Bao Cao Thuc Hanh

BO CO THC TP TT NGHIP
LI M U
Thng 9 nm 2013 va qua, chng em c tri qua k thc tp cng
nghip ti Cng ty c phn Bt git v Ha cht c Giang. y thc s l c
hi tt cho em m mang vn hiu bit, p dng nhng g c hc trong
nh trng. Hn na c tip xc trc tip vi mi trng lm vic thc t
trong nh my, mt vic m em v cc bn khng th c t nhng kin thc
sch v. Qu trnh thc tp 2 thng, c s hng dn chi tit, ch bo tn tnh
ca cn b, cng nhn vin nh my cng cc thy c gio trong b mn, em
tip thu c mt lng kin thc nht nh, tng hp li hon thnh bi bo
co ny.
Tuy nhin vi trnh ca sinh vin mi bc sang nm th 4, hiu bit cn
rt hn ch, qu trnh thc tp vn thiu kinh nghim v cha khoa hc nn bi
bo co ca em khng th trnh khi nhng thiu xt, cha tht chnh xc. Em
rt mong nhn c nhng gp cng nh hng dn ca cc thy c trong b
mn hon thin hn bi bo co ny.
Em xin chn thnh cm n !
MC LC
LI M U .......................................................................................................................................... .
DANH MC CC BNG V HNH V ............................................................................................. 5
CHNG 1: GII THIU V CNG TY C PHN BT GIT ...................................................... 6
V HA CHT C GIANG. ............................................................................................................. 6
1.1.Gii thiu chung............................................................................................................................ 6
1.2. Qu trnh pht trin ca cng ty: .................................................................................................. 8
1.3. Gii thiu v cc phng ban v cc phn xng sn xut trong cng ty. .................................... 9
1.3.1. Phng nghin cu v pht trin sn phm. ........................................................................... 9
1.3.2.Phng kim tra cht lng sn phm. .................................................................................... 9
1.3.3.Phn xng bt git. .............................................................................................................. 9
1.3.4.Phn xng ha cht tinh khit. ............................................................................................. 9
1.3.5.Phn xng axit photphoric. .................................................................................................. 9
1.3.6.Phn xng cht hot ng b mt LAS.............................................................................. 10
CHNG 2: PHN XNG BT GIT. ......................................................................................... 12
2.1. Nguyn liu. ............................................................................................................................... 12
2.1.1. Cht hot ng b mt LAS (Linear Alkylbenzene Sulfonate). ......................................... 14
2.1.2. STTP( Sodium tripolyphosphat). ........................................................................................ 15
2.1.3. Sodiumcacbonat( Na2CO3).................................................................................................. 16
2.1.4. Natri hydroxit( NaOH). ....................................................................................................... 16
2.1.5. Natri sunfat( Na2SO4). ......................................................................................................... 16
2.1.6. Cht thm. ........................................................................................................................... 16
2.1.7. Cc loi ph gia khc. ......................................................................................................... 17
2.2. Quy trnh sn xut bt git. ....................................................................................................... 17
CHNG 3: PHN XNG CHT HOT NG B MT LAS. ................................................ 19
3.1. Nguyn liu chnh: ..................................................................................................................... 19
3.2. S khi. ................................................................................................................................. 21
3.3. Quy trnh cng ngh................................................................................................................... 22
3.3.1. Phn khu 11: Khu lm kh khng kh. ................................................................................ 25
3.3.2. Phn khu 25: Khu gia nhit lu hunh................................................................................ 27
SVTH: NGUYN THNH CHUNG 20109705 CN HA DU
3.3.3. Phn khu 12: Khu sn xut SO3. ........................................................................................ 28
3.3.4. Phn khu 16: Khu phn ng to sn phm LAS. ................................................................ 30
3.3.5. Phn khu 14: Khu x l kh thi. ........................................................................................ 32
CHNG 4: PHN XNG AXIT PHOTPHORIC. ........................................................................ 34
4.1. Tng quan l thuyt. .................................................................................................................. 34
4.1.1. Tnh cht vt l v ha hc ca photpho: ........................................................................... 34
4.1.2. Axit photphoric. .................................................................................................................. 36
4.2. Phn xng sn xut axit photphoric bng phng php nhit. ................................................ 39
4.2.1. Nguyn liu ......................................................................................................................... 39
4.2.2. S khi. .......................................................................................................................... 39
4.2.3.S cng ngh sn xut axit photphoric bng phng php nhit.................................... 39
CHNG 5: PHNG KIM TRA CHT LNG SN PHM. ..................................................... 43
5.1. Axit phosphoric k thut: TC 02:2005/HCG. ........................................................................ 43
5.1.1.Yu cu k thut: ................................................................................................................. 43
5.1.2. Xc nh hm lng axit photphoric................................................................................... 44
5.1.3. Ghi nhn, vn chuyn, bo qun, bao gi. .......................................................................... 45
5.2. Xc nh hm lng clo. ............................................................................................................ 46
5.2.1. Thuc th v dung dch....................................................................................................... 46
5.2.2. Cch tin hnh..................................................................................................................... 46
5.3. Xc nh hm lng sunfat. ....................................................................................................... 46
5.3.1. Thuc th v dung dch....................................................................................................... 46
5.3.2. Tin hnh th. ..................................................................................................................... 46
5.4. Xc nh hm lng st. ............................................................................................................ 47
5.4.1. Thuc th v dung dch....................................................................................................... 47
5.4.2. Cch tin hnh..................................................................................................................... 47
5.5. Xc nh hm lng kim loi nng. ........................................................................................... 47
5.5.1. Thuc th v dung dch....................................................................................................... 47
5.5.2. Cch tin hnh..................................................................................................................... 47
5.6. Xc nh hm lng NO3 trong axit. ........................................................................................ 48
5.6.1. Thuc th v dung dch....................................................................................................... 48
5.6.2. Cch kim tra. ..................................................................................................................... 48
5.6.3. Tin hnh th. ..................................................................................................................... 48
5.7. Kim tra cht lng bn sn phm xc nh ch s axit tng (AV). .......................................... 48
5.7.1.nh ngha:........................................................................................................................... 48
5.7.2.Ha cht v dng c. ............................................................................................................ 48
5.7.3.Ni dung quy nh................................................................................................................ 49
5.8.Kim tra cht lng LAS. ........................................................................................................... 50
5.8.1. Yu cu k thut: ................................................................................................................ 50
5.8.2. Phng php th: ................................................................................................................ 50
5.9.Xc nh hm lng H2SO4. ....................................................................................................... 51
5.9.1. Nguyn tc: ......................................................................................................................... 51
5.9.2. Ha cht v thuc th: ........................................................................................................ 51
5.9.3. Thit b v dng c: ............................................................................................................ 52
5.9.4. Cch tin hnh: ................................................................................................................... 52
5.9.5.Tnh kt qu. ........................................................................................................................ 52
5.10. Xc nh hm lng nc bng phng php Karl Fisher: ..................................................... 53
5.10.1. Phm vi p dng:............................................................................................................... 53
5.10.2. nh ngha hm lng nc. ............................................................................................ 53
5.10.3. Nguyn tc. ....................................................................................................................... 53
5.10.4. Ha cht v thuc th. ...................................................................................................... 53
5.10.5. Thit b v dng c............................................................................................................ 53
5.10.6. Cch tin hnh................................................................................................................... 54
5.10.7. Tnh kt qu: ..................................................................................................................... 55
5.11. Xc nh hm lng du t do. ................................................................................................ 55
5.11.1. Nguyn tc: ....................................................................................................................... 55
5.11.2. Ha cht v thuc th: ...................................................................................................... 55
5.11.3. Dng c: ............................................................................................................................ 56
5.11.4. Cch tin hnh................................................................................................................... 56
5.11.5. Tnh kt qu: ..................................................................................................................... 56
5.12. Ch s axit. ............................................................................................................................... 57
5.12.1. nh ngha ch s axit: ...................................................................................................... 57
5.12.2. Ha cht v thuc th: ...................................................................................................... 57
5.12.3. Dng c: ............................................................................................................................ 57
5.12.4. Cch tin hnh:.................................................................................................................. 57
5.12.5. Tnh kt qu: ..................................................................................................................... 57
5.13. Xc nh mu. ..................................................................................................................... 58
5.13.1. Nguyn tc: ....................................................................................................................... 58
5.13.2. Ha cht v thuc th: ...................................................................................................... 58
5.13.3. Dng c: ............................................................................................................................ 58
5.13.4. Cch tin hnh:.................................................................................................................. 58
KT LUN........................................................................................................................................... 59
TI LIU THAM KHO .................................................................................................................... 60
DANH MC CC BNG V HNH V

Bng 1: n phn ng kem ti 3kg.
Bng 2: Yu cu v cht lng kem v bt nn:
Bng 3: Cc ch tiu v mc cht lng ca sn phm axit photphoric.
Bng 4: Cc ch tiu ngoi quan.
Bng 5: Cc ch tiu ha l.
Hnh 1: S sn xut bt git:
Hnh 2: S khi xng LAS.
Hnh 3: S khu lm kh khng kh.
Hnh 4: S khu gia nhit lu hunh.
Hnh 5: S khu sn xut SO3.
Hnh 6: S khu sunfonat ha.
Hnh 7: S khu hydrat ha sn phm.
Hnh 8: S khu x l kh thi.
Hnh 9: S khi phn xng axit photphoric.
Hnh 10: S cng ngh sn xut axit photphoric bng phng php nhit.
CHNG 1: GII THIU V CNG TY C PHN BT GIT

V HA CHT C GIANG.
1.1.Gii thiu chung.

Cng ty Ha cht c Giang l mt cng ty Nh nc, trc thuc Tng
Cng Ty Ha Cht Vit Nam.
Cng ty Ha cht c Giang l mt trong nhng cng ty hot ng trong
lnh vc Ha cht thnh lp t nm 1963, trn din tch 6000m2 cch trung
tm H Ni 15km.
Tn ting Vit
: Cng ty c phn Bt git v Ho cht

c Giang
Tn ting Anh
: Ducgiang Chemicals & Detergent

Powder Joint Stock Company
Tn vit tt
: DGC
Tr s
: 18/44 ph c Giang, phng

Thng Thanh, Long Bin, H Ni
in thoi
: (04) 8 271 620
Fax
: (04) 8 271 068
Website
: www.ducgiangchem.vn
Email
ducgiangchemco@hn.vnn.vn
ng k kinh doanh s
0103003850
M s thu
0101452588
Ti khon
: 002 - 107068 - 001 Ngn hng Hng

Kng v Thng Hi Chi nhnh H
Ni.
Vn iu l
66.000.000.000 ng
Ngnh ngh ng k kinh doanh:

- Sn xut v bun bn nguyn liu v cc mt hng ho cht (tr ho cht
Nh nc cm);
- Sn xut v bun bn cc mt hng cao su, sn, cht do, phn bn, st,
thp, kim loi mu;
- Sn xut v bun bn my mc, thit b in v cc linh kin ca chng,
vt liu in, dng c c kh;
- Sn xut v bun bn cc mt hng nhin liu khong, du khong v cc
sn phm chng ct t chng; cc cht cha bi tum; cc loi sp khong
cht;
- Cho thu nh xng;
- Thm d, khai thc, ch bin v tiu th khong sn.
Cng ty c Giang chuyn cung cp cc sn phm ha cht ph cho sn
xut nng nghip, cng nghip nng v cng nghip nh cc mt hng bao gm
c: Hng tinh khit v cng nghip.
Hi ng qun tr v ban gim c.
- Hi ng qun tr:
ng o Hu Huyn
Ch tch
ng o Vit Hng
U vin
ng Lu Bch t
U vin
B Phan Th Nhung
U vin
ng Li Cao Hin
U vin
- Ban kim sot:

ng V Vn Ng
Trng ban
ng V Minh Thuyt
U vin
ng Nguyn Tin Khang
U vin
- Ban Gim c:
ng o Hu Huyn
Tng Gim c
ng o Vit Hng
Ph Tng Gim c
ng o Hu Duy Anh
Ph Tng Gim c
1.2. Qu trnh pht trin ca cng ty:

