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tổng hợp zeolite 4a từ kaolin

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B GIÁO DO
I HC C




VÕ TH TÚ QUYÊN


TNG HP ZEOLITE 4A T KAOLIN



LUI HC



Chuyên Ngành: HÓA HC






C
i


B GIÁO DO
I HC C




VÕ TH TÚ QUYÊN



TNG HP ZEOLITE 4A T KAOLIN



LUI HC



Chuyên Ngành: HÓA HC




NG DN KHOA HC
NG THIN




C



i Hc C Cng Hòa Xã Hi Ch tNam
Khoa Khoa Hc T Nhiên c lp - T do - Hnh phúc
B Môn Hóa Hc
NHN XÉT A CÁN B NG DN
1. Cán b ng dn: TS. ng Thin
2.  tài: tng hp zeolite 4A t kaolin.
3. Sinh viên thc hin: Võ Th Tú Quyên MSSV: 2102290
Lp: C nhân Hóa  Khóa K36
4. Ni dung nhn xét:
a) Nhn xét v hình thc ca LVTN:


b) Nhn xét v ni dung c ngh ghi chi ti):
 i dung thc hin c tài:


 Nhng v còn hn ch:


c) Nhi vi tng sinh viên tham gia thc hi tài (ghi rõ tng
ni dung chính do sinh viên nào chu trách nhim thc hin nu có):


d) Kt lu ngh m:
C
Cán b ng dn

ng Thin




i Hc C Cng Hòa Xã Hi Ch t Nam
Khoa Khoa Hc T Nhiên c lp - T do - Hnh phúc
B Môn Hóa Hc
NHA CÁN B CHM PHN BIN
1. Cán b chm phn bin:
2.  tài: Tng hp zeolite 4A t kaolin
3. Sinh viên thc hin: Võ Th Tú Quyên MSSV: 2102290
Lp: C nhân Hóa  Khóa 36
4. Ni dung nhn xét:
a. Nhn xét v hình thc ca LVTN:


b. Nhn xét v ni dung c ngh ghi chi ti):
 i dung thc hin c tài:


 Nhng v còn hn ch:


c. Nhi vi tng sinh viên tham gia thc hi tài (ghi rõ tng
ni dung chính do sinh viên nào chu trách nhim thc hin nu có):


d. Kt lu ngh m:


Cn 

Cán b phn bin

 V
i







 





           


 
















 V
ii

TÓM 

Zeolite 4A là sn phm bt màu tr c tng hp bng phn ng
thy nhit kaolin hot hóa (metakaolin), sn phm chuyn hóa ca kaolin
i, mt loi khoáng có giá r, có b sung sodium aluminate. 

 
            
hydroxide (NaOH). Trong lu    ng ca thi gian già hóa,
n ng mm zeolite lên hình dng và hiu sut sn phc
nghiên cu. Hình dng, kí c c     nh bng nh
hin t quét (SEM). Cu trúc tinh th nh bng
u x tia X (XRD). Kt qu cho thy chúng có hình khi lp
i nhng tính cha zeolite 4A.






















 V
iii

ABSTRACT


Zeolite 4A, a white powder, was synthesized by the hydrothermal
reaction of activated kaolin (metakaolin) derived from commercial kaolin, a
low cost mineral, with sodium aluminate. The use of the Sothern of
Vietnam-kaolin as an alternative cheap raw material for the synthesis of
zeolite 4A for sodium tripoly phosphate to production washing powder was
carried out by hydrothermal treatment of metakaolin with aqueous alkali
Sodium hydroxide (NaOH). In this study, the influence of aging time,
concentration of HCl and crystal of zeolite 4A on the characteristics and the
yield of the product have been studied. The characteristics and morpholo gy of
zeolite 4A crystals were determined using scanning electron microscopy

(SEM), X-ray diffraction (XRD). The particles had a cubic shape,
characteristics of standard zeolite 4A























 V
iv





              



Ký tên





Ngày: 






 V
v

 

 I
 II
ABSTRACT III
 IV
 V
 VII
 VIII

 IX
 1 1
  1
 1
1.2. hh 1
1.3.  2
C 2 3
 QUAN TAI LIÊU 3
 3
2.1 3
2.1.2. Phân  zeolite 5
zeolite 7
 10
 18
 23
,
 23
 25
2.2.3 Các yu t ng ng hp zeolite
26
 27
 27
 29
C 3 33
 PHÁP NGHIÊN  33
 V
vi

3.1  33
 33

 33
 34

 34
 36
 37
38
 38
 41
NG 4 42
KT QU VÀ THO LUN 42

3
trong
kaolin 42
 42
 
 42

 44
4.2.3. Kho sát ng ca mm lên quá trình tng
hp zeolite 46
4.2.4 Kt qu tng hp zeolite 4A  u kin tt
46
 5 51
  VÀ   51
5.1. K 51
 51
TÀI  THAM  52
 V

vii


Hình 2. 1 
[12]
4
Hình 2. 2 Mô t t din SiO
4
và AlO
4
-[6]
8

[3]
9

[9]
9
Hình 2. 5 nh zeolite A, Sodalith, zeolite X, Y
[9]
10

[4]
13
Hình 2. 7 
[4]
. 14
Hình 2. 8 
[4]
14


[17]
15
Hình 2. 10 Chn lc trng thái trung gian
[17]
16
Hình 2. 11Chn lc sn phm to thành
[17]
17
Hình 2. 12Cu trúc tinh th ca Zeolite X và Zeolite Y
[18]
18
Hình 2. 13ZSM-5
[2]
19
Hình 2. 14 Zeolite Mordenite
[12]
20
Hình 2. 15 S
5-[11]
21
Hình 2. 16 C
[18]
21

