SAN XUT ETHYL ACETATE

I / GII THIU V ETYLACETAT: Axetat etyl hay Etyl axetat l mt hp cht hu c vi cng thc CH3CH2OC(O)CH3. y l mt cht lng khng mu c mi d chu v c trng, tng t nh cc loi sn mng tay hay nc ty sn mng tay, trong n c s dng. L mt loi este thu c t tanol v axt axetic, n thng c vit tt l EtOAc, v c sn xut quy m kh ln lm dung mi. 1.Cc thuc tnh: Axetat etyl l mt dung mi phn cc nh, d bay hi, tng i khng c hi v khng ht m. N l cht nhn cng nh cho lin kt hir yu. Axetat etyl c th ha tan ti 3% nc v n c ha trong nc l ~8% nhit phng. Khi nhit tng cao th ha tan trong nc ca n c tng ln. N c th trn ln vi mt s dung mi khc nh tanol, benzen, axeton hay dietyl ete. N khng n nh trong dung dch c cha axt hay baz mnh. 2.ng dng c bn: Axetat etyl c dng rng ri lm dung mi cho cc phn ng ha hc cng nh thc hin cng vic chit cc ha cht khc. Tng t, n cng c dng trong sn mng tay v thuc ty sn mng tay hay dng kh cafin ca cc ht c ph hay l ch. Axetat etyl cng c mt trong mt s loi ko, hoa qu hay nc hoa do n bay hi rt nhanh v li mi nc hoa trn da. N cng to ra hng v tng t nh ca cc loi qu o, mm xi hay da. y l mt c trng ca phn ln cc este. Axetat etyl cng c mt trong ru vang. N c coi l mt cht gy nhim khi nng cao, khi cc loi ru vang lu trong khng kh. nng cao trong ru vang, n c coi l cht to ra mi v l, l v chua bt thng do b thy phn dn dn tr thnh axt axetic Axetat etyl l mt cht c c hiu lc s dng trong thu thp v nghin cu cn trng. Trong cc l cha axetat etyl, hi ca n s git cht cn trng rt nhanh m khng lm hng hnh dng ca chng. Do khng ht m nn axetat etyl cng gi cho cn trng mm c th thc hin cc cng vic p xc tip theo.

II. S CNG NGH V QUY TRNH CNG NGH :

Dung dch sa 10%

Thit b phn ng

Thit b chng ct

Thit b phn tch lp

Thit b chng ct Sn phm

Dung dch ra

S cng ngh sn xut etyl acetat

Thuyt minh quy trnh cng ngh sn xut etylacetat T acid acetic,etanol,acit sunfuric c cho chm chm ,c a vao thit bi phan ng tao ester, thit bi phan ng duy tri nhit 1000C thu c san phm ethyl acetate,nc va lng d acid acetic,etanol,v H2SO4 Ta a vao thap chng ct, (chng ct hn hp nhit thap 900C),thu c hn hp ng ph gm nc, etyl acetat, acid acetic San phm con lai gm ester va etanol ,acid acetic cho dn qua thit bi tach lp , y ngi ta cho thm dung dch Na2CO3 vao ra sach san phm,loai bo etanol ,loi b acidacetic.Ti thit b phn tch lp thu c 2 pha : pha hu c cha >95% ester v dung dch ra bao gm dung dch Na2CO3,ru, acid ,a san phm hu c vao thit bi chng ct thu tt c cc sn phm l hn hp cng ph c nhit nh hn 700C loai bo phn etanol va nc sau phan ng con lai cho ra san phm etyl acetate tinh khit hn III. TNH TON THIT K THIT B Phn ng to etylacetat l phn ng thun nghch bc 2 . Gi s phn ng sy ra nhit khng i 1000C trong bnh phn ng hot ng gin on. Dng nhp liu ban u cha vi xc tc l HCl c nng 30% . Phng trnh phn ng: CH3COOH + C2H5OH CH3COOC2H5 + H2O K1 l hng s tc phn ng ca phn ng thun K2 l hng s tc phn ng ca phn ng nghch Cc gi tr K, K ln lt nh sau: K1 = 4.76.10-4(l/mol.ph) K2 =1.63.10-4 ( l/mol.ph) I) Tnh chuyn ha ti a ca phn ng II) Tnh thi gian cn thit chuyn ha t III) Xc nh th tch bnh phn vi xut lng este thu c l 50kg/h. thi gian on gia hai m l 0.5 h