1963 1985: Sn xut ho cht tinh khit, ho cht k thut cung cp
cho min Bc.
1986 1990: Sn xut kem git, bt git.
1990 n nay:
- Sn xut phtpho vng, Natritriphotphat;
- Axt pht phoric, cc hp cht ca photpho ch yu xut khu, mt
phn cung cp cho th trng ni a;
- M rng hin i ho phn xng ho ho cht tinh khit, ho cht
k thut;
- Sn xut bt git v cht ty ra;
- Tng doanh s hin ti l 20 triu USD ;
- S nhn cng: 220 ngi;
Cc gii thng cng ty t c:

- Cng ty c phong tro bo v thit b v mi trng xut sc nm
2007;
- Gii n v tiu biu v sinh mi trng (PX LAS);
- Gii tit kim vt t (PX LAS).
1.3. Gii thiu v cc phng ban v cc phn xng sn xut trong cng ty.
1.3.1. Phng nghin cu v pht trin sn phm.
L phng c nhim v nghin cu v pht trin sn phm ra m hnh
cng nghip bt u t nhng nghin cu v th nghim nh ri n m hnh
sau y mi n thc nghim. Phng gm cc thit b nh my sy, my nung,
my o quang, my o Ph, F-, cn in t,
1.3.2.Phng kim tra cht lng sn phm.
y l phng th nghim chuyn phn tch cht lc sn phm xem
t yu cu cha, ng thi l phng nghin cu to mi cho bt git, nc
x vi
1.3.3.Phn xng bt git.
Sn xut bt git, thnh phn chnh ca bt git l LASNa (khng nh hn
18%), STTP, Sodiumcacbonate, Natrisunfate, cht ty trng quang hc, hng
liu. Sn phn bt git c phn phi trn ton quc (ch yu l trong khu vc
min Nam).
1.3.4.Phn xng ha cht tinh khit.
Sn xut cc loi ha cht tinh khit cho mt s ngnh cng nghip, phng
th nghim. y, sn xut ch yu l: Cn tuyt i, HCl 36-38%, H2SO4,
Na2SO4, Ch yu sn sut theo phng php chng ct.
Ngoi ra cn c: Nc lau nh, nc ra chn, nc x vi, du gi, nc ty .
1.3.5.Phn xng axit photphoric.
Nguyn liu:
P trng, lu ngoi nh sng th P chuyn thnh mu vng v mt phn
ha .
Axit Photphoric gm 3 loi:
- Axit photphoric cng nghip 86-87%;
- Axit photphoric cng nghip 85%;
- Axit photphoric cng nghip 70%.

Thnh phn trong cng nghip ln hn 85%; lng As nh hn 0.0001%;
34 C : 1.688g/ml.
C 2 phng php sn xut l nhit luyn v trch ly. Hin ti nh my
ang dng phng php nhit luyn do n to H3PO4 tinh khit hn:
Phn ng: P4 + O2 P2O5
P2O5 + H2O H3PO4.
0
Dy chuyn sn xut:
HA
LNG
PHOTPH
O
THNG
CHA
THP
T
THNG
TRN
NG
GI
Photpho c ha lng bng hi nc, sau cho vo thp t, va t va

hp th dc axit photphoric 85%. Sau em i lc cn to axit (sn phm ).
1.3.6.Phn xng cht hot ng b mt LAS.
LAS c sn xut t dn xut Benzen:
LAB
LAS
vi R = C11 C13
LAS hay LABSA Liner Alkyl Benzen Sulfonic Acid l mt trong nhng
thnh phn quan trng nht trong bt git, khi kt hp vi mt s cht n nh
Na2SO4 s to liner alkyl benzen sulfonat natri l mt cht hot ng b mt
dng anion c tc dng ty ra vt bn.
10
Cht hot ng b mt LASNa c chia thnh 2 phn: phn a nc l

nhm NaSO3- ; phn k nc l gc alkyl benzen.
C ch ty nh sau:
Cc phn t ca chng c mt u phn cc v mt u khng phn cc, v
vy cc phn t c cn bng trong cc mi trng c cc v khng c cc.
Trong nc, cc phn t ny to thnh nhng cu trc hnh cu nh c gi l
mixen, vi cc u phn cc hng ra ngoi v cc u khng phn cc hng
vo trong. bn trong, phn mixen khng phn cc ny s ha tan trong cc
phn t du. V vy, khi git cc mixen ca x phng s bt cc phn t khng
c cc (du, m) phn ct chng li ko chng v pha nc v b ra tri i.
i vi x phng c tc dng c th b hn ch trong nc cng v cc ion
dng ca st, magi, canxi c trong nc cng kt hp vi u mang in m
ca cc chui phn t trong x phng to kt ta hao ph x phng lm gim tc
dng git ra v nh hng n cht lng vi si. Tuy nhin, cc cht ty ra
hay x phng tng hp c th gii quyt c kh khn ny. Cc cht ty ra
tng hp c cc nhm c cc nh cc hp cht sulfonat (- SO3 ) hoc
etoxysulfat c gn vo cc chui hyrocacbon. Cc nhm tng hp ny mang
in m, chng ch lin kt yu vi cc ion dng (ca st, magi, canxi) trong
nc cng v nh kh nng lm sch vn rt tt.
Ch : s khc bit gia x phng loi c v mi; u ging nhau v cu
trc 2 u, khc nhau ch c l gc HC ca axit bo mi l gc HC bt k,
c c u phn cc l COO-Na+ cn mi c th l cacboxylat hoc sunfat v c
th ty ra tt trong nc cng.
11
CHNG 2: PHN XNG BT GIT.

2.1. Nguyn liu.
Cc nguyn liu th:
- Soda kh;
- STPP;
- Cc mui sunfat (Na2SO4);
- xt NaOH;
- LAS;
- Cht thm (tinh du);
- Ph gia.
Sau y l n phn ng kem ti 3kg ca phn xng bt git:
Bng 1: n phn ng kem ti 3kg.
n Quy
v cch
nh
mc 1
tn
sn
phm
n
phn
ng
STT
Tn
nguyn
liu
Nc
Kg
S a
Kg
98%
82
190
Sunfat
Kg
98%
545
1000
STTP
Kg
56%
30
70
NaOH
Kg
96%
34
80
Bt nn
m 1%
600
Lng
thc t
Quy
trnh
Thng
lng
Th ht
s a
phi
khuy
k
20 bao
3 bao +
5kg
5 pht
ri cho
tip cc
mui
khc
12
LAS
kg
96%
176
420
Thng
lng
Th
LAS t
t(
khong
7 pht)
Silicat
kg
40%
290
670
Thng
lng
Tinopan
kg
0,3
0,68
Javen
kg
11
17
10
Tinh du
kg
11
Ht xanh
(s a)
Sau khi
ht LAS
phi
khuy
7-10
pht
mi th
tip
silicat
13
Tng kh
1000,3 2028,7 2048,97
Khi
lng kem
3047,7
Bt sn
phm:
2400 kg
Bng 2: Yu cu v cht lng kem v bt nn:

% m kem
33,4
% LAS kem
13,2
T trng kem
1,3 - 1,4 kg/lt
% LAS nn
19,7 0,2
T trng bt nn
0,40 - 0,45 kg/lt
13
2.1.1. Cht hot ng b mt LAS (Linear Alkylbenzene Sulfonate).

Cht hot ng b mt l mt cht c tc dng lm gim sc cng b mt
ca mt cht lng, L cht m phn t : mt u a nc v mt ui k nc.
Cht hot ng b mt c dng lm gim sc cng b mt ca mt cht
lng bng cch lm gim sc cng b mt ti b mt tip xc ca hai cht lng.
Nu c nhiu hn hai cht lng khng ha tan th cht. Hot ng b mt
lm tng din tch tip xc gia hai cht lng . Khi ha cht hot ha b mt
v trong mt mt cht lng th cc phn t cu cht hot ho c xu hng to
m. Nu cht lng l nc th cc phn t s chm ui k nc li vi nhau
v quay u a nc ra to nn nhng hnh dng khc nhau nh hnh cu, tr
hay mng.
Cc cht hot ng b mt l thnh phn ch yu ca mt s sn phm ty
ra. Cht hot ng b mt c dng lm gim sc cng b mt ca mt
cht lng. Nu c nhiu hn hai cht lng khng ha tan th cht hot ha b
mt lm tng din tch tip xc gia hai cht lng . Khi ha tan cht hot
dng b mt vo trong mt cht lng th cc phn t ca cht hot ng b mt
c xu hng to mixen, nng m ti cc phn t bt u to m c gi
l nng to m ti hn.
Tnh a k nc ca cht hot ng b mt c c trng bi thng s l
cn bng a k nc HLB( Hydrophilic Lipophilic Balance), gi tr ny c
gi tr t 0 n 40. HLB cng cao th cht hot ng b mt cng d tan trong
nc, HLB cng thp th cht hot ng b mt cng d tan trong cc dung mi
khng phn cc.
Cng thc cu to ca LAS:
Tnh cht LAS:

- Cht lng st, mu nu en, mi hc, tan nhiu trong nc.
14
- L mt acid mnh, n mn thit b nn thit b khuy v bn ra

phi lm bng inox.
- Lm kh da.
- D phn hy sinh hc trong iu kin hiu kh.
- Kh nng ha tan trong nc gim khi chiu di chui alkyl tng v
ty thuc vo ion dng ca mui.
- Bn trong mi trng oxy ha.
LAS l mt b mt anion vi cc phn t c trng bi mt k nc v
mt nhm a nc. LAS l hn hp phc tp ca cc ng ng ca di
chui khc nhau alkyl (C10 n C13 hoc C14) v phenyl ng phn v tr ca
phenyl-5 2 theo t l c quyt nh bi cc nguyn liu ban u v iu
kin phn ng, mi c cha mt vng thm sunfonat ha ti cc on v thuc
chui alkyl tuyn tnh bt k v tr vi cc trng hp ngoi l u cui (1phenyl). LAB nguyn liu ban u (tuyn tnh alkylbenzene) c sn xut bi
cc ankyl ha benzen vi n -parafin trong s hin din ca hydro florua (HF)
hoc clorua nhm (AlCl3) l mt cht xc tc.
2.1.2. STTP( Sodium tripolyphosphat).
Cng thc ha hc: Na5P3O10
Tn gi khc:
- Triphosphoric acid pentasodium salt;
- Pentasodium triphosphate;
- Tripolyphosphate pentasodium;
- Sodium triphosphate;
- Armofos;
- Empiphos stp-D;
- Freez-gard FP 19;
- Polygon;
- Rhodiaphos H5;
- Thermphos;
15
Tripoly.
N th bt tan d trong nc, c tnh hi kim. Va l mt cht xy

dng ng thi n cng c kh nng chng ti bm.Cc polyphosphate trong
khi hp ph vi cc ht bn, tng mt cch ng k in tch ca chng , nh
vy c s gia tng lc y gia hai ht bn.
2.1.3. Sodiumcacbonat( Na2CO3).
Natri cacbonat l mt loi mui cacbonat, c cng thc ha hc l
Na2CO3. Natri cacbonat l mt mui bn trong t nhin, thng c trong nc
khong, nc bin v mui m trong lng t. Mt s rt t tn ti dng tinh
th c ln canxi cacbonat.
Na2CO3 trong thnh phn bt git, x bng lm cht ph gia to thnh
mi trng kim, thy phn cc cht bn du m v cng l cht n lm gim
gi thnh sn phm.
2.1.4. Natri hydroxit( NaOH).
L cht rn, tinh th c mu trng, trong khng kh rt d ht m chy
ra. Xt l mt trong cc ha cht c bn nht. N c ng dng rt nhiu
trong cng ngh giy, cng ngh sn xut cht ty ra, cng ngh nhum ty
vi, cng ngh sn xut thy tinh lng...
L thnh phn khng th thiu ca bt git, n cho vo bt git trung
ha LAS, chuyn LAS v dng hot ng. thng s dng xt 30 33%.
2.1.5. Natri sunfat( Na2SO4).
L mt cht rn kt tinh mu trng ca cng thc Na2SO4 c gi l
khong sn thenardite decahydrate.
L tinh th mu trng v khi dng trong sn xut cc cht ty git phi
khng c cha cc cht c hi nh mui st, mui mangan...L cht in ly
r tin nht, n lm gim sc cng b mt ca dung dch, gim lng cht hot
ng b mt cn thit v tng kh nng ty ra ca chng. L cht n ng vai
tr lm gim sc cng b mt dung dch v l cht n gim gi thnh sn
phm.
2.1.6. Cht thm.
L mt ph gia khng ng gp g vo c ch ty git nhng khng km
phn quan trng, l nhng cht hu c thin nhin hoc tng hp c a vo
16
bt git giai on cui cng trc khi ng gi, lm sn phm c mi thm d

chu, c trng cho tng mt hng thng phm.
2.1.7. Cc loi ph gia khc.
Cht n nh bt alkylolamit: Lm tng kh nng to bt ca cht git ra,
l cht hot ng b mt loi khng sinh ion.
2.2. Quy trnh sn xut bt git.
S cng ngh sn xut bt git:
L phn
ng 1
L phn
ng 2
Xyclon
Khay
Ni
Trung gian
Qut ht
Bm
Cao p
Sng
Phn ly
Bomke
Bomke
L t
u trn
Qut y
Hnh 1: S sn xut bt git:
17
Quy trnh sn xut bt git:

