DAI HOC QUOC GIA HA NOl
TRUONG
DAI
HOC
KHOA
HOC
TL/NHIEN
BAG CAO KET QUA DE TAI NCKH
'^fiH
(te tai:
NGmEN CUU QUA TRINH DIEU
CHE
BpT
MAU
LITHOPON
Tl/CAC
NGUON QUANG
KEM VA BARITIN VIET NAM
CHU TRI DE TAI: PGS. TS. TRINH NGOC CHAU
DA! HOC QUOC GIA HA
MOi i
•p:jNG
TA?/
Ti-iOV-':^
TiM THij
ViR:
•
DT/5/iO
HA NOI, 2004
L BAO CAO TOM TAT
a. Ten de tai: Nghien ctru qua trinh che tao
baritin
ciia
Viet nam. Day la sac to mau trang dugc
sir
dung nhieu trong cong
nghiep son, cao su ma hien nay chiing ta van phai nhap ngoai .
-
Npi
dung:
- Xac dinh thanh phan
ciia
cac loai quang ban dau.
- Khao sat cac yeu to anh
hucmg
den qua trinh chuyen hoa
BaS04
trong quang baritin Ha Bac thanh BaS.
- Nghien
ciru
quy trinh thfch hgp de' dieu che dung dich
ZnS04
sach
tir
kem oxit Tuyen Quang
-Tim
dieu kien toi uu cho phan ung dong ket tua lithopon tu hai dung
dich BaS va
ZnSO^
a
tren.
- Da nghien cuu anh huong cua ti le so
moi
BaS :
ZnS04
va pH den qua
trinh dong ket tua de thu dugc bot mau lithopon.
- Da xac dinh thanh phan va mot so tfnh chat
ciia
litopon tdng hap duac
bang cac phuang phap vat
If
va hoa
li
khac nhau.
- Tu cac ket qua nghien cuu da de xuat qui trinh dieu che bot mau lithopon
tii 2 loai quang noi tren.
De tdi
dd gap phdn dao
tgo:
01 Luan van thac sT.
03 Khoa luan tot nghiep.
f.
Tinh hinh
su dung kinh
phi.
+ Tong kinh phf dugc cap:
+ T6ng
kinh phf thuc chi:
KHOA HOA HOC
20,0 trieu dong
Prof. Dr.
c. Members:
- Vu
Dang
Do, Prof. Dr.
- Trieu
Thi
Nguyet, Assoc.
Prof. Dr.
- Nguyen
Thi
Thuy Hang,
Ma.
student
d. Researching Attitudes
and
Contents:
Researching attitudes:
- Study
on
using baritin
and
zinc oxide from Vietnam
for
producing
pigment lithopone
Researching Contents:
- Study
on the
process dissolving baritin from
barium sulfide,
-The process
of
removing
Si02 AI2O3
and
some heavy metals from
ZnO
from Tuyen Quang
for
preparing
the pur
solution
of
ZnS04
-The process
of
precipitation
the
wihte pigment lithopone from
the
salt
solutions
of
zinc sulfate
and
barium sulfide
-
Tlie
chemical composittion
I. Xac dinh thanh phan quang ban dau 11
1.
Phan
tich
thanh phan quang baritin 11
2.
Phan tfch thanh phan quang kem 11
II.
Dieu che dung dich bari sunfua 11
I. Anh huang ciia nhiet do tai hieu suat phan huy quang 12
2
Sir
phu thupc
ciia
hieu suat phan huy quang vao luang than. 12
3.
hieu suat phan huy quang
phiJ
thupc vao loai than 13
4.
Sir
phu thupc cua hieu suat phan huy quang vao thai gian nung 13
5.
So sanh hieu suat phan huy cua
BaSOj
va quang baritin 14
III.
Dieu che dung dich
ZnS04tLr
quang kem
va tfnh chat cua litopon 17
1.
Dp trang va do tham dau cua litopon 17
2.
Nghien
ciai
litopon bang phuang phap nhidu xa tia X 18
3.
Nghien
cuu
htopon
bang
phuang phap kfnh hien vi dicn
tuquet
20
4.
Phan tfch
cohat
2
5. Phan tfch thanh phan san
phfim
bang phuang phap huynh quang tia X 25
KET LUAN 26
TA\1
LIEU
1
HAM KHAO 27
5
MODAU
Cac
lieu
dau de san xuat litopon co
a
nhieu nai nhu Cao Bang, Thanh Hoa, Nam Xe (
Ha Bac ). Nhung lugng can
ddi
vai sac to nay van phai nhap tu ngoai.
