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MODELANSWER

M. Sc. (I" Semester) Examinatio nr 2013

CHEMISTRY

Paper: FIFTH

CMT- 105: POLYMER CHEMISTRY

PAPER CODE: A5-2146

Submitted

BY

Dr. Arti Srivastava

Assistant Professor

and

Dr. Bhaskar Sharma

Assistant Professor

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Ftn^nw, w%n #q Ak;+ fP p*.<*<,tk (t.e-.,dfu4

- -@t4/, A>4t^^bd e*1pal-s%:ffi r: -n"

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= d K* WJ'I*

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t Yr-f El \ lu\-a- )\/

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=t t<rt S' L rlKr

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w

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4e Ur$'rA^< clruta

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ftrxvo\T,-T '

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u nPln-aL) A

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Kp trn:,e tK&r<* ffr:S f'L-

DT* y on-t2a!&t-,

[i) ft =2N ,atlu"n kj.,r"rrt^^k4^ aQ-{fi +!0o*g&nft-

ri,tr r^ df r.'.r ..'^'ld^* rV 'L^A ? W ^T(_',) PP = I - 'r ^_ka"^ Wd b*+Ln*

s.r lil'#*ffi % *r{p-rla-'A | -Y'

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P ol6"ard64y-.,,

ta) Ytru3 t \-{n trm Cr:rT:oJ>q- 1 k r"^berraJ^tts

t'

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=

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II

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i LIN) Potd^nruu /'zJ P

i

C O^nrr-tl-- 6 { *- tL kr<-.^A/.'; ,.o i |4"

\

Section 8:

Q3: What are polymers? Explain their classification based on structure, and the modes ofpolymerization.

ote- n -

Ans: Poly meaning 'many' iurd mer meaning 'part' (in Greek). Poiyrner is made up oimany sri.iall units as monorrers which have linkcd to each other to form a long or largemolecule. Polymers are conrplex and giant moiccules and they are different from lorvmolecular weight compounds. The process by lvhich the monomer molecules are linkedto form a polymer is called polymerization.On the basis of structure, polymers are classified into following categories.Linear chain polvmers: The monomers react to each other and form a straisht lons chain.Linear polymers are well packed and therefore the possess:

(a) High crystallinity,(b) Tensile strength,(c) High densities,(d) High melting point

Example: HDPE, Amylose

$vo* fu'1,"

D y'at'rt

/o furr*,* '

Cross-linked polymers: Polymers in which adjacent polymeric chains are linked to eachother directly or through side chains are called cross-linked polymers.The crosslinking of polymeric chains forms a network type structures. When heated in amould, cross-linked polymers become infusible and form an insoluble hard mass. As aresult once molded, these polymers can not be reshaped or remelted by heating.Example: Bakelite , urea formaldehyde resin, vulcanized rubber

j'i, lt:.

i,a

t ir.o*, a linF, b m/:(

Branched chain polymers: Polymers which have side chains attached to side chainsattached to the linear chain. The branched chain polymers are irregularly packed and theyhave:

(a) Lower tensile strength(b) Lower melting point(c) Lower density(d) Lower crystallinity

Example: LDPE, Amylopectin etc.

Lwss- )inVd

On the basis of mocles of polymerizatiol, there are two mocle s of polymerizatioi.rA) Addition polymerizationB) Condensation polymerization

Addition polymerization or chain growth polymerisation: The repeated addition ofmonomers to the growing polymer chain is called addition polymerization. It isperformed using the molecules containing double or triple bonds (unsaturatedmonomers). The monomer units combine in a head to tail manner to give the polymerchain. The polymers have the same empirical formula as their monomers.

E@'1,'l ncHy:cH)- ,folt^o"-ti'< ^rLcHz- cHrlPE

CHz-= CH 4l

Condensation polymerization or step-growth polymeri sation:This polymerization is carried out by monomers containing two or more reactivefunctional groups such as -OH, -COOH, -NH, react with each other with a loss of smallmolecules like HrO, NH, and HCI. Some typical examples are given below.

t n HLN'(H,6MHz - HzOn H7oC<HLhloo H + n HLtvtn'6,'J'tz -,

t-f -'?,t f -Nu-(ctr't"ln O tl.,l,..^ / 1Nylo^ (, /

tii) Hoor@cwH + H;* tHt-cHz-oft

t= EP S-' :2s1'-cHz-ol;, 1

PDh e -t'LY /en' T?^/Ph/4-'1^'t

(PtU

oe< |

(ttt) n

(iit (l Lt+t-ct-t = c/az t.ur- f "ttHJPP7ca,- f,'ht)

PV

I;l4lL

f, L,n ,

o /ob.^'4- HzO

fl "^ue '

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q Wq at1el b* ' mobu*laA ryel* h'ow 4 &t's+o'- "\

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^ )

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:

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tua1lmn h natoe-,^b ,itg . ^? e rld'-^+'ffi '{i,,ffi;w*Yw?