- nguyn liu bao gm Na2SO4, Na3P3O10, Na2CO3, NaOH,
Na2SiO3, STPP, LAS, H2O vo thng phn ng cha cnh
khuy,thi gian thc hin phn ng l 45 pht, to kem.
- Sau , bm vo thng cha ph bng bm bnh rng, y tip
tc c gia nhit v khuy ri s dng bm pitton bm ln nh
thp to sng, cp nhit nng cho qu trnh sy. S dng qut ly
tm thi kh nng t l t du to nhit sy trong thp.
L t nhin liu hot ng :
-
Nhit 500C.
p sut du t 23 at.
Nhit du ngoi 40-50C.
p sut du ngoi 1at.
Bt c sy, a vo my trn, lc ny cng nhn s cho thm ph gia

v to mi vo my trn o ln (lm vic theo m) sau ra sn phm.
18
CHNG 3: PHN XNG CHT HOT NG B MT LAS.
3.1. Nguyn liu chnh:

Sn xut LAS i t LAB, khng kh kh tuyt i, lu hunh.
LAB:
sn xut cht ty ra mm(loi LAB) nguyn liu u thng l cc
parafin mch thng C12-C16 v benzene. Tuy nhin u tin phi x l nparafin thnh dng hot ng cho qu trnh alkyl ha. C hai phng php
thng c s dng trong cng nghip:
- Clo ha parafin s dng chng lm tc nhn cho qu trnh alkyl ha c
mt xc tc AlCl3.
- Dehydro ha c xc tc cc paraffin thnh olefin v s dng chng cho
qu trnh alkyl ha tip theo, vi s c mt ca xc tc HF.
Trong cng nghip phng php th hai c chung hn c v tnh u
vit v kinh t ca n. Ngi ta cng c th s dng dng - olefin hnh thnh
t qu trnh oligome ha etylen lm tc nhn alkyl ha nhng phng php ny
him khi c p dng trong cng nghip v gi thnh nguyn liu cao.
Trong cng ngh alkyl ha ca UOP sn xut alkylat ty ra s dng xc
tc HF c s kt hp hai qu trnh dehydro ha n-parafin v alkyl ha benzene.
Cc mono olefin hnh thnh t phn xng dehydro ha c a vo thit b
alkyl ha lp xc tc rn c nh. Cc qu trnh c s dng xc tc l HF v tin
hnh trong pha lng nhit khong 40-700oC. Cc paraffin khng tham gia
phn ng c tun hon tr li phn xng dehydro ha. Sn phm chnh ca
qu trnh alkyl ha l alkylat mch thng v mt lng nh alkylat phn t
lng ln to thnh t qu trnh alkyl ha diolefin. Loi sn phm ph ny cng
c th c thu hi v c s dng lm cc cht ty ra c bit cho cng
nghip du bi trn. Alkylat mch thng c chuyn sang phn xng sunfo
ha bng SO3 v sau khi trung ha bng NaOH sn phm thu c l
alkylbenzen sunfonat mch thng cht hot ng b mt chnh trong thnh phn
cht ty ra.
Mt s tnh cht ca lu hunh:
Tnh cht l hc:
19
Lu hunh tn ti di mt s dng th hnh khc nhau. Hai dng tinh th

thng thng nht ca lu hunh l dng t phng v dng n t. Lu hunh
t phng, cn gi l S c mu vng, nng chy 112,8oC v c t khi l
2,06. Lu hunh bn nhit thng, trn 95,5oC chuyn sang dng n t.
Lu hunh tn ti t do trong thin nhin l lu hunh t phng.
Lu hunh n t cn gi l S, c mu vng nht , nng chy 119,2oC v
c t khi l 1,96, bn trn 95,5oC, di nhit chuyn dn sang dng t
phng. Hai dng tinh th c th chuyn ha cho nhau:
S S ,
Ho = 0,401kJ/mol.
Tnh cht ha hc:

Lu hunh l nguyn t tng i hot ng, nhit thng hi km
hot ng, nhng khi un nng tng tc vi hu ht cc nguyn t tr cc kh
him, ni t, iot, vng v platin.
Khi un nng nhit 300oC th lu hunh tng tc vi hydro to
thnh hydrosunfua: S( t phng) + H2 H2S. Ho = -20,08kJ.
Phn ng xy ra km mnh lit hn so vi tng tc gia oxi v hydro.
Lu hunh tc dng vi kim loi to thnh sunfua kim loi: vi cc kim loi
kim v kim th, bc, thy ngn, phn ng xy ra nhit thp; cn vi
niken, coban, crom th nhit cao.
Vi nhng nguyn t khng kim loi hot ng, lu hunh th hin tnh
kh. Lu hunh chy c trong khng kh to nn sunfu i oxit cho ngn la
mu lam nht: S + O2 SO2 , Ho = - 297kJ.
v to nn mt t l rt b ca sunfu trioxit( SO3).
Lu hunh tc dng vi flo nhit thng , vi clo v brom khi un
nng to nn cc halogenua ca lu hunh. 100oC, lu hunh tc dng vi
photpho trng( 250oC th tc dng vi photpho ) to nn mt s sunfua nh
P4S6, P4S7, P4S10.
Phn ng to LAS:
.
R = C11C13
20
3.2. S khi.
Khng kh
Qut ht
Trao i nhit 2 tng (11E3, 11E4)
Lu hunh rn
Thp hp ph silicagen (11C1)
Thit b ha lng lu hunh (25V1)
Thp t lu hunh (12H1)
Thp chuyn ha SO2 thnh SO3 (12C1)
Trao i nhit ng chm (12E5,12E6)
Thit b lc (16F3)
Thp phn ng to LAS
Thit b lm gi
Thit b hydrat ha (16MX2)
Thit b lm lnh (16E1)
Sn phm LAS
Hnh 2: S khi xng LAS.
21
3.3. Quy trnh cng ngh.

Phn xng LAS gm 5 khu chnh:
- Phn khu 11: Khu lm kh khng kh.
- Phn khu 12: Khu sn xut SO3.
- Phn khu 14: Khu x l kh thi.
- Phn khu 16: Khu phn ng to sn phm LAS.
- Phn khu 25: Khu gia nhit lu hunh.
Quy nh cng vic sy my: trong khu chun b sn xut ca phn
xng LAS:
- Kim tra LAS, lu hunh, du DO, gas, du nhn, m, hi nc,
nc lm lnh, nc nng, xt, theo Q 02/QT 7.5.1/LAS, nu
cha t th bo co cho CNH1 np, x cc NL,NHL, VT,
BSP,SPKPH theo Q 07/QT7.5.1/LAS.
- M in vo t MCC, kim tra in th cc pha: in th pha ln
hn hoc bng 380V, in th cc pha ch c khc nhau
10V.
Nu khng t thng bo cho phn xng c in x l, khi no

t mi tin hnh sy my.
- Kim tra phn c ca 11K1, 11K2, 12K1 v 31K1.
- Bo cho CNH1 kim tra v sinh cc cc lc nc, cc ca quan
st.
- M bm 32P1( 32P2), m qut 32K1, 32K2 cp nc lm lnh.
- M bm 33P1, 33P2, cp xt, cp nc nng.
- M my nn kh iu khin 31K1, m my sy kh 31D1.
- M nc lm lnh vo 25P1, 25P2, 14P1.
- M UPS, m my tnh.
- Kim tra cc trang mn hnh my tnh.
- Kim tra v tr cc van iu khin.
22
- t TIC 11.1 v A, t S.P. = 2.

- M KU 11.1; m 11P1.
- Th bm lu hunh 25P1, 25P2.
- Th bm: 16P1, 16P2, 16P3, 16P4, 16P5.
- Kim tra mc LAB trong 16V3, nu thiu th m bm 16P5 np
thm LAB n khi c tn hiu mc.
- Xem s NKSX 01/QT 7.5.1/ LAS, xc nh tng sy ca 11C1.
- t FRC 16.3 v M; OUT = 100.
- t LIC 16.1 v M; OUT = 90.
- M bm 16P5 np LAB vo 16R1 n khi mc LAB theo P.V ca
LIC 16.1 = 60 th dng.
- M bm 16P2 cho LAB tun hon.
- Khi P.V ca TIC 11.1 5oC th:
- M bm 16P1 cho nc lm lnh vo 16R1.
- t AIC 14.1 v A; S.P = 7.
- M bm 14P1.
- M qut 14K1.
- M 11K1 nh sau:
M ht van vng ca 11K1.
M KV 16.1.
t FRC 16.2 v A; S.P = 1200.
t PIC 16.1 v A; S.P = 300.
t FRC 16.1 v M; OUT = 0.
M 11K1; ng van vng 2 rng, sau khi m 12K1 th ng thm
1 rng.
- M 12K1 nh sau:
t FRC 12.7 v A; S.P = 440.
M 12K1.
- M BK 12.1 nh sau:
23
ng van b sung khng kh vo 12H2.

M khng kh iu khin.
M gas.
ng ht l gi.
M qut 12K2.
M bm du.
M l t v ON, ch l nh la, sau 40-50 giy l phi chy.
Khi l chy m 50% l gi.
Khi nhit TR 12.13A = 100oC m ht l gi.
ng gas.
-
iu chnh van b sung khng kh gi nhit TR 12.13A
650oC.
- iu chnh van khng kh lm lnh vo 12E5, 12E6 TR 12.11
65oC, TR 12.12 55oC.
- Sy my n khi TR 12.10 210oC, TR 12.12 50oC, TR 12.4
380oC th chun b m my.
24
3.3.1. Phn khu 11: Khu lm kh khng kh.

FROM 12E2/E5
Khng kh nng
TIC 11.1
HV11.2
HV11.1A
HV11.3B
11E3
11C1
11E4
11E2
HV11.3A
HV11.5
HV11.1B
11E1
TO 12H1
KU11.1
TO16F3
11RG1
11V1
11V2
11P2
11P1
11F1
11K2
11K1
Hnh 3: S khu lm kh khng kh.

