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REACTION

FORMULATION

CHEMICAL QUANTITYmethyl methacrylate

butyl acrylate

Sodium lauryl sulfate 3 of char!e "

#otassium $ersulfate % of char!e "

N&'%(( 3 of char!e "

CALCULATION

Material Balance Calculations,

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EMULSION COPOLYMERIZATION OF

METHYL METHACRYLATE AND BUTYL

ACRYLATE

AIM

Emulsio) co$olymeri*atio) of methyl methacrylate +MMA, a)d butyl acrylate +-A,.

APPARATUS

Three')ec/ed flas/0 silico) stirrer0 reflu1 colum)0 thermometer ca$0 thermometer0 heati)!

ma)tle0 2ea)'Star/ a$$aratus0 clam$s0 electric motor0 rubber ire0 bea/er0 co)ical flas/. !lass

rod0 burette0 etc.

CHEMICALS

Methyl methacrylate +MMA,0 butyl acrylate +-A,0 N&'%((0 sodium lauryl sulfate0 $otassium

$ersulfate etc.

THEORY

Emulsio) $olymeri*atio) is a 4ersatile tech)i5ue0 idely used i) i)dustry to $roduce late1es for a lar!e

4ariety of a$$licatio)s i)cludi)! $ai)ts0 coati)!s0 adhesi4es0 a)d bi)ders i) the te1tiles a)d $a$er

i)dustries% Acrylics are a family of emulsio) $olymers e1te)si4ely used i) i)dustry0 ith )'butyl

acrylate6methyl methacrylate +)'-A6MMA, bei)! o)e of the most commo)ly used mo)omer systems.

This como)omer system is e1tremely 4ersatile0 a)d de$e)di)! o) the ei!ht ratio betee) the

como)omers0 late1es used for 4ery differe)t a$$licatio)s ca) be $roduced. Ty$ically0 co$olymers ith a

7(67( t6t )'-A6MMA com$ositio) are used for coati)!s0 a)d those ith at least of 8( t of )'-A areused as adhesi4es. The e)d'use $ro$erties of these late1es de$e)d o) the microstructural $ro$erties of the

$olymer9 therefore0 to meet the i)creasi)! dema)ds o) $roduct 5uality0 the structural $ro$erties of the

$olymer should be co)'trolled. To achie4e this co)trol0 it is im$orta)t to u)dersta)d the fu)dame)tal

$hysicochemical $he)ome)a i)4ol4ed i) the emulsio) co$olymeri*atio) of )'-A a)d MMA. A)

im$orta)t as$ect of this mo)omer system is that a !el ca) be formed0 a)d the !el fractio) stro)!ly affects

the fi)al $ro$erties of the $roduct. To de4elo$ $ro$er co)trol strate!ies0 a mathematical model able to

describe the co$olymeri*atio) /i)etics a)d the e4olutio) of the aforeme)tio)ed $olymer $ro$erties should

be used. N'-A6MMA semi batch emulsio) $olymeri*atio)s at a fi1ed 7(67( molar com$ositio). No

substa)tial effect of the CTA o) the /i)etics as obser4ed0 but the M:2 decreased ith the CTA

co)ce)tratio)0 a)d a co)ce)tratio) of % t CTA as e)ou!h to a4oid !el formatio) duri)! the $rocess.

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PROCEDURE

%. Set the reactio) assembly a)d char!e o)e'third !ram moles of a)d %.; moles of ##< i)

the reactor alo)! ith #TSA a)d hydro5ui)o)e.

;. Start heati)! a)d stirri)! a)d co)ti)ue for o)e hour u)der co)ditio)s of total reflu1.

For Polymer content,

#olymer co)te)t " :t. of sam$le before heati)! = :t. of sam$le after heati)! 1 %((

:t. of sam$le before heati)!

For NVM,

N>M " :t. of sam$le before heati)! = :t. of sam$le after heati)! 1 %(( :t. of sam$le before heati)!

3. After ?7 mi)utes add to'third !ram moles of Maleic a)hydride a)d co)ti)ue heati)!

u)der total reflu1 for o)e hour more.

?. Attach a*eotro$ic le!0 i.e.0 the 2ea)'Star/ a$$aratus a)d fill it to o4erflo $oi)t ith

&yle)e a)d add %7 mL of &yle)e i) the reactio) mi1ture.

7. Heat the reactio) mi1ture sloly u$to %7((C to ;(((C0 a)d after e4ery %7 mi) ta/e out

about % ! of sam$le to fi)d out acid 4alue.

@. :he) the acid 4alue dro$ to betee) ;7 to 7(0 sto$ the reactio). 2rai) out the a*eotro$ic

mi1ture from the 2ea)'Star/ a$$aratus.

. Sitch off the heati)! ma)tle as ell as electric motor. Collect the fi)al U#B resi)+$roduct,.

. :ei!h the resi) to fi)d the yield.

DETERMINATION OF POLYMER CONTENT

%. Ta/e 7 ! of emulsio) formed i) a bea/er a)d add 7( mL +e1cess, of metha)ol.

;. :ei!h the bea/er i) hich the sam$le is ta/e).

3. The co$olymer ill !el a)d the emulsio) ill brea/. Be$eat this ashi)! se4eral times.

?. Add ;'3 dro$s of (.;N HCl so to com$letely brea/ the emulsio).

7. No deca)t the sol4e)t layer /ee$i)! the co$olymer safe.@. Dee$ this for heati)! for ;( to 3( mi)utes i) a) o4e) at 7(C.

. Calculate the $olymer co)te)t.

DETERMINATION OF NON-VOLATILE MATTER (NVM)

%. Ta/e a clea) a)d dry $etri dish a)d ei!h it.

;. Ta/e about % ! of resi) o) the $etri dish.

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3. Dee$ it i) the o4e) at about %(('%%(oC for o)e hour to remo4e the 4olatile com$o)e)ts.

?. :ei!h the $etri dish ith the sam$le.

7. Calculate the N>M of the resi).

PRECAUTIONS

Dee$ a )ote o) the tem$erature e4ery time. 2o )ot let it cross @(C.

.Dee$ a co)trol o) the froth formed by ashi)! the bea/er ith cold ater.

:hile $ouri)! hot resi) i) the bea/er0 ma/e sure that the bea/er is dry.

Use o)ly silico) oil i) the thermometer ca$. Ma/e sure that the bulb of the thermometer

is fully immersed i) the oil.

A4oid direct i)halatio) of the fumes.

Clea) the $i$ette ith hot ater immediately after use to a4oid bloc/a!e by solidified

resi).

OBSERVATIONS

The $olymer co)te)t of the co$olymer formed is

The 4olatile matter $rese)t is

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RESULTS

Weight ! "e#i$ %t&i$e'

P*+e" ,$te$t

V&tie ,$te$t

HANDLIN HAZARDS

Inhalation - Can cause central nervous system (CNS) depression. Irritating to

respiratory system.

Ingestion - Can cause central nervous system (CNS) depression.

Sin - Irritating to sin. !ay cause sensiti"ation #y sin contact.

$yes - Irritating to eyes. Chronic e%ects - Contains material that can cause target organ damage.

Carcinogenicity - Contains material &hich may cause cancer' #ased on animal

data. is o cancer depends on duration and level o e*posure.

+arget organs - Contains material &hich causes damage to the ollo&ing

organs, idneys' liver' upper respiratory tract' eyes' central nervous system

(CNS)' ears.

PROPERTIES

APPLICATIONS