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wtnriu

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@

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tu,

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\n,rn = t<f fry! Q p ,-- @

bLr.*/ tu-b3,

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a

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-' *rf vT^+ o.r .4 P@4n $olve-,nf .tAP-aA YattuLl Y T ls ,id^vJ"<- +q 7dd F-lre-^|ahet*aa q tloA' v. W Valut E T rn ei na a.

beo'Y Fr,'l rct ') .

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aFrn kr il,.,rfuTtrtf,flS, Phfo) =-*e?= ffi":m\fu"ffiW,,? 4utkar,,,

-/

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bseomn)

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h, o-f* +len @ / c4^e AqM<

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+ +M).f ^_l * @on apl,ofo*ta-h- 6c,&( o.\u^*:, rff**' tr, tn.ptt t*

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e *_ ^)?;,-:- tA-X) cLr *^l _ @. -frnw' ";

s-\IY

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a'n't : -

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Q6: Explain Nitroxide Mecliated Polymerization (NMP) mechanisin giving a suitableexample. How is it different from atom transfer rarlical polymerization (ATRP)?

Nitroxicle Mediated polyme ri z-ation:

A controtrled polyrgerization of styrene in the presence of benzoyl peroxide and the

mediating stable free radical TEMPO (2,2,6, 6-tetramethyl-1-piperidynyl-N-oxy) was ,the first example of a successlul CRP utilizing a :ritroxide-based system.

Control in NMP is achievecl rvith dynamic equiiibration between dorrnant alkoxyamines

and acti.rely propagating radicals (Scheme 1).

In order to effectively mediate polymerization, TEMPO (and other stable free radicals)

should react neither with itself nor with monomer to initiate the growth of new chains,

and it should not participate in side reactions such as the abstraction of B-H atoms.These persistent radicals should also be relatively stable, although their slowdecomposition may help maintain appropriate polymerization rates.

Scheme 1: Dynamic equilibration between dormant alkoxyamines and activelypropagating radicals

&tw

,t*

-t-*ar{rgr*sr{rtrtn t*{ }i

n1 u'.u {eijj .".

TEMPO and its derivatives form a relatively strong covalent bond in alkoxyamines.The SFRP equilibrium constant [ratio of dissociation (kd) to cross-coupling/association(kc) rate constantl is generally very small.The values of Keq are often so low that in the presence of excess TEMPO, theequilibrium become very strongly shifted towards the dormant species and significantlyreduces the polymerization rate.

Atom Transfer Radical Polymerization:

Polymerisation of styrene, acrylates, methacrylates, and acrylonitrile by using varioustransition metal complexes, including nickel, iron, palladium, and rhodium have beenperformed via ATRP.The name ATRP comes from the atom transfer step, which is the key elementary reactionresponsible for the uniform growth of polymeric chains.ATRP originates in atom transfer radical addition. (ATRA) reactions, whieh target theformation of 1:l adducts of alkyl halides and alkenes, which are catalyzed by transitionmetal complexes.In copper mediated ATRP, the carbon-halogen bond of an alkyl halide (RX) is reversiblycleaved by a Cu(I)X/ligand system resulting in a radical (Rx) and Cu(Il)Xrlligand.

4

The radical will mainly either reversibly deactivate or irreversibly terminate [Scheme 21. ,

Scheme 2: Simplified ATRp Mechanism

R-X + Cu(i))Ul-igand X-Cu(Il))Vligand

\R-R

,k,

The rate coefficients of termination decrease significantly with the progress of thepolymerization reaction due to the increase in the chain length and increaseJvir;";rty;ithe system.In fact, the progressive reduction of kt is one of the most important features of manycontrolled radical polymerizations.The role of the different ingredients like monomers, alkyl halide initiators, catalyst,ligand and solvent employed during ATRP is of paramount importance.