Cc thit b trong khu lm kh khng kh:
- B lc 11F1;
- My nn 11K1;
- Trao i nhit ng xon rut g 11E3 v 11E4;
- Bm 11P1, 11P2;
- Thng cha 11V2;
- Gin lm lnh KU11.1 v 11RG1;
- Thp hp ph s dng cht hp ph silicagen 11C1;
- Qut ht 11K2;
25
- Thit b 11V1 gm 2 h thng trao i nhit ng xon rut g 11E1 v

11E2;
Khng kh c ht t bn ngoi vo qua b lc 11F1, sau qua my
nn 11K1 tng p sut to iu kin thun li cho qu trnh ngng t.
Khng kh c chuyn vo bnh ngng t, bn trong c gn hai h thng
trao i nhit kiu ng xon rut g 11E3 v 11E4, trong 11E3 l thit b
trao i nhit s dng nc cn 11E4 s dng glycol. Khng kh i trong lng
cc vng ng, nc ngng c tho ra ngoi. iu khin qu trnh c phn
phi bng van 3 ng ( b phn iu khin TIC11.1) nu dung mi glycol sau khi
lm lnh cn m bo th c bm v bm 11P1 hi lu ngay, nu khng
s c bm v thng cha 11V2 trao i nhit lm lnh n nhit cn
thit nh lng mi cht lm lnh t gin lm lnh KU11.1 v 11RG1.
Khng kh sau khi c lm kh bng nc v glycol c dn sang thit
b lm kh bng vic s dng cht hp ph l silicagel.
- Silicagel thc cht l dioxxit silic, dng ht cng v xp( c v s
khoang rng li ti trong ht. Cng thc ha hc n gin l SiO2.nH2O
vi n < 2, n c sn xut t natri othosilicat( Na2SiO4) hoc silic
tetraclorua( SiCl4).
- Silicagen c pht minh ti i hc John Hopkins, Baltimore, Bang
Maryland, Hoa K trong nhng nm 1920. iu ch bng cch cho
natri silicat tc dng vi axit sunfuric:
Na2O.3SiO2 + H2SO4 3SiO2 + Na2SO4 + H2O ;
sau ra, sy kh, ri nung ta thu c silicagen. l cht rn c
l xp nh, dng cc hoc vin hnh cu ty thuc vo phng php
to ht khi iu ch, c loi trong sut nh thy tinh, c loi c.
- xp thay i trong gii hn 20-60%, ng knh l xp khong 310 nm, b mt ring 200-800 m2/g, thng l 800 m2/g. Ht silicagen
c kh nng ht nc mnh, ngoi ra vi c tnh xp cn c dng
lm cht mang xc tc, cht hp ph( pha tnh) trong phn tch sc k.
Silicagel l mt cht v c, bn, khng c, bo qun v vn chuyn
d dng,
- Silicagel l mt cht hp ph a nc n hp ph tt nc v cc cht
c cc, c bn c hc nhit cao, cc tnh cht hp ph khng
26
thay i xu khi silicagel c gia cng nhit 500oC, ngoi ra

cn c b mt ring kh ln.
Trong thp hp th 2 tng ti sinh, Silicagel c ri trn cc tm li
bn trong thit b 11C1, mi tng cao tm 1m. Khi hp ph i t trn xung (
yu cu nhit thp v p sut cao) cn khi nh hp ph th ngc li: khng
khi nng s c ly t h thng qua van HV11.2 sau qua van HV11.3A qua
qut ht 11K2 ri i vo thit b 11V1. Thit b 11V1 gm 2 h thng ng xon
rut g 11E1 v 11E2 trong 11E1 l thit b t nng cn 11E2 c nhim v
lm lnh. Khi nh hp ph th thit b t nng 11E1 hot ng v ban u cha
c kh nng t khu vc trao i nhit vo h thng nn nng dn nhit ti
135oC trong 1h sau ti 170oC( yu cu nh l nhit cao v p sut thp)
ri tin hnh nh hp ph. Sau lp Silicagel ngui dn dn ri tin hnh
lm lnh a v trng thi ch. Chu k lm vic ca h thng 2 thp l 8h.
Khng kh sau khi c hp ph hi nc t kh cn thit c
chuyn qua cc thp t 12H1 (to SO2 ) v dn i pha long SO3 trc khi cho
i vo b lc 16F3. Kh nng t cc b trao i nhit 12E2 v 12E5 c dn
qua thc hin qu trnh nh hp ph mt trong hai ngn(ngn cn li ang
thc hin qu trnh hp ph) m bo h thng lm vic lin tc.
3.3.2. Phn khu 25: Khu gia nhit lu hunh.
S khu gia nhit lu hunh:
TO 12H1
FROM TAH12.1B
25P2
25P1
25V1
25F1
25F2
Hnh 4: S khu gia nhit lu hunh.
27
Cc thit b trong khu gia nhit lu hunh:

- Thit b ha lng lu hunh 25V1;
- B lc 25F1, 25F2;
- Bm 25P1, 25P2.
Lu hunh rn c np vo ngn 1 ca thit b 25V1, thit b ny c cu
to gm 4 ngn, dc. Ti y lu hunh c ha lng khong 119C nh s
dng hi qu nhit (khong 135C) trao i nhit gin tip vi lu hunh qua
cc ng xon dn hi ngm trong b, nhit ny lu hunh nng chy c
mu vng v c nht thp nht to iu kin thun li cho vic vn chuyn
lu hunh, lu hunh lng chy trn qua ngn 2 sau qua ngn th 3, ri qua
2 b lc 25F1 v 25F2 nhm lc bt tp cht trong lu hunh, tip lu hunh
c bm vo thp chuyn ha lu hunh thnh SO2 (12H1) nh 2 bm nh
lng 25P1 v 25P2 thay nhau lm vic.Trong khu gia nhit lu hunh s dng
hi qu nhit v yu cu nhit 119oC nn s dng hi qu nhit c nhit
143oC (nh nht l 128oC). ng ng vn chuyn lu hunh l ng lng ng
m bo n nhit duy tr S trng thi lng. Bm nh lng c iu khin
nh thng s TAH12.1B u ra ca thp t lu hunh 12H1.
3.3.3. Phn khu 12: Khu sn xut SO3.
S khu sn xut SO3:
TO HV11.2
FROM 25P1/2
TO 16P3
12E2
12E3
FROM 11C1
KU12.1
12E6
12E5
12H2
12H1
12K1
TO 14C1
FROM 16F3
12V1
12C1
12P1
12P2
12V2
12K2
Hnh 5: S khu sn xut SO3.
28
Cc thit b trong khu sn xut SO3:

- Thp t lu hunh 12H1;
- Thit b gia nhit 12H2;
- Thp 12C1 l thp chuyn ha SO2 thnh SO3;
- Thit b lm ngui kiu ng xon rut g 12E2, 12E3;
- Bm 12K1, 12K2;
- Thng cha 12V1, 12V2;
- Thit b trao i nhit ng trm 12E5, 12E6
Ti thp t lu hunh(12H1) bn trong c t nhng tm li ,pha trn
tm li c lp bi s c nhim v gi lu hunh pha trn b mt bi lm tng
din tch tip xc vi khng kh c lm kh c dn i t thit b 11C1
xung di y thp v i ln, lu hunh thc c phun vo thp dng tia
v chy trn b mt bi s v thc hin phn ng chy trong khng kh y.
Phn ng c khi mo bng 1 dy mai xo t lm mi sau do phn ng t
sinh nhit nn phn ng tip tc din ra, nhit trong thp phn ng khong
620-660C. SO2 to ra c dn qua thp chuyn ha SO2 thnh SO3.
Ti thp chuyn ha SO2 thnh SO3(12C1), SO2 c dn t trn xung, do
nhit ca SO2 qu cao so vi nhit thun li cho phn ng din ra
(khong 450C) nn i hi phi lm ngui kh SO2, vic ny c thc hin
nh 3 thit b lm ngui kiu ng xon rut g 12E2, 12E3.
Khng kh c dn t bm 12K1 vo cc trong ng xon rut g ca cc
thit b 12E2 v 12E3 thc hin qu trnh trao i nhit, ring vi dng kh
vo thit b 12E2 c s khc bit cht t,khng kh c bm qua thit b 12H2
sau mi c dn vo trong cc ng rut g, khi h thng vn hnh n nh
th thit b 12H2 khng c vai tr g ngoi ng dn,nhng bn chat thit b 12H2
l thit b gia nhit s dng du t c bm t thng cha 12V1 qua bm
12K2 vo thit b vi mc ch gia nhit cho khng kh i vo 12E2 lc ban u
nhm tng nhit trong thp hot ha lp xc tc V2O5 trong thp(khi thp
vn hnh n nh thit b ny b tt). Khng kh sau khi trao i nhit c
dn qua van HV11.2 tn dng gii hp ph cho thit b lm kh khng kh.
Cu to cc tng trong thp 12C1 kh n gin, mi tng c 1 lp li
trn c 1 lp bi s sau ln 1 lp xc tc sau ri ln trn b mt 1
lp bi s ri n 1 lp xc tc, chiu cao mi tng tng t trn xung di theo
chiu cao: 0.5m; 0.8m; 1m; 1.2m. Phn ng din ra ch yu 2 tng u tin(
99%), 2 tng cui c b sung khng kh kh nhm lm ngui hn hp kh v
gim nng SO3.
29
Kh SO3 sau khi ra khi thp c nhit kh cao khong 404C do c

dn qua 2 thit b trao i nhit kiu ng chm s dng khng kh 12E5 v
12E6. Khng kh c dn t bm 12K1 i vo thit b, hn hp kh c a
t trn xung tin hnh trao i nhit. V trong hn hp kh vn cn 1 t hi
nc do trong hn hp kh c oleum cun theo, nh vic h nhit oleum
s c ngng t y thit b, sau c dn xung bnh cha 12V2. Khng
kh sau khi trao i nhit vi hn hp trn c nhit cao nn c tn dng
gii hp ph trong thit b 11C1. Hn hp kh SO3 sau khi qua 2 thit b trao i
nhit 12E5 v 12E6 c nhit khong 47C c b sung khng kh kh
nhm gim nng SO3 trnh n mn thit b trc khi c dn qua b lc
16F3 tin hnh loi b bt tp cht, phn tp cht thu c y 16F3 c
dn v bnh cha 12V2. Hn hp kh sau khi c lm sch c a vo trong
thp 16R1 to sn phm chnh LAS.
3.3.4. Phn khu 16: Khu phn ng to sn phm LAS.
S khu sunfonat ha:
16V3
KV16.1
KV16P3
16F4 A/B
HV16.4
KV16.2
16F3
TO 14F1
FROM 12E6
TO 16A1
16S1
16MX1
16P5
16V4
TO 16MX2
FROM 11C1
16AB1
16V5
M
16P3
TO 12V2
FROM 16V13
16P2
16P1
Hnh 6: S khu sunfonat ha.
30
Cc thit b trong khu sunfonat ha:

- Thp phn ng to LAS;
- B lc 16F3;
- Bnh cha 16V4, 16V5;
- Xyclon 16S1;
- Bm 16P1, 16P2, 16P3, 16P5;
- Thit b trn tnh 16MX1;
- Thit b hydrat ha 16MX2
Cu to thp phn ng gm cc u phn phi LAB vo trong cc ng,
LAB chy vng quanh pha ngoi u phn phi sau i vo cc ng, cn kh
SO3 i vo phn khng gian gia u phn phi v thi vo trong lng ng.
Thp c mt b phn bo him l bnh cha LAB 16V3 trong trng hp c s
c nh mt in lc ny bm LAB 16P3 ngng hot ng trong khi SO3 vn
tip tc chuyn vo thp trnh s tn hao nguyn liu v trnh lm hng thp
x l kh thi, van t ng KV16.3 s t ng m dn LAB vo trong thp
phn ng phn ng vi lng SO3 va a vo.
Kh SO3 sau khi qua b lc 16F3 c dn vo nh thp 16R1, LAB c
bm t bm 16P3 qua hai b lc 16F4 A/B vo thp phn ng nhit
khong 30C chy mng trong cc ng.Phn ng din ra trong lng ng.
Vic LAB chy mng trong thit b nhm mc ch tng din tch tip
xc gia SO3 v LAB nh tng tc phn ng, phn ng din ra thun
li cn duy tr nhit khong 30C. Do y thp c b phn lm lnh
bng nc h nhit hn hp ra nhm chun b iu kin thun li cho qu
trnh .
Hn hp ra trong cn c kh cun theo lng do cn chuyn qua b
phn lc tch bt gm 1 bnh cha 16V4 v xyclon 16S1 lc tch lng a
v 16V4 cn kh dn qua thit b lc 14F1 x l.
S khu hydrat ha sn phm:
31
16A1
M
FROM 16P3
16MX2
M
TO BL
FROM 16P2
16E1
16V13
16P4
TO 16P3
Hnh 7: S khu hydrat ha sn phm.

i vi hn hp trong bnh 16V4:
- Nu nng LAS to ra cha t yu cu th c chuyn qua bnh
16V5 c thit b gia nhit y nhm tng nhit hn hp nh
gim nht thun tin cho vic vn chuyn trong cc ng ng, sau
hn hp c bm 16P3 bm ln trn vi LAB (t bnh nguyn
liu) ti thit b trn tnh 16MX1 sau c a ln thp lm hn hp
u vo.
-
Nu hn hp trong bnh 16V5 t yu cu (v nng LAS v

lng d LAB) th c bm 16P2 chuyn qua thng c cnh khuy
16A1 tin hnh vi mc ch lng d LAB tip tc phn ng
tip vi lng SO3 b ln trong lng to LAS, vic khuy trn s lm
tng tc phn ng. Hn hp sau c nng LAS kh c
(khong 99%) c a sang thit b hidrat ha 16MX2, ti y hn
hp c trn thm nc (c bm t thng cha 16V13 qua bm
16P3) vo nhm lm gim nng LAS n nng cn thit. Hn
hp sau c bm 16F4 bm qua thit b trao i nhit 16E1 lm
lnh hn hp gin tip bng nc sau c vn chuyn n bnh
ng sn phm t pha ngoi xng.
3.3.5. Phn khu 14: Khu x l kh thi.