IV) Tnh ton b dy ca thit b phn ng Gii: I)Tnh chuyn ha ti a: Theo phng trnh vn tc dng tch phn ca phn ng thun nghch bc 2 : ln ta c : ( 1 1) = X Ae 1 Kc KC = Thay gi tr K1,K2 vo KC= 2.92 Vy chuyn ha ti a l: XAe =0.63 II) Tnh thi gian cn thit chuyn ha t 50% V nhp liu ban u cha 3 mol etanol/1 mol acid acetic do tnh ton cc thng s theo acid acetic CH3COOH + C2H5OH CH3COOC2H5 + H2O Ban u: Phn ng: Sau phn ng : 1 mol x mol 1-x mol 3mol x mol 3-x mol 0mol x mol x mol 0 mol x mol x mol
K1 K2

X Ae (2 X Ae 1) X A K1 =2 C Ao.t = 2.K1( X Ae X A KC

Phng trnh vn tc ca phn ng c dng : -r A = K1 CCH3COOH CC2H5OH K2 CCH3COOC2H5 CH2O

Vy vn tc ca phn ng s l: -r A = C2Ao (4.76.10 (1-x)(3-x) 1.63.10 x )( mol/ l pht) x l

chuyn ha ca axid acetic

-4

-4 2

Khi lng ring ca mi cu t 100 0C nh sau: aciacetic = 0.958g/m

l, etanol= 0.716 g/ml, etylacetat =0. 800g/ml Khi lng ring ca hn hp phn ng coi nh khng i l 0.7765(g/ml) CA0 = Thi gian phn ng c xc nh theo cng thc: ln X Ae (2 X Ae 1) X A K1 =2 C Ao.t = 2.K1( X Ae X A KC t =0.0039(mol/ml)= 3.9 (mol/l)

Thi gian phn ng chuyn ha l 50% : t= 632 pht Thi gian phn ng l 10.5 h l rt ln. do thay v dng xc tc HCl 30% ta dng H2SO4 m c ht lng nc sinh ra sau phn ng. Gi s lng nc sinh ra sau phn ng b ht ht. Vy phng trnh vn tc ca phn ng l:
X A = 0 ,5 0

- r A= C

Ao.

-4 4.76.10 (1-x)(3-x)

t = CAo t=

d XA 2 k CA o(1 )(3 )x x
0.5

ln
0

=137,59 (ph)

vy thi gian phn ng:

t = 137.59 ph

III)xc nh th tch bnh phn ng: Gi mA l khi lng acidacetic cho vo bnh nhp liu ta c phng trnh: mA (0,5.88) =50 60 2, 29 + 0,5 mA = 190,23kg (acidacetic / m) vy tng khi lng nhp liu : 190,23+
.3.46 =627 (kg)

Vy th tch hn hp phn ng cha trong bnh : V=627/0,7765= 807.5(l) Do khi thit k thit b c th tch ti thiu ca bnh phn ng l 807.5(l)
V1

IV) Tnh ton b dy ca thit b phn ng: Th tch ca thit b phn ng l 1000(l) chn H=2D , y np elip tiu chun h= 0.25 D V= V1+V2+V3
V1+V3= 4/3 . R.R. h= 4/3 D/2. D/2. 0.25D P1
P 2

V2 P3

V2= R2H =2 R3 = D3/2 Vy D=0.817( m =>H = 1.64 (m) Gia nhit bng hi nc bo ha 120 0C vi p sut l 2.025 kg/cm2

V3 V3

Gi s p sut trong bnh phn ng l 1.9 kg/cm2 1. Chn vt liu ch to thit b: Thit b cha acid sunfuric c tnh n mn cao chn vt liu ch to thit b l OX18H10T 2. Cc thng s tnh ton: p sut tnh ton : p sut kh quyn P1, P2=2.025 kg/cm2, P3= 1.9 kg/cm2 Nhit tnh ton 120oC l nhit ca hi nc bo ha

3. Tnh ton thit b:

Tnh ton thn thit b: Thn ca thit b chi p sut ngoi l 2.025kg/cm2= 1.987N/mm2 Chu p sut trong l 1.9 kg/cm2=1.8639 N/mm2

Tnh ton thn thit b chu p sut trong: 1200C = 120N/mm2 vi = 1

Ta tnh gi tr ca biu thc :

. h

. h= 64.38 > 25
S =

P.Dt = 6,35 (mm) 2.[ ] h

S = 8.75( mm)