Scheme 3: Values of the rate constant for activation (ka), deactivation (kd), propagation(kp) and termination (k) for a bulk styrene polymerizailon ut I10"c.

,"*iS* *4r-'* *SS

*&/ qAtr **or*riprsrd

tr

##. sr-d,'\4ih\

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Q7: How are pol{T* nanocomposites formed? Discuss the types of polymernanocomposites. What are their potential applications?

Als; Nanocomposites are new materials made with fillers which have nanosoze.

I:idffi:,zed inclusions are defined as those have at r.urt on, oi**;;;;;; range of

Polymer nanocomposites zrre polymers (thermoplastic, thermosets) that have been

reinforced with small quantities (less than 5To by rveight) of nano size il particles.Polymer nanocomposites represent an alternative to a filled polymer or polymer blend.

In contrast to conventional composites, where the reinforcement is on the order ol'

microns. PNCs consist of ciiscrete constituents on the order of few nanometers.

There are three mairyrnateriel constituent in aily composite: the matrix, the reinforcement(Fiber) and the ifierfacial region.

Many r:'iethods have been <ievised to prepare polymer/clay nanocolt:posites. In generrrl,

these rnethods (as shown in Figure 1) achier.e molecular level incorporation of the

layered silicate (e.g, montmorillonite (MMT) clay, or synthetic layered silicate) into the

polymer by addition of a modified silicate during the polymerization (in sitttpolymerization).

ffiWffi61ffiffi] |*ruffir-*'| 1**--x;ffi*-1Lffi*,*j{ .:'y:: I i rr-il!j:,'T J

'Jli-d*jp

Figure l: Various methods used to prepare polymer layered-silicate nanocomposites

Most of the studies have been performed on polymers/polymer blends like polystyrene(PS), polypropylene (PP), epoxy resins, pollamides, PVC, PET, polysiloxanes,polyesters, polyurethanes, polyamide 6-PP blends, polyisoprene-PEO blends etc. Thesenovel materials have shown drastic enhancements in the mechanical, electrical, opticaland thermal properties. For example, dramatic improvements in the stiffness and strength,increased dimensional stability, improved flame t'etardancy, improved solvent and UVresistance, and reduction in permeability of gases have been reported.Rheological properties of nanostructured polymer/clay nanocomposites are stronglyinflu-enced by the morphology of the materials, which depends on the clay dispersion inthe polymer matrix as shown in Figures2aand2b.'

If the extended chains are inserted in the self-assembled, well ordered gallery spaces, it istermed as intercalated structure as illustrated,in Figure 2a.lf the individual silicate layersare no longer close enough to interact with adjacent layers it is termed as delaminated orexfoliated structure as explainedin Figure 2b.

6

li li.

Figure 2{t. Intercalated structure Figure 2b. Exfoliated stracture

Polymerization of caprolactum, along rvith modified MlvlT (montmorillonite). resulted inthe first synthesis of an exfoliated Nylon-6 polymer/clay nanocomposite prepared withjust 57o(by weight) loading of clay. They reported 40Vo higher tensile strength,6SVohigher tensile modulus, 60Vo higher flexural strength, 126%o higher flexural modulus andincrease of heat distortion temperature from 65*C to L52*C.As the size of the particle is reduced, the number of defects per particle is also reducedand mechanical properties rise proportionately.

New polymericlay nanocomposites have been developed like polyurethane, PVC,polyesters, polystyrene and polypropylene. Also, some biocompatible polymers likePLA, poly (e-caprolactone) have been synthesized by varying methods and with differentclay loadings (Voby weight).

These materials have applications in the following industries and more.

l. Automotive2. Aerospace3. Construction4. Electrical application5. Food packing

In addition, polymer nanoparticle compounds have very interesting functional applications. Forinstance,l-Fe zO:/ polymer nanocomposites are used as advanced toner materials for high qualitycolour copiers and printers and as contrast agents in NMR analysis, memory devices.These nanocomposites are being used commercially in making tough, heat resistant,nylon timing belt coversRecently, considerable efforts have been devoted to the development of methods for thepreparation of composite particles consisting of polymer cores covered with shells of differentchemical composition. These particles covered with magnetic materials have been used as beadsfor gas separation, or as pigments, catalysts, coatings, flocculents, toners, raw materials recovery,drug delivery and anticorrosion protection.

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