S khu x l kh thi:
32
FROM 16S1
KU14.1
14F1
FROM 12P2
14E1
14C1
14K1
14V3
14P1
Hnh 8: S khu x l kh thi.

Hn hp kh t xyclon c chuyn qua khu vc x l kh trc khi thi
ra mi trng, hn hp kh c a vo thp lc tnh in 14F1, thp cu to
gm nhng tm chn tnh in, ti y LAS b cun theo hn hp kh bm vo
cc tm chn v ri xung y thp v c tho xung thng cha 14V3,hn
hp kh lc ny ch yu l Nito v SO2 c a qua thp 14C1.
y thp 14F1 c lp mt b gia nhit nhm lm chy LAS t y thp
do LAS c tnh ht nc mnh, khi tip xc vi hi nc b vn cc ngay s
lm tc y thp.
Hn hp kh sau khi lc tnh in c a qua thp hp th SO2 14C1
hn hp kh c a t di ln, NaOH c bm ln thp nh bm 14P1 v
phun ma t trn xung nh gin phun t trn nh thp, thp hp th SO2 l
dng thp m, cc vin m hnh tr, do din tch tip xc pha ca SO2 v
NaOH l kh ln, SO2 b ko xung di dng mui sunfonat c a xung
y thp. m bo vic lc tt nht SO2 ra khi hn hp kh ta phi s dng
d xt, do c ng ng b sung xt vo y thp, ng thi oleum cng
c bm sang y thp tin hnh phn ng trung ha trc khi thi ra mi
trng. Trong trng hp s c m khng c bnh cp cu 16V3 hn hp kh i
vo khu lc c hm lng SO3 rt m c, khi i qua thp lc dng NaOH
phn ng xy ra rt mnh lit v ta nhit rt ln c th gy chy thp do
vic s dng bnh cp cu 16V3 l cn thit.
33
CHNG 4: PHN XNG AXIT PHOTPHORIC.

4.1. Tng quan l thuyt.
4.1.1. Tnh cht vt l v ha hc ca photpho:
Tnh cht vt l:
Photpho(P) c mt s dng th hnh:
- Photpho trng;
- Photpho ;
- Photpho en.
Photpho trng l khi trong sut, ging nh sp v c mng li lp
phng. Kin trc ca mng li bao gm nhng phn t P4 lin kt vi
nhau bng lc Van e Van. L cht c mng li phn t, photpho trng d
nng chy( nhit nng chy l 44oC), d bay hi (nhit si l 257oC),
mm v d tan trong cc dung mi khng cc nh CS2 v benzene. Trng thi
hi v trng thi dung dch ca trng cng gm nhng phn t P4. Phn t P4 c
cu to hnh t din u vi cc nguyn t photpho nm nh, di lin kt
P-P l 2,21ngstrm v gc PPP l 60o.
Hi ca photpho trng c mi ti x v c th chng ct 100oC cng vi
hi nc. Ngi ta li dng tnh cht ny tinh ch photpho.
700oC phn t P4 bt u phn hy thnh phn t P2 v 1700oC phn
hy khong 50%. Phn t P2 c cu to ging nh phn t phn t N2, trn
2000oC phn t P2 phn hy thnh nguyn t.
Gc PPP trong phn t P4 b hn so vi gc gia cc obitan nguyn t 3p
nn phn t P4 vo mt trng thi cng mnh v lin kt P P khng c
bn lm.
Bi vy photpho trng khng bn, di tc dng ca nh sang hoc nhit,
n chuyn dn sang mt dng bn hn l photpho . Cng v lin kt P-P trong
P4 km bn, photpho trng rt hot ng v mt ha hc. V qu trnh chuyn t
photpho trng sang photpho xy ra d dng, photpho trng thng c mu
vng nht. Qu trnh chuyn photpho trng sang photpho c th thc hin
34
trong vo chc gi nhit 250oC. Phn ng c th tng ln nhanh chng khi

c mt iot lm cht xc tc. photpho trng ht sc c.
Photpho ( hay cn gi l photpho tm) l cht bt mu . Di p sut,
n nng chy 600oC v di o sut cao hn, n thng hoa cng nhit
to thnh hi gm nhng phn t P4. Hi ny ngng t li to thnh photpho
trng. photpho l cht dng polime, gm mt s dng khc nhau m kin
trc ca chng n nay cng cha xc nh c, cho nn ty theo cch iu
ch, photpho c nhng tnh cht khc nhau, chng hn nh t khi ca chng
bin i t 2,0 n 2,4, mu sc bin i t nu n v tm.
Photpho en c to nn khi un nng photpho trng 220 n 370oC,
trong mt thi gian di( khong 8 ngy), hoc di p sut cao( 12000 atm),
hoc khi c thy ngn lm cht xc tc. Photpho en cng l cht dng polime
c mng li nguyn t. Mi nguyn t photpho lin kt vi ba nguyn t
photpho khc bao quanh bng ln kt cng ha tr vi di lien kt P P l
2,18 ngstrm. Mng li c kin trc lp hi tng t vi than ch, khong
cch gia cc lp l 3,68 ngstrm . Photpho en l cht bn dn, nng chy
gn 1000oC, di p sut 18000 atm. photpho en bn hn photpho v
photpho trng.
Khc vi photpho trng, photpho v photpho en kh nng chy v
khng tan trong dung mi no c. V photpho cng nh P en l cht
polime, khng d dng t mt phn s lin kt P-P trong tinh th to thnh
nhng lin kt mi cn thit cho qu trnh nng chy hay ha tan trong dung
mi. photpho v photpho en u khng c.
Tnh cht ha hc:
Photpho trng hot ng nht v photpho en km hot ng nht.
V d nh: iu kin thng photpho trng b oxi khng kh oxi ha dn
cho nn phi trong nc, cn photpho v photpho en u km bn.
photpho trng t bc chy trong khng kh nhit 40oC, photpho trn
250oC v photpho en trn 400oC.
Photpho va c tnh oxi ha va c tnh kh. Khi un nng photpho c th
tng tc vi nhiu kim loi to thnh photphua. Tuy nhin tnh cht c bn ca
photpho l tnh kh.
35
Khi chy trong iu kin c d kh oxi, photpho to nn oxit P4O10 v

trong iu kin khng d kh oxi to nn P406 v P4O10. Khi trng v m sinh
ra khi photpho chy trong khng kh chnh l axit metaphotphoric( HPO3) do
P4O10 kt hp vi hi nc to nn. iu kin thng, photpho trng cng b
oxi khng kh oxi ha dn dn ng thi pht ra nh sang mu lc yu nhn thy
c trong bng ti. nh sng c pht ra trong qu trnh oxi ha chm
photpho l nng lng ca phn ng ha hc. Hin tng ny c gi l s
pht quang ha hc. Chnh tn gi photpho theo ting Hy Lp c ngha l cht
mang sng. Ngoi hin tng ny, qu trnh oxi ha chm photpho cn km
theo s to thnh ozon, c th n c sinh ra trong qu trnh tring gian to nn
gc photphoyl (PO);
P + O2 PO + O;
O + O2 O3.
Hin tng pht quang ha hc cng xy ra trong mt s qu trnh ha hc
v sinh ha hc khc.
Photpho trng c th gii phng kim loi ra khi dung dch mui ca vng,
bc, ch v ng.
nhit cao, photpho c th tc dng vi hi nc to thnh H3PO4
khi c cht xc tc l Pt hay Cu:
2P + 8H2O 2H3PO4 + 5H2. Nhit khong 800oC.
Photpho c th bc chy khi va chm vi nhng cht oxi ha mnh nh
KClO3, K2Cr2O7, KNO3. Tnh cht ny a n cng dng ch yu ca photpho
l lm dim.
4.1.2. Axit photphoric.

Cng thc cu to:
36
hay ng hn gi l orthophotphoric( H3PO4). L cht dng tinh th khng mu,

nng chy 42,5oC. Trong kin trc tinh th ca n gm c nhng nhm t
din PO4 lin kt vi nhau bng lin kt hydro.
Kin trc vn cn c gi li trong dung dch m c ca axit trong
nc v lm cho dung dch snh ging nh nc ng. Axit
orthophotphoric tan trong nc l do s to thnh lin kt hidro gia nhng
phn t H3PO4 vi nhng phn t nc( H2O):
Dung dch m c ca axit H3PO4 thng bn trn th trng c nng
85%.
Khi un nng dn n 260oC, axit H3PO4 mt bt nc thnh axit iphotphoric( hay gi l axit pirophotphoric).
Axit i-photphoric l cht dng thy tinh, mm, nng chy 61oC v d
tan trong nc. Trong nc lnh n chuyn chm thnh axit H3PO4, nhng khi
un si v s c mt ca cc axit mnh th qu trnh chuyn tng ln rt
nhanh.
Khi un nng n 300oC, axit i-photphoric chuyn thnh axit metaphotpho
l cht polime c thnh phn l (HPO3)n. y cng l cht dng thy
tinh,nng chy gn 40oC. N cng tng tc rt chm vi nc chuyn
thnh axit H3PO4, qu trnh tng nhanh khi un si dung dch v s c mt
axit mnh.
Axit H3PO4 l axit ba nc v c mnh trung bnh, c cc hng s phn ly
axit l:
K1 = 7,6.10-3;
K2 = 6,2.10-8; K3 = 4,4,10-13; v to nn ba loi
mui:
Mui i.hydrophotphat: cha anion H2PO42-;
Mui monohidrophotphat: cha anion HPO22-;
Mui photphat trung ha: cha anion PO43-.
Nu dng dung dch NaOH trung ha axit H3PO4:
Nc th nht c trung ha khi cht ch th metyl da cam i mu( v
dung dch NaH2PO4 long c pH khong 4,5);
Nc th hai c trung ha khi cht ch th phenolphtalein i mu( v
dung dch Na2HPO4 long c pH xp x bng 9);
37
Nc th ba phi dng nhng cht ch th khc( v dung dch Na3PO4 long

c pH xp x bng 12).
Axit i.photphoric mnh hn axit H3PO4 v l axit bn nc, c cc hng s
phn ly axit l: K1 = 3.10-2 ; K2 = 4.10-3 ; K3 = 2.10-7 ; K4 = 5.10-10.
Tuy nhin ngi ta ch bit c hai loi mui ca axit i.photphoric l
mui i.hidrodiphotphat( cha anion H2P2O72-) v mui diphotphat trung ha.
Trong cc mui trung ha ch diphotphat ca kim loi kim mi d tan.
Axit metaphotphoric mnh hn c hai axit kia, hai dng ph bin l axit
trimetaphotphoric (HPO3)3 v axit tetrametaphotphoric (HPO3)4, c hng s
phn li hai nc cui l K3=9.10-3 v K4= 2.10-3. Trong cc metaphotphat ch
mui ca kim loi kim v magie l tan c, cc mui khc khng tan trong
nc nhng tan trong HNO3 hoc tan trong axit polimetanitric (HNO3)n nng
chy v d.
phn bit axit ortho vi cc axit i v metaphotphoric ngi ta dng
phn ng gia mui ca chng vi dung dch AgNO3: mui orthophotphat cho
kt ta Ag3PO4 mu vng cn mi diphotphat v metaphotphat cho cc kt ta
Ag4P2O7 v AgPO3 u c mu trng. Axit diphotphoric v axit metaphotphoric
khc nhau ch: axit meta lm ng long trng trng cn axit diphotpho khng
lm ng.
Axit H3PO4 rt bn: cc trng thi tan, rn v lng u khng c kh nng
oxi ha di nhit 350-400oC. Nhng nhit cao hn, chng l cht
oxi ha yu, c th tc dng vi kim loi. nhit cao, cc axiy photphoric
cn c kh nng tng tc vi thch anh v thy tinh.
Axit H3PO4 tinh khit c dng ch yu trong cng nghip dc phm.
Axit k thut c dng ch yu sn xut phn bn v c, dng trong
vic nhum vi v sn xut men s.
Axit H3PO4 c th iu ch bng tng tc ca PCl5 hay P4O10 vi nc,
hay tng tc ca P vi dung dch axit nitric c nng di 52%.
Trong cng nghip, axit H3PO4 k thut c iu ch bng cch cho axit
sunfuric c nng trung bnh tng tc vi photphoric thin nhin:
Ca3(PO4)2 + 3H2SO4 3CaSO4 + 2H3PO4.
38
Sau tch mui CaSO4 t tan ra v c c dung dch n 150oC ri lm lnh