Xuat phat
tir
thuc te do chiing toi nghien ctru qua trinh dieu che litopon
tir
cac nguon quang kem va quang bari ctia Viet Nam vai hi vgng dong gop cho qua
trinh nghien cuu san xuat litopon tu cac khoang vat trong nuac dt thay the cac
san pham nhap ngoai. Gop phan giai quyet yeu cau truac mat va lau dai cua
nganh cong nghiep son va cao su
ciia
nuac nha.
L (Jidi
thieu ve litopon
Litopon la tinh the; co mau trang, thanh phan gom ZnS va
BaS04
vai ti
le
1:
I
va
iSn
mot lugng nho ZnO. Litopon dgc dung lam chat mau cho
scTn,
da
khiic
xa
ciia
ZnS la
n^
= 2,37
va
BaS04
la
n^
=
U64.
ZnS chiia trong litopon cang nhidu
thi
do xop ctia no cang
Ion.
Sac mau cua litopon cung phu thuoc vao ti le tron giiia ZnS va
BaS04.
Theo
Bogaia Valen va Kudanhexop
thi
chi so khiic xa
ciia
litopon tieu chuan
n^
= 2,0,
ti le ZnS chiia trong litopon cang lan
thi
chat
Igng
muoi
ZnCl2
tan trong nuac. Ong suy ra rang litopon ben trong anh sang sau khi
ngam no trong axit sunfuric rat loang (2%) de hoan toan
riia
sach cac muoi
ciorua tan trong nac. Nhilu cong
Irinh
nghien
ciru
ve tfnh ben vung doi vai anh
sang
CLia
litopon
ddu
la do
sir
phan huy ZnS thanh kem kim loai va lu huynh.
Nguai la giai thfch hien tugng litopon den roi trang tra lai dugc la do
sir
oxy
hoa kem kim loai thanh ZnO bang oxy khong khf. Kaphir va Davidolexcaia cho
rang neu muon tong hgp litopon khong bi thay ddi mau sac duai tac dung
ciia
anh sang, can phai dua vao dung dich
ZnS04
nhiing muoi tan trong nuac vai
lugng coban khoang
0,005%
so
4 CO
-121.7
kcal
(1)
BaSO,
+
2 C
->
BaS + 2
CO.
44,3
kcal (2)
Xpini Donob da da ra ket luan rang
sir khir
barit xay ra nh sau : ban dau mot phan
than chay trong dilu kien thieu khong khf tao ra oxit cacbon va sau do xay ra
qiia
trinh
khii
barit bang oxit cacbon theo phan ting :
BaS04
+ 4 CO
^
BaS +4
CO2 + 33.1
kcal
4
CO,
+ 2 C
true
tiep len barit ma la oxit cacbon.
Nghien
ciiu
anh hudng ciia cac hgp chat trong hdn hgp tu nhien vai quang
barit len qua trinh khu cho ta thay su co mat
Si02
lam giam hieu suat tao thanh
BaS.
6
nhiet do tren
l000^BaSO4
trong quang tac dung vdi
SiO.
theo cac phuang
trinh
phan ting sau :
BaS04
+
S1O2 = BaSi03 + SO3
BaS04 -H
BaSiO,
=
Ba2Si04
+ SO3
2
BaS04
+
BaSi03 =
Ba3SiO,
de tao ra
BaSi03.
Cac tac gia ndi tren cung da khao sal
sir
phu thuoc
ciia
tdc do khu barit bang mot
sd loai than khac nhau va nhan thay tdc do khu barit bang than cdc cung gidng
than da.
2.
Dieu
che
ZnSO^
tif
ZnO tac dung voi dung dich
H.SO4
Dau tien lam giau quang va loai bd nhung tap chat khong cd
Igi
cho qua
trinh dieu che
ZnS04
can loai tru. Sau dd dem quang da dugc lam giau d tren tac
dung vdi dung dich
H2SO4
cd ndng do thfch hgp. Khdi lugng rieng cua
H2SO4
dugc diing trong nhung tnrdng hgp nay la 1,675
g/ml.
Mot phuang phap khac de'
dieu che
LHC
do la litopon
BaS +
ZnSO,
-^
BaSO,
+ ZnS
-
24 kcal
Nghien curu tfnh chat cua litopon phu thuoc vao
di^u
kien ket tua cua no.
