisticeffect. %e interaction

$etween P*4 w%ic%is cationic and P*Sw%ic% is

ig. 2. 4o!ol#mers structures.

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11< .S. S!inelli et al. Journal of Petroleum Science and Engineering 58 (2007) 111 –118

a$le Scale in%i$ition efficienc# for t%e commercial additives !ol#meric

$ases and t%eir mi&tures

4ommercial additives Pol#meric /ases

S#stems Efficienc# (R) S#stems Efficienc# (R)

10 mg 50 mg 10 mg 50 mg(

Scale in%i$itor 58 DD P*S 7D Scale in%i$itor 52 D1 P*S 7D D8locculant P*4Scale in%i$itor 52 D5 P*S D D8Bemulsifier 4>P1Scale in%i$itor D5 D1 P*S 11 D8

ig. . Besta$iliation of K> emulsions $# !ol#meric $ases. ($) locculant P*44>P1 (100 mg)= ( ) 4>P1 (100 mg) C P*4 (10 mg)= (●) Bemulsifier 4>P14>P1 (100 mg) C P*S

% (10 mg)= (▴) 4>P1 (100 mg) C P*4

⋄ Error' O 1.5R. (10 mg) C P*S(10 g)= ( ) 4>P2 (100 mg).

anionic reduces t%e interfacial tension of t%es#stem im!roving t%e flocculation !rocess.

%ese results suggest t%at t%e s#nergistic effects

o$served for t%e commercial additives are not

caused $# t%e ?ind of !ol#meric $ase used in t%e

res!ective for9mulations. >t%er constituents of t%e

additives are !ro$a$l# res!onsi$le for t%e variation

in t%e flocculation efficienc#.

D.. Scale in%i$ition

4alcium car$onate !reci!itation tests led tot%e assessment of t%e scale9in%i$itingefficienc# as well as to ?nowledge of some

!ositive or negative interference of t%e ot%er additives on !erformance. or t%e sa?e of

com!arison a$le s%ows t%e values for scale in%i$ition efficienc# for t%e commercialadditives as well as for t%e !ol#meric $ases.

*t a 10 mg P*S concentration t%e additionof P*4 (flocculating $ase) did not cause an#

c%ange in P*S efficienc#. Since t%e scale9in%i$ition !rocess seems to $e related to t%egrowt% of cr#stals $# lin?ing P*S molecules andcalcium ions t%e P*S molecules are not

a$le Dlocculation efficienc# for commercial additives

!ol#meric $ases and t%eir mi&tures

4ommercial additives Pol#meric /ases

S#stems Efficienc# (R) S#stems Efficienc# (R)

locculant 7 P*4 12locculant 77 P*4 0

Bemulsifier 4>P1locculant

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t%e t%ree !ol#meric $ases t%e negatives#nergistic effects were !otentialied as %ad

$een o$served for commercial additives.

%e P*S concentration of 50 mgm isa$ove t%e o!timum concentration since t%att%e efficienc# %as decreased. %is means t%atit is not useful to %ave too man# in%i$itor

molecules in t%e s#stem. /esides t%is t%eeffect caused $# t%e addition of t%e ot%er $ases is

ig. 5. ,esidue formation in $rine for commercialadditives and t%eir mi&tures.

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.S. S!inelli et al. Journal of Petroleum Science and Engineering 58 (2007) 111 –118 117

milder. 4oncerning t%e effect of t%e ot%er additives t%e lower t%e efficienc# of t%escale in%i$itor t%e lower t%e negativeeffect caused $# t%ese ot%er additives. *

!ossi$le suggestion is t%at if t%ere is an#interaction among t%e various additivest%ese occur onl# for a reduced num$er of scale in%i$itor molecules due to t%erelativel# low concentration of t%e ot%er additives so t%at t%e s#stem still containsfree scale in%i$itor mole9cules a$ove t%eo!timum concentration.

D.5. ,esidue formation

%is test aims at evaluating t%esolu$ilit# of additives usuall# using !roduced oil# water.

Iowever in order to %ig%lig%t t%eeffect of t%e normall# !resent salts inoil# waters on t%e solu$ilit# of t%ecommercial additives at first we used

$rine alone. %e resulting data are

summaried in ig. 5.K%en inde!endentl# tested t%e t%ree

additives formed residues wit% t%e larger amount $eing originated $# t%edemulsifier. %e amount of residue formed

$# t%e flocculant increased wit% t%e rise inits concentration in salt solution. /roadl#s!ea?ing t%e Foint use of t%ese additivescauses a residue amount t%at corres!ondsto t%e sum of t%e residue formed $# eac%additive individuall#. Iowever t%eaddition of a scale in%i$itor to t%eflocculant causes a !ositive s#nergisticeffect !romoting t%e reduction in t%eamount of de!osit generated $# t%e

flocculant alone. Suc% !ositive s#nergismstill occurs as a result of t%e mi&ture of t%et%ree additives.

Ke t%en !erformed t%e same test aswit% $rine wit% !roduced oil# water instead and o$served t%at t%e residuecontents were clearl# %ig%er t%an t%oseo$tained for $rine w%ose salinit# wassimilar to t%at of t%e oil# water. %is

$e%avior is related to t%e lower solu$ilit#of t%e additives caused $# t%e !resence of

oil in t%e !roduced water.

ig.

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negative s#nergistic effects s%own $#commercial additives.

%e !ol#meric $ase is res!onsi$le for t%e !ositive s#nergistic effect occurringin t%e !resence of t%e flocculant andor t%e scale in%i$itor on t%e demulsifier

!erformance as well as $# t%e negative

s#nergistic effect occurring $# t%e !resence of demulsifier and t%e mi&tureof demulsifier and flocculant on t%e

!erfor9mance of scale in%i$itor.urt%ermore it is also res!on9si$le for t%e lower residue formation o$served int%e flocculating mi&ture and scalein%i$itor w%ic% is a !ositive s#nergisticeffect.

Ac(no)led*ments

%e aut%ors would li?e to t%an?

4E:PESPE,>9/,*S *PE,J4*PES 4:P+P"/"4and *:P":EP4PE,> for financial su!!ort=PE,>/,*S for t%e

commercial additives=Bow ;uLmica >&itenoand 4ME4 for t%e

!ol#mer sam!les= and,"/E and A>E**/"E:* for rec#cling t%e c%emicalwaste !roduced $# t%ee&!eriments.

Appendix A.+omenclature

-a -olume ofEB* utilied in t%esam!le

containingt%e !roductafter

!reci!itation

-$ Ialf of t%eEB*volume utilied int%e calcium9

containing $rine $efore !reci!itation(total

volume is related tot%e titrated volume $#

t%emi&turecalcium and

$icar$onate ina 1'1 ratio.

8/19/2019 10.1016j.petrol.2006.11.009

15/15


-c -olume of EB* utilied in t%e $lan? (wit%out !roduct) after !reci!itation.

"e,erences

Bavies .*. Mang . Stewart *.4. 1

10.1016j.petrol.2006.11.009

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