axit kt tinh.
4.2. Phn xng sn xut axit photphoric bng phng php nhit.
4.2.1. Nguyn liu
Nguyn liu chnh l photpho trng, lu ngoi nh sng photpho chuyn
thnh mu vng v mt phn ha .
Thnh phn trong axit cng nghip ln hn 85%, lng As nh hn
0.0001%, 34C.1.688g/ml.
4.2.2. S khi.
Ha lng
photpho
Thng
cha
Thp t
Thng
trn
ng gi
Hnh 9: S khi phn xng axit photphoric.
4.2.3.S cng ngh sn xut axit photphoric bng phng php nhit.
Phn ng:
P4
+ 5 O2 P4O10
P4O10
+ H2O H2P4O11
39
H2P4O11 + H2O H4P4O12 (4HPO3)

H4P4O12 + H2O H6P4O13
H6P4O16 + H2O H5P3O10 + H2PO4
H5P3O10 + H2O H4P2O7
H4P2O7
+ H3PO4
+ H2O 2 H3PO4
S cng ngh:
106
THCV
Bm
tuye
Axit oxi
TH
Axit
oxi TH
NC
NC
xyclon
124(1)
BUNG T
124(2)
p sut: 1 at
TN
nc
nc
nc
lc
Bung hp th
Axit 75%
bm
Nc
105
Thng pht pho
Axit
TH
102
103
104
Axit
TH
Bm
125
bm
Hnh 10: S cng ngh sn xut axit photphoric bng phng php nhit.
40
- Thit b 101 : Balang, a cc thng phi ln thit b 102.

- Thit b 102: thng ha lng t 80-90C, dng hi nc duy tr nhit
.
Trong mi 102 c cha 9 phi ng photpho. Trc khi a sang thit b
tip theo phi kim tra photpho ha lng cha vi mc ch kim tra
cht lng v xem photpho ha lng hay cha.
Phng php ha lng photpho l ha lng gin tip.
Sau khi ha lng 102, ngui dung dch xung 60C, qua ng ng
xiphong xung thng cha 103.
Yu cu kim tra m vi xiphong trc khi xung 103: nhit phi
nng, nc chy u, trnh hin tng photpho keo li thnh tng cc.
Xiphong phi chu c nhit, chu p cao. Trong qu trnh cho photpho
xung thng cha lng hi nc v nhit phi m bo yu cu.
Lng photpho ha lng xung thng 103 khng qu 60 vch.
Qua van chy trn, dd t 103 xung 104 thit b nn.
- Thit b nn 104 c 2 van lp ngc nhau, m van phi trc van tri sau,
khi ng van th lm ngc li. Nn mt lng dng khng qu 60
vch.
- Thit b 105: bnh n p, l thit b b tr ln 106.
Thit b bm cp nc, mun nn p sut cn bt bm cp cho 106
(thng cao v).
p sut lm vic : 3at, m van iu p, ng van x p, van x kh m,
khi nn p sut cn ng van x kh.
Bm tuye nn kh kiu phun ti v bm gi vo, lm vic p sut chn
khng.
Thit b trao i nhit kiu ng chm.
X l nc dn in < 60 bng cch sc H2S + H3PO4 kt ta
asen, lc b kt ta As2S3, PbS c axit thc phm.
41
- Trong thit b phn ng:

Photpho lng c bm vo bung t v t bc chy (do photpho t bc
chy 44oC ) v do phot pho bc chy u v chy hon ton th ta
phi cung cp thm oxi vo trong bung t trong n t c p sut l :
1 at, v nhit trong l t rt cao ln n 700 800oC khi photpho
chy to thnh P4O10 sau do P4O10 dng m khan cho ln ta cn
phi cung cp axit tun hon i t trn xung thnh l. Do trong l t
nhit cao 700-800oC nn nc trong axit tun hon bay hi v cc
P4O10 hp th hi nc v to thnh H3PO4 ngoi ra cn to ra nhiu loi
axit khc nhng ch yu l H3PO4 v vi p xut bn trong l 1 at nn
H3PO4 l dung dch v dung dch H3PO4 b ht ra ngoi a qua thit b
trao i nhit gim nhit xung (< 70oC) bo v thit b ko b n
mn.
Bn ngoi l t photpho c bm nc bo v thit b v lm gim
nhit ca xng dch qua thit b trao i nhit mt phn dung dch
a sang thit b khuy trn 124, phn cn li vn cha ha lng ht
c bm tuye ht v a qua xiclon tch lng kh. Kh thi c a
ln trn cn lng a xung di v a sang 124 y dung dich c
khuy trn to axit t yu cu axit H3PO4 y c nng 83% v
c lc v a vo thng cha 125.
42
CHNG 5: PHNG KIM TRA CHT LNG SN PHM.

5.1. Axit phosphoric k thut: TC 02:2005/HCG.
5.1.1.Yu cu k thut:
- Yu cu v nguyn liu chnh: pht pho vng: hm lng P4 tnh bng
phn trm khng nh hn 99,9.
- Yu cu i vi sn phm:Sn phm Axit photosphoric k thut c cc
ch tiu v mc cht lng theo quy nh ti bng di y:
Bng 3: Cc ch tiu v mc cht lng ca sn phm axit photphoric.
Mc cht lng
Tn ch tiu
1. Ngoi quan
Dung dch c mu
vng
2. Hm lng axit phtphoric (H3PO4) tnh

bng phn trm, khng nh hn
85
3. Hm lng Clo (Cl) tnh bng phn

trm, khng ln hn
0,0005
4. Hm lng SO4, tnh bng phn trm,

khng ln hn
0,005
5. Hm lng st (Fe)
trm, khng ln hn
tnh bng phn
0,005
6. Hm lng kim loi nng quy ra ch

(Pb), tnh bng phn trm, khng ln
hn
0, 05
7. Hm lng asen (As) tnh bng phn

trm, khng ln hn
0,01
8. Khi lng ng gi , tnh bng kg
35
43
5.1.2. Xc nh hm lng axit photphoric.

Phng php A( Phng php trng ti).
Thuc th, dung dch, thit b.
- NaOH 0,1N.
- My o pH.
- My khuy t.
Cch tin hnh.
- Cn khong 2,5g mu( khong 1,5ml) . Trong cc cn m c np cha 5
ml nc chnh xc n 0,0001g, chuyn vo bnh nh mc dung tch 250
ml. thm nc n vch mc lc u.
- Dng pipet ly 25ml dung dch nh mc, cho vo cc dung tch
200ml, cho que khuy t vo thm 75ml nc v t ln my khuy t.
- Cho in cc vo dung dch, bt my khuy t v chun bng dung
dch NaOH n pH bng 4,6.
Tnh kt qu.
Hm lng axit phosphoric H3PO4 tnh bng phn trm, tnh theo cng thc:
% H3PO4 =
trong :
V l th tch dung dch NaOH 0,1N tiu tn chun , ml
m l lng mu chun , g
0,009799 l lng H3PO4 tng ng vi 1ml dung dch NaOH 0,1N, g.
Phng php B.
Thuc th v dung dch.
- Dung dch NaOH 0,5N
- Dung dch bo ha NaCl , chun b nh sau: ha tan 400g NaOH trong
1000ml nc, yn trong 24 gi, khuy u, lc ly dung dch trong.
- phenolphthalein, dung dch 1% pha trong etanol 95%.
44
Cch tin hnh.

Cn khong 1g mu trong cc m cha 5ml nc, chnh xc n 0,0001g ,
ha tan bng 10ml nc, thm 30ml dung dch bo ha NaCl v chun bng
NaOH 0,5N cho ti khi xut hin mu hng( ch th phenolphthalein).
Tnh kt qu.
Hm lng axit photphoric H3PO4 tnh bng phn trm, theo cng thc:
% H3PO4 =
trong :
m l lng mu ly chun , g.
V l th tch dung dch NaOH 0,5N tiu tn chun , ml.
0,0244975 l lng H3PO4 tng ng vi 1ml dung dch NaOH 0,5N, g.
5.1.3. Ghi nhn, vn chuyn, bo qun, bao gi.
Ghi nhn:
-
Tn c s a ch.
Tn sn phm.
- Cng dng.
- Cch dng.
- Thnh phn.
- Cc ch tiu, mc cht lng chnh.
- Khi lng tnh.
- Sn xut theo tiu chun TC 02:2001/HCG.
- Ngy thng nm sn xut.
- Thi hn s dng.
-
Bao gi.
Axit photphoric k thut c cha trong can nha chuyn dng c hai ln
nt. Bn ngoi can c gn nhn ph hp vi iu 3.1 ca tiu chun ny. Cc
can nha cha axit photphoric k thut phi chc chn, kh sch c nt vn kn,
m bo khng nh hng n cht lng axit.
45
Vn chuyn: Axit photphoric k thut c vn chuyn trn cc phng

tin giao thng nh t, tu ha,..
Bo qun: Cc can cha axit photphoric k thut c bo qun ni
kh mt. Axit photphoric k thut trong kho: cho php xp hai lp
chng ln nhau
5.2. Xc nh hm lng clo.
5.2.1. Thuc th v dung dch.
- Dung dch axit HNO3 25%.
- Dung dch AgNO3 0,1N.
- Dung dch clo chun cha 0,01ml Cl/ml, chun b theo tiu chun TCVN
1056-86.
5.2.2. Cch tin hnh.
- Cn 5g mu( khong 3ml) chnh xc n 0,01g, thm10 ml nc chuyn
dung dch vo ng so mu.
- Thm 1ml axit HNO3, 1ml AgNO3, lc u.
- Mu t tiu chun nu sau 10 pht dung dch mu khng c hn dung
dch chun c chun b dng thi vi dung dch mu, cha trong th
tch 1ml HNO3, 1ml AgNO3, v 0,025 mg Cl.
5.3. Xc nh hm lng sunfat.
- Bariclorua( BaCl2) c h tinh bt chun b nh sau: ha tan 20g BaCl2
trong 90 ml nc, nu dung dch c th lc qua giy lc khng tn, thm
2.5 axit clohidric m c 35-38 %, un si dung dch, thm vo dung
dch cn nng( va thm va khuy u), 0,25g h tinh bt.
- Dung dch sunfat chun cha 0,01mg SO4/ml, chun theo TCVN 105686.
5.3.2. Tin hnh th.
- Cho 2g mu( khong 1,2ml) chnh xc n 0,01g , thm 10ml nc,
chuyn dung dch vo ng so mu, thm 2ml BaCl2, lc u.
- Mu t tiu chun nu sau 30 pht dung dch mu khng c hn dung
dch chun c chun b ng thi vi dung dch mu v cha trong
cng mt th tch 2ml BaCl2, 0,1mg SO4.
46
5.4. Xc nh hm lng st.