Sunxa
cho
rang
muon co litopon ben vung ddi voi anh sang ket
tiia
can tien hanh
trong
di6u
kien co du luong bari sunfua.
Bogoia
Volexki
va Nhe Roxlacaia da nghien cuu tfnh chat
ciia
litopon thay
ro tfnh chat cua no phu thuoc vao pH cua moi truong ket tua
Chat lucmg litopon phu thuoc chu yeu vao do pH
a
thoi diem
Sau do barisunfua hydroxyt phan huy thanh
Ba(SH)2
va
Ba(OH)2
SH
2 Ba ( .5
H2O -^ Ba(SH)2
+
Ba(0H)2
+ 10
H.O
OH
Ke't qua cua su thuy phan la tong tac
ciia
chiing voi
ZnSO,
:
SH SH
Ba
<
+
ZnSO,
->
BaSO,
+ Zn <
OH OH
Ba(SH)2
+
ZnSO,
^
thuy phan nen ZnO chiia trong litopon khdng qua
1%.
Trong dung dich bari
sunfua va bari hydroxit la :
Ba(SH)2 _ 203
Ba(0M)2 ~ 111
Thuc te ti le bari sunfua va bari hydroxit khong dugc qua 1,1
-
1,3 bdi vl
mot phan
Ba(0H)2
bi oxy hoa bdi khdng khf thanh
pdli
sunfua va hypo bari
sunfua. Trong dung dich BaS loang BaS bi thuy phan vdi mot lugng
Idn
va
Ba(SH)2
bi oxi hoa nhilu han do dd
ti
le tren giam xudng nhd hon
I.
Neu dung
dung dich nay
d^
san xuat litopon
thi
lugng ZnO se tang len tu 2%- 3%.
0
PHAN THLC
210"C.
Khi
den
120"C thi
nhiing tang con quang bat dau nd
lach
tach va tinh the'
BaS04bat
dau
va ra .
Cii
30 phiit, lay
mSu
ra ray qua ray 0,2nm. Tinh
thi BaS04
va vun khi
nung con thach anh, sunfua kim loai nang, cudi cung nam lai tren mat ray va
bi loai bo.
Ket qua thu dugc lugng bgt
la
366,820g va lugng tap chat cdn lai la
132,820g
Bang phuang phap hoa hgc, chiing toi xac dinh dugc thanh phan cac chat cd
trong quang sau khi lam giau. Ket qua thu dugc d bang 2:
Bdng
I:
Thanh phdn {%) cua quang baritin sau lam giau.
BaSO,
82,74
Fe^O,
quang ZnO bang phuang phap
huynh quang
tui
X thu dugc
kit
qua ham luang
ZnC)
la
86.99r
(Phu luc 2)
H.
Dieu che dung dich bari sunfua
11
L
Anh
huang
cua
nhiet
dp den
hieu sudt phdn
huy
quang.
Lay
9
mau
quang baritin
mdi
mau
cd
khdi luang
San pham
sau khi
nung dugc
dem di xac
dinh
ham
lugng BaS
di
tfnh hieu
suat phan
hiiy.
Ket qua
dugc trinh
bay d
bang
1.
Bdng
2:
Sit
phu thupc
ciia
hieu sudt phdn
BaSO_f
vdo
nhiet
dp.
Mau
1
2
3
(phan
huy)
2,17
2,20
2,15
2,17
%
72,45
73,49
71,49
72,48
m
quang
(dau)
3
3
3
1000"C
m
quang
(phan
huy)
2,30
2,29
2,35
2,31
%
76,60
76,27
78,33
theo phan
ung.
BaS04
+ 4C0 =
BaS
+
4CO2
+ 33,1
Kcal
4CO2
+ 2C
=
4C0
+ 2CO2
-
77,4Kcal
2.
Sit
phu
thuoc
ciia
hieu sudt phdn
huy phu
thuoc
vdo
lupng than.
Lay
6 mfiu
quang
moi mau co
la 3 gid. Tir
ket
qua xac
dinh
ham
luang BaS trong
cac
chen
san
phiim
thu
duac
tinh
dugc
hieu suat
qua
trinh phan
huy
quang.
12
Bang 3: Hieu sudt phdn huy phu thupc vdo luang than.
TT
1
2
3
m.
than(g)
1
1
2
Ket qua thuc nghiem cho thay khi diing lugng than la 3g nung d nhiet do
900"Ctrong
thdi gian
3gidthl
hieu suat phan huy dat 74,08%.
3.