[ P] =

2 [ ] h ( S Ca ) Dt + ( S Ca )

thay s ta c [P]= 2.173 N/mm2 tha

Tnh ton thn thit b chu p sut ngoi: Khi thn tr lp vi hai y elip th:L= 2.0,817+1/3. 0.25. 0.817=1,702(m)

S ' = 1,18 D(

Pn L 0,4 ) Et D

Et= 2.105 (N/mm2) S= 13 mm Vy S= 15 mm Tnh gi tr biu thc Dt = 21,5 2( S Ca )

1.5

Dt = 0.1 2( S Ca )

L = 2.083 Dt

Biu thc

1,5

2( S Ca ) L Dt < < tha Dt Dt 2( S C a )

Kim tra tnh thit b: 0,3 Et 2( S Ca ) 3 ( ) c Dt

c = 220 N/mm2 0,3 Et 2( S Ca ) 3 ( ) c Dt L = 2.083 Dt L Et 2( S Ca ) 3 ( ) tha .Vy b dy ca thn thit c Dt

= 1.02

Vy biu th D > 0,3

t

b l 15 mm
Tnh b dy ca y:

y ca thit b chu p sut ngoi l 2.025kg/cm2= 1.987N/mm2 Chu p sut trong l 1.9 kg/cm2=1.8639 N/mm2

Trng hp y chu p sut trong 1200C = 120N/mm2 vi = 1

ta tnh gi tr ca biu thc :

. h . h= 64.38 > 25

thay cc gi tr vo ta c :

vy

S'=

PRt 2 [ ] h

thay cc gi tr vo ta c S= 7.65.10-3 m= 7.65 mm S= 10 mm Kim tra p sut cho php

[ P] =

2 [ ] h ( S Ca ) Rt + ( S Ca )

thay s ta c [P]= 2.173 N/mm2 tha

Trng hp y chu p sut ngoi: Rt/S=Dt/S= 57.94 X= 0.9

Tnh biu thc 0,15Et = 151, 5 X c 2 [ ] ( S Ca ) Rt 0,15 Et < nn [ P ] = S Xc Rt

Et ( S Ca ) + 5 XRt c Et ( S Ca ) 6, 7 X .Rt (1 X ) c

vy =1.36 [P]=

= 5,255 tha iu kin bn

Vy b dy y, thn , np ca thit b l 15 mm

IV:Mt s phng phap nhm tng nng sut quy trinh tng hp etyl acetat:
Thng co ba phng phap c ban nng cao hiu sut: Cho mt lng d tac cht nh etanol hay acid acetic (thng thng ngi ta dung lng d etanol).Lam cho cn bng chuyn dich v bn phai.Co th lam tng hiu sut ester. Phng phap tach nc:lam cho phan ng chuyn dich v bn phai (do thiu hut mt lng nc phan ng co xu hng tao nc),chung ta co th chng ct ng phi hai cu t.Hay cho vao lng d acid sunfuric (hut nc) Tao hn hp ang phi ba cu t etyl acetat etanol nc.Phng phap thng c s dung trong cng nghip,loai nc hoc ester.

Trc ht xet vic loai nc ra ngoai: Dung d lng etanol lin tuc chng ct keo ra,etanol keo theo ca nc ra cung,vi etanol tao vi nc mt hn hp si ng phi hai cu t,vi vic thng xuyn bi ct ra cung vi etanol lam cho lng nc trong hn hp giam,lng etyl acetat tng ln. Ct nc ra khoi phan ng nh vic cho thm dung mi tr khng hoa tan vi nc tao hn hp si ba cu t nc etanol dung mi tr,co nhit si thp hn nht si cua nc,ct loai chung ra khoi phan ng nhit nay,hn hp c ct ra ngng tu lam lanh tach thanh hai pha ,pha nc loai ra ngoai,pha hu c co cha etanol quay lai thit bi phan ng ester hoa.Cac dung mi tr thng c s dung o la benzen,toluen,cloroform,dicloetan,tetracloruacacbon Ct ester ra ngoai: chng ct hn hp ng phi ba cu t,chng ct ester ra c ngng tu lam lanh,phn pha tach ra ester

 c trng cua cac nguyn liu thanh phm:

-

Axit axetic co nhit si la 118,50C,etanol la 78,390C,etyl axetat si 770C,im si ng phi cua ba cu t ester,etanol,nc la 700C,chung co thanh phn la 832% ester,9% etanol;7,8%nc im si ng phi hai cu t nc,etanol la 78,20C. Ester,etanol la 71,80C. Ester,nc la 70,50C

V. tai