- Axit sunfosalisilic , dung dch 5%.
- nc ammoniac 25%.
- dung dch chun cha 0,01mg Fe/ml, chun b theo tiu chun TCVN
1056-86.
5.4.2. Cch tin hnh.
- Cn 1g mu (khong 0,6 ml) chnh xc n 0,01g, thm 10 ml nc,
chuyn dung dch vo ng so mu, thm 2ml axit sunfisalisilic, 5 ml nc
ammoniac lc u.
- Mu t tiu chun nu sau 15 pht mu vng ca dung dch mu khng
m hn mu vng ca dung dch c chun b ng thi vi dung dch
mu cha trong cng th tch 0,05mg Fe, 2ml axit sunfosalisilic v 5 ml
nc ammoniac.
5.5. Xc nh hm lng kim loi nng.
- Natri hidroxit, dung dch 10%.
- Giy cng g chun b nh sau: ha tan 0,1g cng g trong 20ml
cn 96%, thm nc n 100ml. Tm dung dch ch th vo giy lc
trng v kh trong khng kh ch ti khng c hi ammoniac.
- thioaxetamit, dung dch 2%.
- dung dch ch chun cha 0,01mg Pb/ml, chun b theo tiu chun TCVN
1056-86.
5.5.2. Cch tin hnh.
- Cn 1g mu ( khong 0,6ml) chnh xc n 0,01g, thm 10ml nc,
chuyn dung dch vo ng so mu, trung ha bng dung dch NaOH n
lc giy cng g chuyn t mu xanh sang mu , thm 2ml kali
natritarat, 2ml NaOH, 2ml thioaxetamit, lc u.
- Mu t tiu chun nu sau 10 pht, mu ti ca dung dch mu khn g
m hn mu ti ca dung dch chun c chun b ng thi vi dung
dch mu v cha trong cng th tch lng dung dch NaOH , 2ml kali
natri tatrat, 2ml thioaxetamit v 0,5mg Pb.
47
5.6. Xc nh hm lng NO3 trong axit.

- H2SO4 98%, 16%;
- HCl 37%;
- NaCl 5%;
- Dung dch cha NO3 chun b nh sau: ha tan 1,630g KNO3 sy n
khi lng khng i 100-105 oC vo nc , thm nc n 1l. 1ml
dung dch c 1mg NO3. Khi cn, dng nc pha long dung dch
- Indigocacmin chun b nh sau: ha tan 0,2g Indigocacmin vo 500 ml
dung dch H2SO4 16% trong bnh 1l.
Thm 20ml HCl m c v thm H2SO4 16% n vch mc.Dung dch
Indigo cac min khng bn, mun bit dung dch cn tt hay khng th c
14 ngy kim tra li 1 ln.
5.6.2. Cch kim tra.
- Cho vo 2 cc 50ml ln lt 0,03 v 0,035mg NO3.
- Thm nc vo dung dch l 10ml. trong khi khuy thm 1ml dung
dch NaCl, 1 ml Indigo cac min , 12m l H2SO4 m c v yn
trong 5 pht..
- Dung dch cha 0,03mg NO3 phi m c hn dung dch cha
0,035mg NO3.
5.6.3. Tin hnh th.
- Cn 2g mu( khong 1,2ml mu) vo cc 50ml. Thm 6ml nc
khuy u. Thm 1ml NaCl 5%, 1ml Indigo v 12ml H2SO4 m c.
- Mu t tiu chun nu sau 5 pht mu cu dung dch khng nht hn
mu ca dung dch tiu chun c chun b ng thi vi dung dch
mu v cng cha trong cng mt th tch.
5.7. Kim tra cht lng bn sn phm xc nh ch s axit tng (AV).
5.7.1.nh ngha:
Ch s axit tng (AV) c th hin bng s mg KOH dng trung ha
1 gam LAS( c ha tan trong cn trung tnh) theo ch th
phenolphtalein.
5.7.2.Ha cht v dng c.
- Cn 95% trung tnh.
- Dung dch KOH hoc NaOH 0,1N.
48
Phenolphtalein dung dch 1% trong cn 95%.

Cc thy tinh 100ml.
Cn phn tch.
My khuy t.
Buret 50ml.
5.7.3.Ni dung quy nh.

- Khi n gi ly mu( t 1 n 2 gi ly mu 1 ln) n 16R1,
16MX2, x khong 0,5 kg BSP qua van ly mu, sau ly khong
10 g mu.
- Cn chnh xc khong 0,5g mu vo cc thy tinh, ghi s gam mu
cn l G, thm vo 50 ml cn trung tnh, cho con t vo cc, cho 5
git phenolphthalein vo cc. t cc ln my khuy t, bt my
khuy t cho mu tan ht. Khi mu tan ht, chun mu bng dung
dch NaOH 0,1N n khi xut hin mu hng. Ghi s ml dung dch
NaOH 0,1N dng chun l V.
- Tnh kt qu:
Ch s axit tng c tnh theo cng thc:
AV =
, mg KOH/ 1g LAS
trong :
V l s ml dung dch NaOH 0,1N dng chun.
C l nng dung dch NaOH 0,1N.
G l s gam mu cn chun.
56,1: 1mg ng lng KOH l 56,1mg KOH.
C th tnh theo cng thc rt gn:
AV =
, mg KOH/ 1g LAS
trong :
V l s ml dung dch NaOH 0,1N dng chun.
F l h s tnh sn = C . 56,1 l s thay i theo nng dung dch
NaOH chun.
49
- Ch s axit tng nm trong khong 175 n 188 l t yu cu.

5.8.Kim tra cht lng LAS.
5.8.1. Yu cu k thut:
Cht hot ng b mt LAS phi ph hp vi qui nh trong bng 1 v
bng 2.
Bng 4: Cc ch tiu ngoi quan.
Tn ch tiu
Yu cu
Lng st, ng nht
1. Trng thi
2. Mu
Nu sng
Bng 5: Cc ch tiu ha l.
Tn ch tiu
Mc cht lng
1. Hm lng LAS, tnh bng phn trm khi

lng, khng nh hn
95,5
2. Khi lng phn t trung bnh, tnh bng gam

3. Hm lng H2SO4, tnh bng phn trm khi
lng, khng ln hn
322 324
1,5
1,0
4. Hm lng nc, tnh bng phn trm khi

lng, khng ln hn
2,0
5. Hm lng du t do, tnh bng phn trm

khi lng, khng ln hn
185 188
70
6. Ch s axit, tnh bng mg KOH

7. mu, tnh theo Klett, khng ln hn
5.8.2. Phng php th:
Quy nh chung:
- Ha cht dng phn tch l loi TKPT;
- Nc phn tch s dng theo TCVN 4851-89.
50
Ly mu v chun b mu:
- Ly mu v chun b mu theo TCVN 5454-1999 v TCVN 5491-1991
vi lng mu trung bnh ti thiu l 300g.
- Mu th nghim c cho vo bnh sch, kh v c nt mi hoc l c
nt kn, ngoi l c ghi nhn:
Tn sn phm;
Tn ni sn xut;
Ngy sn xut;
Ngy v ni ly mu;
K hiu tiu chun.
nh gi ngoi quan sn phm
- Ly khong 50 g mu vo cc thy tinh dung tch 100 ml. Dng mt
quan st mu, cn tin hnh ni sch s, nh sng, khng chiu trc
tip, khng c vt g mu sc sc s v khng c mi l.
- nh gi mu th theo cc yu cu qui nh bng 1.
Xc nh hm lng LAS
- Bng phng php chun hai pha trc tip theo TCVN 5455-1998 v
xc nh khi lng phn t trung bnh bng sc k kh lng theo TCVN
6335-1998.
5.9.Xc nh hm lng H2SO4.
5.9.1. Nguyn tc:
- Hm lng H2SO4 (l lng H2SO4 khng c sunfonic ha) ca mu
c xc nh bng phng php chun vi dung dch tiu chun ch
theo ch th dithizon, trong mi trng m axeton c pH = 4 0,2. Ti
im tng ng mu xanh l cy ca dung dch chuyn sang mu
gch.
5.9.2. Ha cht v thuc th:
-
Axeton 99%;
Etanol 95%;
Axit nitric, dung dch 1N;
Amoni hidroxit, dung dch 10%;
Natri hidroxit, dung dch 40 g/lit v 1 N;
Dithizon, dung dch 0,5 g/lit trong axeton, bo qun trong chai nu
v bn trong 1 tun;
Amoni dicloaxetat, dung dch m pH 1,5 1,6;
51
Ha tan 110 ml axit dicloaxetic trong 500 ml H2O. Trung ha dung

dch ny bng amoni hidroxit theo giy o pH n pH khong 7
ngui, thm tip 55 ml axit dicloaxetic. Thm nc n 1000 ml.
(Dung dch m ny trong mi trng axeton 70-85% (V/V) c gi
tr pH = 4,1 = 0,2);
Dung dch chun ch 0,01 M Ha tan 3,35 g Pb (NO3)2 trong
1000 ml H2O. Xc nh li nng dung dch ch bng phng
php chun o complexon III theo TCVN 1272 86.
5.9.3. Thit b v dng c:

-
Cc, dung tch 250 ml;

Burret 25 ml, phn vch 0,1 ml;
Bnh tam gic, dung tch 250 ml;
Bnh nh mc, dung tch 100 ml, 1000 ml;
My khuy t, tc 150 300 vng/pht v que khuy;
Cn phn tch c chnh xc 0,001 g.
5.9.4. Cch tin hnh:

- Cn khong 3 g mu (chnh xc n 0,001 g) vo cc 250 ml, ha tan
mu bng 10 ml etanol. Trung ha mu bng dung dch NaOH 1 N theo
ch th phenolphtalein, pha long bng nc, nh mc ti vch 100 ml,
lc k. Ht 10 ml dung dch trn vo bnh tam gic 250 ml, thm vo
75 ml axeton v 1 ml ch th dithizon. Thm ba git axit nitric 1 N v 2
ml dung dch m amoni dicloaxetat.
- Chun mu trn my khuy t bng dung dch ch vi tc 1 git
trn 1 giy cho n khi mu ca dung dch chuyn t xanh l cy sang
gch, bn trong 15 giy. Th tch dung dch ch tiu tn chun l V
ml.
5.9.5.Tnh kt qu.
- Hm lng axit sunfuric tnh bng phn trm khi lng, theo cng thc:
% H2SO4 =
V C 98,08 100
m 1000
trong :
V l th tch dung dch ch tiu tn chun , tnh bng mililit;
C l nng dung dch ch, tnh bng mol;
52
m l khi lng mu ly chun , tnh bng gam;

98,08 l khi lng phn t H2SO4, tnh bng gam.
5.10. Xc nh hm lng nc bng phng php Karl Fisher:
5.10.1. Phm vi p dng:
- Phng php ny p dng xc nh hm lng nc khng ln hn
1% trong cht hot ng b mt LAS.
5.10.2. nh ngha hm lng nc.
- Hm lng nc bao gm nc t do, nc kt tinh, nc hp th v
nc trong sn phm.
5.10.3. Nguyn tc.
- Thuc th Karl Fisher c mu nu, khi kt hp vi nc trong mu th
n tr thnh khng mu. Dung dch thuc th ny c chun ha trc
bng cch chun vi mt khi lng nc chnh xc bit trc.
Hm lng nc c tnh l % khi lng t lng thuc th dng.
5.10.4. Ha cht v thuc th.
- Metanol, hm lng nc nh hn 0,005% (m/m);
- Thuc th Karl Fisher, tt nht mua sn trn th trng hoc iu ch
theo ph lc A.1.
5.10.5. Thit b v dng c.
- Thit b Karl Fisher t ng hoc bn t ng theo ph lc A.2;
- Bnh chun c in cc bch kim kp hoc bnh thng, dung tch 100
ml;
- Buret t ng hoc bnh thng, 25 ml c phn vch 0,1 ml;
- Bnh lm kh c cha silicagel hot tnh, hoc clorua canxi, dung tch
500 ml;
- Bnh cha dung dch chun , dung tch 1 lt;
- Thit b khuy t, tc 150 300 vng/pht;
- Bm tim microlit, dung tch 100 l;
- Bm tim thy tinh, dung tch 20 ml c ng knh t 2 mm n 4 mm
c th gn thay i cc kim khc nhau.
53
5.10.6. Cch tin hnh.