Hieu
sudt
phdn huy phu thupc vdo loai than.
Lay cac
mau
quang baritin, mdi miu co khdi lugng 3g, tron
diu
voi 3g bgt
than d day diing 3 loai than khac nhau. Than gd, than da, than hoat tfnh.
Nung cac mau d cac nhiet do
900'*C.
Thdi gian nung dugc giu nguyen: 3h.
Ket qua thu dugc
trinh
bay d bang sau:
Bdng 4: Hieu sudt phdn
hiiy
BaSO^
phu thuoc vdo loai than.
Nhiet
do
nung
900"C
1
%
58,95
%
Kei qua d bang 4 cho thay, trong 3 loai than nghien
ciiu
than gd va than da
cd tac dung gan ngang nhau. con hieu qua
khii BaS04 bang
than hoat
tinh
thap
hcfn
nhilu. Dilu nay cd the dtrgc giai thfch
la
do mot phan than hoat tfnh da bi
chay trudc nhict do xay ra phan ung
khii BaS04
4.
Sir
phu thuoc cua hieu sudt phdn
hiiy
vdo thoi gian nung.
Lay ra 8 mau quang mdi
miu
cd khdi lugng 3g
iron
deu
vai
3g bgt than.
Cho hdn hgp vao chen
3
3
3
3
3
3
3
m.quang.g
(phan huy)
1,42
1,39
2,65
2,67
2,17
2,20
2,48
2,49
Hieu
.suat
(%)
47.26
46,26
68.19
69.15
72.45
73,49
82.62
82,13
46,74
68,67
3gid. Tu ham lugng BaS
tinh
ra hieu suat phan
hiiy.
Ket qua trung
binh
cua 3
mau dugc chi ra d bang sau:
Bdng 6. Hieu sudt phdn
hiiy
BaSO^
vd quang Baritin.
BaSOjtinh
khiei
m.(g)dau
3
m.(g) phan
huv
2.97
'
%
99,0
m. (g)
dau
3
Quang Baritin
m(g)phan
huv
2,17
%
Fe.O,,
FeO, CuO
+ddH.SO,20%
ZnS04,
Fe2(S04)„ CUSO4
+ Zn hot
SiO,,PbS04
ZnS04,
FeS04,Al2(S04)
u +
CLZnO,^
Pb,
Cu.
ZnS04
Fe(0H)„Al(0H)3
Dung dich kem sunfat thu dugc dugc ket tinh lai va dem di phan tfch bang
phuang phap nhilu xa tia X, ket qua thu dugc trinh bay d phu luc 4. Tren gian dd
nhilu xa tia X chi co cac pic cua
ZnS04
,cac pic cd do net cao, so sanh vdi
alat
chuan ASTM thay hoan loan
phi!i
hgp vdi bg pic chuan. Dilu nay cho phep ket
luan dung dich
ZnS04
thu dugc dam bao do sach de dilu che litopon.
IV. Tong hgp Litopon
I.
Khda sdt dnh hudng
thanh phan cua BaS va
ZnS04.
Litopon cd mau trang nhai
iing
vdi ti le BaS
:ZnS04
la gan
1:
1
2,
Anh hudng cua pH den mot so
tinh
chdt cua litopon
Dung dich
ZnS04
dugc dieu chinh tdi co gia tri pH khac nhau:
5.
6, 7. 8, 9
va
10.
Sau dd dugc tron vdi dung dich BaS theo ti le
moi
1:1
dl kei
tiia
lithopon.
Vira
tron
vira
khuay
phdni.
Sac to litopon dilu che dugc dem nung d
nhung
nhiet do khac nhau: 0 40
-
50"C
nd van giu nguyen mau trang. Khi tang nhiet dp litopon chuyin tu mau
trdng sang mau nga. Neu nhiet do nung cao niia mau cua no chuyin sang vang
nhat.
Hien
tugng nay dugc giai thfch la nhiet
dp
cang cao thanh phan kem sunfua
trong litopon thay ddi, vl mpt phan kem sunfua bi phan huy.
Nhu vay: Mau sac cua litopon phu thupc vao ti le chai ban dau, pH cua
phan ling tdng hgp va nhiet do nung san pham.
4. Dieu che litopon di tu hod chdt tinh khiet.
Cach lien hanh
cilng
tuang
tir nbu
tren.
