BI 4: TNG HP POLY METHYLMETHACRYLATE I. Mc ch: iu ch poly methylmethacrylate. Xc nh khi lng phn t trung bnh v a phn tn. II.

. Gii thiu Poly methylmethacrylate (PMMA) l mt loi polymer quan trng v c nhiu ng dng thc tin. PMMA bn vi thi tit, va p, khng dung dch acid v bazo long, d nhum v t b mi mn so vi thy tinh. Thng c dng lm sn xut thy tinh hu c, knh chiu hu, knh n tn hiu, mt ng h, Khi lng phn t trung bnh v a phn tn, nhit chuyn ha thy tinh chu nh hng ca nhit phn ng, lng cht khi mo v dung mi thc hin phn ng. III. Thc nghim 1. Dng c, ha cht Bnh 3 c, 250 ml H thng khuy Hon lu (ngng t MeOH) Nhit k 2000C Ni nhm Gi nng Bnh kh nitrogen Chai thy tinh 100 ml ng dn kh Kim ly mu MMA Ethylene glycol monoethyl ether Ammonium persulphate Silicone oil Nc tinh khit

2. Tin trnh th nghim - Chng ct li monomer MMA:

Thit lp h thng phn ng khuy t pha trong ni nhm cha silicone oil, t h thng trn bp gia nhit. Sc kh nitrogen lin tc Gia nhit n nhit cn phn ng Cho dung mi v monomer vo khuy u Ch cho nhit ca h phn ng n nh Cho cht khi mo vo bnh phn ng Theo di phn ng v tin hnh ly mu phn tch. C ch phn ng trng ngng PMMA: - Giai on khi mo: Cht khi mo S2O82- ha tan trong nc phn ly thnh gc t do l ion sulphate. Ion gc t do ny s len li vo trong mixel v tc kch vo ni i ca MMA to thnh gc t do MMA.
NH4+ -O S O O O O S O ONH4+ O

O-

ammonium persulphate

ion sulphateradical

CH3
-

CH3 CH2
-

CH2

C OCOCH3

C OCOCH3

methyl methacrylate

- Giai on pht trin mch: Cc gc t do MMA tip tc tc kch vo ni i ca cc monomer khc v sinh ra gc t do mi lm tng thm n v CH2C(CH3)OCOCH3, chu k c lp li nhiu ln to thnh chui polymer trong mixel.

CH3 CH2
-

CH3

CH2

C OCOCH3

OCOCH3

H2 C CH2
-

CH3
CH2 C

CH3OCO

OCOCH3

- Giai on tt mch: Cc gc t do trn cc chui polymer gn li vi nhau theo kiu u ni ui.

H2 C CH2
-

CH3
CH2 C

CH3
C CH2

H2 C CH2 C O O-

CH3OCO

OCOCH3

n OCOCH3

n OCOCH3

CH3
-

CH3 C CH2 SO-4

O4S

CH2 C

CH3OCO n+1

OCOCH3 n+1

1. Kho st nh hng ca nhit a. nhit 700C ( ngy thc hin 27/10/2011) Bng s liu lng ha cht cn thit cho phn ng. Tn ha cht S lng MMA 8.06 g Ethylene glycol monoethyl 5.072 g ether Ammonium persulphate 0.102 g Nc tinh khit 40 ml 13h 35: Trn tt c cc ha cht, nhit phn ng 550C, 350 rpm. 13h 45: Cho mt na lng phn ng vo bnh phn ng, nhit phn ng 600C, 350 rpm. 14h 5: Cho mt na lng cn li vo bnh phn ng, nhit phn ng 650C, 500 rpm.

14h 15: Hn hp bt u c, nhit phn ng 650C Quy trnh ly mu: Thi gian 14h 15 14h 30 14h 45 S ln ly mu Nhit (0C) Nhn xt 1 1 1 70 76 76 Hi c c hn, hat mn Ht mn hn, nht cao

b. nhit 900C ( ngy thc hin 27/10/2011) Bng s liu lng ha cht cn thit cho phn ng. Tn ha cht MMA Ethylene ether glycol monoethyl S lng 8.04 g 4.0184 g 0.101 g 40 ml

Ammonium persulphate Nc tinh khit

15h 20: Trn tt c cc ha cht, nhit phn ng 700C, 350 rpm. 15h 22: Nh tng git monomer vo bnh phn ng, nhit phn ng 760C, 350 rpm. 15h 30: hn hp bt u uc, nhit phn ng 760C, 500 rpm. 15h 45: Kt thc nh monomer, nhit phn ng 850C Quy trnh ly mu: Thi gian 15h 37 15h 52 16h 37 S ln ly mu Nhit (0C) Nhn xt 1 1 1 81 90 91 c nhanh Hat mn Ht mn hn, nht cao

Kt lun: Khi gia tng nhit s lm tc phn ng trng hp tng. iu th hin qua mn ca ht.

2. Kho st nh hng ca cht khi mo ammonium persulphate. a. nhit 900C ( ngy thc hin 28/10/2011) Bng s liu lng ha cht cn thit cho phn ng. Tn ha cht MMA Ethylene ether glycol monoethyl S lng 8.04 g 4.0184 g 0.302 g 40 ml

Ammonium persulphate Nc tinh khit

7h 49: Trn tt c cc ha cht, nhit phn ng 800C, 350 rpm. 7h 55: Nh tng git monomer vo bnh phn ng, nhit phn ng 850C, 350 rpm. 8h 00: hn hp bt u uc, nhit phn ng 870C, 500 rpm. 8h 15: Kt thc nh monomer, nhit phn ng 920C Quy trnh ly mu: Thi gian 8h 00 8h 30 9h 00 S ln ly mu Nhit (0C) Nhn xt 1 1 1 87 92 90 c rt nhanh Ht mn, nhiu bt Ht mn hn, nht rt cao

Kt lun: Khi gia tng cht khi mo hay nng cht khi mo m nhit khng i th vn tc phn ng tng c th hin qua c v nht.

Kt qu o kch thc ht trung bnh v a phn tn ca PMMA. Nhit (0C ) Th tch pha Zaverage PDI

long (ml) 70 (ln 1) 70 (ln 2) 70 (ln 3) 50 50 50

(nm) 129.2 299,5 7746 164.1 409.3 670 227.9 504.9 604.5 0.237 0.063 1.000 0.009 0.014 0.276 0.046 0.099 0.018

90 (0.101) (ln 50 1) 90 (0.101) (ln 50 2) 90 (0.101) (ln 50 3) 90 (0.302) (ln 50 1) 90 (0.302) (ln 50 2) 90 (0.302) (ln 50 3)

Kt lun: T bng s liu ta thy kch thc ht trung bnh t l theo a phan tn. IV. Tho lun iu kin ti u tng hp polymer PMMA: Kh nitrogen phi sc vo lin tc to mi trng tr cho phn ng. Mi trng thc hin phn ng nn gi nhit phng. Cc t l cht khi mo, monomer dung mi a vo phn ng phi tht s chnh xc, trnh tht thot. Cc khong nhit kho st khng c trn lch qu cao v tt nht l nm trong khong 10C. Qu trnh ly mu kho st phi m bo nhanh v hiu qu nu khng polymer s b cc yu t bn ngoi tc ng nh oxy ha