m ca mi trng l nguyn nhn sai s ln nht trong phng php
chun Karl Fisher. c bit phi ch lm kh ton b cc thit b
c s dng v thao tc nhanh vi cc dung mi v mu th.
Xc nh hm lng nc tng ng trong dung dch Karl Fisher
- Phi xc nh hm lng nc tng ng trong mi bnh dung dch
thuc th Karl Fisher v phi kim tra li trc khi s dng.
- a 20 ml metanol vo bnh chun ca thit b Karl Fisher (Ph lc
A.2) bng bm tim 20ml, bt my khuy t ri chun vi dung dch
thuc th Karl Fisher, khng ghi th tch tiu tn ln chun ny.
- a chnh xc 40 l nc ct t bm tim microlit tng ng 40 mg
H2O, (m1) vo bnh chun ca thit b Karl Fischer.
Chun bng phng php o in (khi thit b c b in cc bch
kim ghp)
- iu chnh cc in cc sao cho chng c nhng ngp di b mt 2
mm 3 mm.
- Chun dung dch bng thuc th Karl Fisher cho n khi t im
tng ng, lc kim in k trn my o in gi khng i trong 30
giy sau khi thm thuc th.
Chun bng phng php thay i mu ti im tng ng. (Khi
thit b khng c b in cc bch kim ghp).
- Chun dung dch bng thuc th Karl Fisher cho n khi t im
tng ng dung dch khng mu tr thnh mu nu.
- Th tch tiu tn chun ny l V1 ml.
- Hm lng nc tng ng trong 1 ml thuc th Karl Fisher (H2O),
tnh bng miligam trn mililit, theo cng thc:
(H2O) =
m1
V1
trong :
m1 l khi lng nc a ra vo chun , tnh bng miligam;
V1 l th tch thuc th Karl Fisher dng trong chun , tnh bng
mililit.
Chun b mu th
54
- Nu mu c hm lng nc nh hn 1% (m/m) th cn 5 g n 10 g, nu
mu c hm lng nc ln hn 1% (m/m) th cn 1 g n 5 g (chnh xc
n 0,001 g) (phn mu xc nh c khong 10 mg n 50 mg nc l
tt nht).
Xc nh hm lng nc trong mu
- a 20 ml metanol vo bnh chun ca thit b Karl Fischer, bt my
khuy t ri chun bng thuc th Karl Fisher nh (4.6.6.1.1) hay nh
(4.6.6.1.2) n im tng ng, khng ghi th tch ln chun ny.
- a mu th (4.6.6.2) vo bnh chun v khuy k cho tan mu, ri
chun n im tng ng. Th tch dung dch Karl Fisher chun
ln ny tiu tn l V ml.
- Thc hin php xc nh ln th hai bng cch cho tip lng mu th
nh trn v lp li s chun .
5.10.7. Tnh kt qu:
- Hm lng nc trong mu (H2O), c tnh bng phn trm, theo cng
thc:
% H2O =
( H 2 O) V 100
m
trong :
V l th tch thuc th karl fisher dng chun mu, tnh bng mililit;
m l khi lng ca mu a vo chun , tnh bng miligam.
5.11. Xc nh hm lng du t do.
5.11.1. Nguyn tc:
- Hm lng du t do (l cc cht hu c khng c sunfonic ha) ca
mu c ha tan trong etanol, sau chit vi ete du ha v xc nh
bng phng php khi lng.
-
Ete du ha;
Etanol, 95% v (1:1);
Phenolphtalein, dung dch 10 g/lit pha trong etanol 95%;
Natri hidroxit, dung dch 0,5 N;
Natri sunfat, khan.
55
5.11.3. Dng c:
-
Phu chit, dung tch 250 ml;

Cc, dung tch 250 ml;
Bnh tam gic, dung tch 250 ml;
T sy, duy tr nhit 105 oC.
Cn phn tch c chnh xc 0,01 g.
5.11.4. Cch tin hnh.

- Cn khong 10 g mu (chnh xc n 0,01 g) vo cc 250 ml, ha tan
trong 100 ml etanol (1:1).
- Chuyn dung dch mu v trng cc nhiu ln bng lng nh tng cng
khong 50 ml etanol (1:1) vo phu chit th nht. Thm vi git
phenolphtalein v trung ha bng NaOH 0,5 N n mu hng.
- Cho vo phu 50 ml ete du ha, y nt v lc mnh trong 1 pht,
yn mu n khi phn thnh hai pha, chuyn pha etanol di sang phu
chit th hai. Lc pha ete du ha qua phu c sn khong 3 g natri
sunfat khan vo bnh tam gic 250 ml c sy kh v cn trc n
khi lng khng i m0.
- Lp li qu trnh chit ny hai ln na trong phu chit th hai, mi ln
dng 50 ml ete du ha. Thu gp tt c pha ete du ha vo bnh tam gic
trn.
- C nh bnh tam gic ny trn bp cch thy n kh, sau cho bnh
vo t sy nhit 1050C trong 15 pht. ngui bnh trong bnh ht
m, sau 30 pht em cn l gi tr m1.
- Lp li qu trnh sy ny n khi chnh lch gia hai ln cn lin tip
khng ln hn 0,1%.
5.11.5. Tnh kt qu:
- Hm lng du t do (D), tnh bng phn trm khi lng, theo cng
thc sau:
D=
(m1 m0 ) 100
m
trong :
(m1 m0) l khi lng ca cn trong bnh, tnh bng gam;
m l khi lng ca phn mu th, tnh bng gam.
56
5.12. Ch s axit.
5.12.1. nh ngha ch s axit:
- Ch s axit c th hin bng n v mg KOH, dng trung ha 1 g
sn phm trong etanol theo ch th phenolphtalein.
- Etanol 95 %, dung dch trung tnh;
- un hi lu cc dung dch ny trong 5 pht loi CO2. ngui n
nhit phng v trung ha bng dung dch KOH 0,1 N theo ch th
phenolphtalein n bt u chuyn sang hng;
- Kali hidroxit, dung dch tiu chun 0,5 N, xc nh li nng trc khi
dng v 0,1 N;
- Phenolphtalein, dung dch 10 g/lt pha trong etanol 95 %.
5.12.3. Dng c:
- Bnh tam gic, dung tch 250 ml;
- Buret, dung tch 25 ml, phn vch 0,1 ml.
- Cn phn tch c chnh xc 0,001 g.
5.12.4. Cch tin hnh:
- Cn khong 2 g mu (chnh xc n 0,001 g) vo bnh tam gic 250 ml,
cho vo 100 ml etanol, lc cho tan mu hon ton ri thm 4 n 5 git
dung dch phenolphtalein.
- Dng buret 25 ml cha dung dch KOH 0,5 N chun n xut hin
mu hng.
5.12.5. Tnh kt qu:
- Ch s axit (T) l s miligam KOH dng trung ha 1 gam sn phm,
c tnh theo cng thc sau:
T=
V C 56,1
m
trong :
V l th tch ca dung dch tiu tn khi chun KOH, tnh bng mililit;
C l nng chnh xc ca dung dch chun KOH, tnh bng nng N;
m l khi lng mu th, tnh bng gam;
57
56,1 l khi lng phn t KOH, tnh bng gam.

5.13. Xc nh mu.
5.13.1. Nguyn tc:
- mu Klett (M) l s o s hp th dung dch mu th 5% trong etanol
bc sng = 420nm v cuvet 40 mm, bng my o mu Klett
Summerson.
- Etanol 95%.
5.13.3. Dng c:
- My o mu Klett Summerson, knh lc s 42, c thang n v Klett;
- Cuvet thch anh, I = 40 mm;
- Cc thy tinh, dung tch 250 ml.
5.13.4. Cch tin hnh:
- Cn khong 5 g mu (chnh xc n 0,01 g) vo cc 250 ml, sau thm
etanol sao cho khi lng ton dung dch l 100 g. Khuy k dung dch
tan mu hon ton.
- iu chnh my o mu n im khng bng etanol.
- o dung dch mu th trong cuvet 40 mm knh lc s 42.
- Ghi gi tr mu M theo n v Klett trn my.
58
KT LUN
Cng ty c phn Ha Cht v Bt Git c Giang l mt cng ty c

truyn thng v b dy trong lnh vc sn xut cc sn phm ha hcv ang
ngy cng pht trin vi nhng d n ang c xy dng trong tng lai.
Khng nhng vy, vi i ng cn b v cng nhn vi tc phong lm vic linh
hot, cng nghip gip em rt nhiu trong vic tm hiu c ch cch thc
hot ng ca nh my. V vy y l n v thch hp sinh vin nm bn
nh chng em c c hi thc tp.
Bi bo co trn l kt qu m em thu thp c sau thi gian thc tp
k thut ti Cng ty CP Bt git & Ha cht c Giang v cng l nhng kim
thc m em tch ly trong ba nm hc i hc. Cng trong thi gian ny em
tn dng c c hi tip cn c vi thc t sn xut, khng kh, tinh
thn lm vic sau ny khng b b ng khi ra cng tc, v em ngh y cng
chnh l mc ch ln nht khi cc thy c a chng em n cng ty thc tp.
59
TI LIU THAM KHO

[1] Phm Thanh Huyn, Nguyn Hng Lin, Cng ngh tng hp hu c- ha
du, Nh xut bn Khoa hc v K thut, 2006.
[2] GS.TS. o Vn Tng, ng hc xc tc, Nh xut bn Khoa hc v K
thut, 2006.
[3] http://www.ducgiangchem.vn
[4] Ti liu sn xut ca Cng ty c phn Bt git v Ha cht c Giang.
[5] Hong Nhm, Ha hc v c, Tp 2, Nh xut bn Gio dc, 2006.
[6] Nguyn Hu Ph, Ha l v Ha keo, Nh xut bn Khoa hc v K thut,
2006.
[7]http://www.hoahocngaynay.com/en/hoa-hoc-va-doi-song/hoa-hoc-daukhi/611-silica-gel-va-cong-dung.html
60

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BO CO THC TP TT NGHIP

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

DANH MC CC BNG V HNH V

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

CHNG 1: GII THIU V CNG TY C PHN BT GIT

1.1.Gii thiu chung.

: Cng ty c phn Bt git v Ho cht

: Ducgiang Chemicals & Detergent

: 18/44 ph c Giang, phng

: (04) 8 271 620

: (04) 8 271 068

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

: 002 - 107068 - 001 Ngn hng Hng

Ngnh ngh ng k kinh doanh:

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

- Ban kim sot:

ng Nguyn Tin Khang

1.2. Qu trnh pht trin ca cng ty:

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

Cc gii thng cng ty t c:

- Axit photphoric cng nghip 70%.

Photpho c ha lng bng hi nc, sau cho vo thp t, va t va

Cht hot ng b mt LASNa c chia thnh 2 phn: phn a nc l

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

CHNG 2: PHN XNG BT GIT.

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

1000,3 2028,7 2048,97

Bng 2: Yu cu v cht lng kem v bt nn:

1,3 - 1,4 kg/lt

0,40 - 0,45 kg/lt

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

2.1.1. Cht hot ng b mt LAS (Linear Alkylbenzene Sulfonate).

Tnh cht LAS:

- L mt acid mnh, n mn thit b nn thit b khuy v bn ra

N th bt tan d trong nc, c tnh hi kim. Va l mt cht xy

bt git giai on cui cng trc khi ng gi, lm sn phm c mi thm d

Hnh 1: S sn xut bt git:

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

Quy trnh sn xut bt git:

Bt c sy, a vo my trn, lc ny cng nhn s cho thm ph gia

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

CHNG 3: PHN XNG CHT HOT NG B MT LAS.

3.1. Nguyn liu chnh:

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

Lu hunh tn ti di mt s dng th hnh khc nhau. Hai dng tinh th

Tnh cht ha hc:

SVTH: NGUYN THNH CHUNG 20109705 CN HA DU

Trao i nhit 2 tng (11E3, 11E4)

Thp hp ph silicagen (11C1)

Thit b ha lng lu hunh (25V1)

Thp t lu hunh (12H1)

Thp chuyn ha SO2 thnh SO3 (12C1)

Trao i nhit ng chm (12E5,12E6)

Thp phn ng to LAS

Thit b hydrat ha (16MX2)

Thit b lm lnh (16E1)

Hnh 2: S khi xng LAS.

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3.3. Quy trnh cng ngh.

Nu khng t thng bo cho phn xng c in x l, khi no

- t TIC 11.1 v A, t S.P. = 2.