Bari sunfua duac
dicu
che bang
cac nung Bari Sunfat tinh
khiei
vdi thau d
900'C,
then gian
trdng vd dp thdm ddu cua litdpon
Chiing toi dieu che litpon
tir
quang va tii hda chat tinh khiet dem xac dinh
dp trdng va dp tham dau d Phong thf nghiem san, Vien Hoa hpc cong nghiep.
Kei qua dugc chi ra d bang 9 va 10.
Bdng 9: Ket qud do dp trdng cua cdc mdu litopon
TT
Kei qua
thii
nghiem
Chi
tieu
Mdu sp dieu
che
tir
quang,
150"C
Mau sp dilu
chetuHCTK,
I50"C
Mau sp dieu
i
Mau sp dieu
che
tii quang,
'
chetuHCTK.
700"C I 700'C
Dp Trang
i
38
Kei qua nay cho thay d
mau
san phdm dilu che
tir
quang
150"C
cd dp tham
dau kem han so vdi mau san pham di ciing hda chai tinh khiet d
citing
nhict do.
Cdn hai mdu san pham dicu
che tu
quang va
tir
hoa chai tinh khiei d
7()0''C
cd do
tha'm ddu nhu nhau. Cac mau san pham
na\
co do tham dau dat
lieu
chuan su
dung cho son.
A
HA.
J.,
j
17
phham di
tir
hda chai tinh khiei chi cd cac pic cua
BaS04
va ZnS so sanh vdi
atlat
chuan ATMS thay hoan toan phii hgp. Dilu dd cd
thi
kei luan rdng san phdm thu
dugc kha tinh khiei. Cac pic nhgn
va
sac net, nhu vay san phdm
co do
tinh khiet
cao.
VNU UN 3iEr/bNS
D50n^
M^i
^
J
i
\
1
'••^•,-'j'.
^ I rieid
icji'
Hinhl: Gian do XRD mdu litopon dieu che
tu
HCTK,
ISffC
hinh
3 va 4.
Kfch
thudc
hat cua mdu san
phdm
di tii
quang cung
Idn
han so vdi mdu san
pham
di tu
hda chai tinh khiei.
vNu
•
iN-Sirf.irN:=
r.'.nci'
'.i-,,
f
J.JiA;y^'UUl!uLLlJ \L j>j:A^' U.ji , ;:v'A^
2
Tneia
Soad
Hinh
3:
Gidn
do XRD mdu
litopon dieu
che tu hoa
chdt tinh
]
;• /-!
A-
\
J
,
_j
//////; -/;
Gidn
dd XRD
dicu
che
tu
quang
7(HfC
19
J. Phuang phdp kinh hien vi dien tu quet (SEM)
Vdi phuang phap nay ta cd
thi
do dugc kfch thudc cua hat trong cac mdu
san pham. (J mdu san pham di tii hda chai tinh thiei cd cac hat
diu
ban mdu san
pham di tii quang d nhiet do
150^t.
Kfch thudc hat nhd nhai khoang 500nm kfch
thudc hat
Idn
nhai khoang 2000nm.
Hinh
6
4_2
1
2)
Hinh 7: Anh SEM mdu litopon dieu che tit
HCTK,
700^C
"):)
Optjralor
UM::>
VNU '
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Client
rione
Job lob number fi
F?es tJltraline
Label
Hang-KHoa-Quang70qoC
'20CiOnrn
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II)
Nov
i)4
UJ
29 Jbi
Hinh 8: Anh SEM mdu litopon dieu che tit
quang,
700 C
4. Phdn tich kich cd hat
Bang phuang phap nay cd
thi
tfch thuc la 55%. Phu luc 10
23
LS Particle
Size
Analyzer
3
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COULTER
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Nov
2004
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f^ame
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numoe'
Commenis
Optical
model
LS
230
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Hinh 9: Gidn dd phdn bd kich
cohat
mdu litopon dieu che tit HCTK
15&'C
24
J,
rnuang
pnap nuynn quang ua A.
Mau san
phiim
dilu che tu quang dac nung d nhiet do
150^'C
va
700^'C
dem
phan tfch bang phuang phap
hijynh
quang tia X. ( phu luc) .
Ket qua tren cho thay trong mau litopon
vira
dilu che dac ZnS chiem ty le la
24%
mau
litopon dilu che duac cd chat
lugng
tdt.
TCr nhung phuang phap phan tfch san phaim tren cho thay chiing ta cd
A1.(S04),
Pb,
Cu
+
ChZnO,
I"
ZnS04
Fe(OH),, Al(OH)-
Rira'
-^
Nuns
Nshien
Litopon,!
25
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