ph controlled assembly of a polybutadiene poly(methacrylic acid) copolymer in water: packing considerations and kinetic limitations
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1 Supplmtry Mtril (ESI) for Soft Mttr This jourl is Th Royl Soity of hmistry 2009 p otroll ssmly of polyuti poly(mthryli i) opolymr i wtr pkig osirtios kiti limittios hristi Fryhough, Athoy J. Ry, Giuspp Bttgli * opolymr Sythsis Th xprimtl prour for th sythsis of th polyuti-poly(tutyl mthrylt) (PB-P(t-MA)) ws prform ur high vuum ulss othrwis stt. Brksls or grslss tps wr us for th trsfr of rgts from mpouls ito glss mixig vssl. -x (Fishr) ws istill from - utyllithium (-Li) for us ttrhyrofur (Fishr) ws ri ovr soium zopho th istill from polystyryllithium just for us. ti (Alrih) ws os t -70 ito msurig ylir gss. It ws istill twi oto soium mirrors ri ovr h for pproximtly 30 miuts for filly ig purifi ovr -Li. Th moomr ws kpt t tmprtur of -30 throughout th prour. t-utyl mthrylt (Alrih) ws gss ri ovr lium hyri for 48 hours th gss o mor for istilltio oto trithyllumiium (Alrih, 1m 3, 1.9M, 25wt.% i tolu) ur ru prssur. stirrig yllow olour ws osrv iitig rsol purity. Th solutio ws stirr for 30 miuts for istilltio ito mpoul log with TF. s-tyllithium (Alrih) ws us s suppli. 1,1-Diphylthyl (DPE) (Alrih) ws istill from 1,1-iphylhxyllithium prior to us. Lithium hlori (98%, Alrih) ws ri i mpoul ur vuum ovright t TF (. 3m 3 ) ws istill ito th mpoul ur ru prssur for it ws sl ur vuum. 1,3-ti gs (10.0g, 0.19mols) ws polymriz i -hx (150m 3 ) t room tmprtur ovright, usig s-utyllithium (5.6mmol) s th iititor. A smpl of th polyuti (PB) ws tk pripitt i mthol, ollt ri. Th -hx ws rmov ur ru prssur TF (150m 3 ) istill oto th polymr. Aitio of DPE (2.1g, 0.012mols) prou p r solutio. Lil (2.35g, 0.056mol) ws issolv with stirrig t -30. t-tyl mthrylt (9.52g, 0.067mols) ws t -78 to giv olorlss solutio. Th rtio ws trmit with gss mthol ftr 45miuts. 2,6-Di-trt-utyl-4- mthylphol ws to th solutio. Th polymr ws pripitt i mthol
2 Supplmtry Mtril (ESI) for Soft Mttr This jourl is Th Royl Soity of hmistry 2009 (1000m 3 ) to yil whit soli whih ws filtr, ir ri ri i vuo. Th grl shm is show i figur 1. yrolysis of th poly(t-utyl mthrylt) ws prform ur itrog y htig 5%w/v solutio of th polymr i 1,4-iox (Fishr, us s riv) to whih slight stoihiomtri xss of 10M hyrohlori i ws. Aftr 4 ys, th solvt ws prtilly rmov ur vuum wtr. Th solutio ws ilys gist wtr (rgrt llulos 1000 molulr wight ut off) th rsultt polyuti-poly(mthryli i) (PB-PMAA) ws isolt y frz ryig. s-li hx room tmprtur - Li + TF - Li+ R= t-tyl (R= ftr hyrolysis) -78 Lil m+1 M R M M - Li + R' R th mthol to trmit Figur 1 Shm showig th sythsis of th PB-P(t-MA) hrtriztio Th Siz Exlusio hromtogrphy (SE) rsults iit tht th rtio ws sussful. Th tr for th ilok hs shift to lowr lutio volum ompr to th polyuti homopolymr smpl s s o figur 2.
3 Supplmtry Mtril (ESI) for Soft Mttr This jourl is Th Royl Soity of hmistry 2009 PB-P(tMA) polyuti lutio volum/mls Figur 2 SE tr of polyuti--poly(t-utylmthrylt) th polyuti homopolymr smpl Th 1 NMR rsults of th ilok for ftr hyrolysis s i figurs 2 3 rsptivly. Both smpls wr ru i utrt hloroform. Th oly hg i th sptrum is th rutio i th itgrl for pk t δ1.35 orrspoig to th rmovl of th t-utyl group, whr thr r two ovrlppig rsos for th t-utyl th mthyl group of th mthrylt i figur 2, thr is just th mthyl group i figur 3. ( ) 3 m
4 Supplmtry Mtril (ESI) for Soft Mttr This jourl is Th Royl Soity of hmistry Figur 3 1 NMR of PB-PtMA ppm m iox ppm Figur 4 1 NMR of PB-PMAA Fourir Trsform Ifr-R Attut Totl Rflt (FTIR-ATR) ws us to ofirm tht th hyrolysis rtio h sussful. This hs th vtg of
5 Supplmtry Mtril (ESI) for Soft Mttr This jourl is Th Royl Soity of hmistry 2009 th msurmt ig prform o th soli polymr. With solutio msurmts prolms ris with rgr to solvt sltivity milliztio oul fft to rsults. t-tyl groups sor t 1366m -1 istitiv pk s t this wvumr i figur 4 whih ot s i th prout of th hyrolysis rtio i figur 5 iitig th sussful hyrolysis of th prt ilok. Th shift i th royl pk sorptio from 1722 to 1704m -1 lso rflts th str hyrolysis log with th ro sorptio from m -1 sigifyig i - strth %T m-1 Figur 4; FTIR-ATR of PB-PtMA (prior to hyrolysis) %T m-1 Figur 5 FTIR-ATR of PB-PMAA
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