[12]
24
Hình 2. 18 
[13]
28

Hình 2. 19 Quy trình tng hp zeolite 4A t kaolin 30
Hình 3. 1 Máy nhiu x tia X 40
   rng vch nhiu x. 40
Hình 4. 1 ng ca n n tng hp zeolite 4A 43
Hình 4. 2 Mu zeolite 4A công nghip 47
Hình 4. 3 Mu zeolite 4A tng hp 47
Hình 4. 4 nh SEM zeolite 4A công nghip 48
Hình 4. 5 nh SEM mu zeolite 4A tng hp 48
Hình 4. 6 Gi nhiu x tia X ca mu zeolite 4A tng hp 50

 V
viii


Bng 2. 1 S bii tính cht ca Zeolite khi t s SiO
2
/Al
2
O
3
7
Bng 2. 2  25
Bng 3. 1 Dng c và thit b 33
Bng 3. 2 T s mol các cht phn ng to zeolite 4A 34
Bu kin thí nghim kho sát ng ca n HCl 35
Bng 3. 4 u kin thí nghim kho sát ng thi gian làm già 36
Bng 3. 5 u kin thí nghim kho sát ng mn quá trình
tng hp 37
Bng 4. 1 Kt qu phân tích mu laolin TLP132-BD 42
Bng 4. 2 Kt qu phân tích mu kaolin TP131-BL 42

Bng 4. 3 ng n HCl lên hiu sut tng hp zeolite 4A 44
Bng 4. 4 ng thi gian làm già lên hiu sut quá trình tng hp zeolite
44
Bng 4. 5 ng SiO
2
c ra: 45
Bng 4. 6 c ra: 45
Bng 4. 7 ng ca mn hiu sut tng hp 46
 V
ix



STTP Sodium tripoly phosphate
ZSM-5 Zeolite Socony Mobil5
MOR Zeolite Mordenite
SBU Secondary Building Unit
LTA Zeolite 4A
AlPO Zeolite Aluminophotphate
SEM Scanning Electron Microscope
c tinh th
 Góc nhiu x tia X
 
 Hng s, có giá tr 0.9
d
c
c tinh th
  rng vch nhiu x ti 1/2 ci vch nhiu x
cao nht
 V

1


 1

1.1.  
          
.
T
          zeolite    
              
. Do zeolite 4A

[1]
.
  zeolite    
n tnh cao, 
zeolite 4A, tháng
zeolite 
 Zeolite 



3

zeolite 4A ph
zeolite
[2]
.
1.2.  hh


zeolite

[3]
.

zeolite


o
C
[4]
.

zeolite-m

[5]
.

zeolite
 V
2

     
o


[6]
.


zeolite

[7]
.
   zeolite
zeolite

aluminate. K
zeolite
o


[8]
.

   

zeolite
1.3. 
zeolite
             
              
(

zeolite
              
zeolite
[9]
.
zeolite

  
zeolite  

zeolite

zeolite 4A.



 V
3


C 2
 
zeolite
Zeolite là 





M
2/n
O.Al
2
O
3
.xSiO
2

.yH
2
O (2.1)



SiO
2
/ Al
2
O
3
.
12 ).
         

[10]
.
 Zeolite A có x = 2.
Zeolite X có x = 2,3 3.
Zeolite Y có x = 3,1 6

2.1zeolite

 






 V
4


n
và iso parafin.









   

       




[11]



Hình 2. 1 
[12]
 V
5


   

 



[13]
.
2.1.2. Phân  zeolite



[14]
.
2.1.2.1. Ptheo

a. Zeolite tự nhiên
 

         

[15]
.
b. Zeolite tổng hợp
Zeolite Zeolite A, Zeolite X, Zeolite Y, Zeolite ZSM-5,
ZSM-11 Zeolite 




Zeolite 
Zeolite, theo cách này ta chia Zeolite 
Zeolite Å Å.
Zeolite 
Zeolite 
[15]

a. Zeolite giàu Al:
Zeolite SiO
2
/Al
2
O
3
 2.
 V
6

          Zeolite hai
Zeolite
-O--Si-O-Si- và
-Si-O-Al- SiO
2
/Al
2
O
3
là    SiO
2
/Al

2

O
3
< 2. Khi t Zeolite 
   zeolite         zeolite    
zeolite

+

+

2+
.
b. Zeolite silic trung bình:
 Zeolite   SiO
2
/Al
2
O
3
= 4       Zeolite
ZeoliteX, ZeoliteY, Sabazit
c. Zeolite giàu silic:



2
/Al
2

O
3
)

= 20 

             
  

4
N
+
.
d. Rây phân tử Silic.



e. Zeolite biến tính:
Là Zeolite 
Zeolite


Zeolite theo  SiO
2
/Al
2
O
3

             Zeolite.


 V
7

Bng 2. 1  SiO
2
/Al
2
O
3

f. Zeolite aluminophotphat ( AlPO
4
)

là Aluminophotphat (AlPO
4


iO
4
]
4-


4
]
5-
và [PO
4

]
3-
theo  
[15]
.
zeolite




4


4
có 4 ion O
2-



4

4




 Zeolite 
nhôm (Al).






 
2
/Al
2
O
3

1300)
0
C


acid acid 

 V
8






Hình 2. 2 
4
và AlO
4
-[6]


 Zeolite

 
TO
4
-Lowenstein.

 




-
-
[16]
.



 V
9



Hình 2. 3 C
[3]

Hai ô m ph TP (Tertairy polyhedra) là sodalite và canrinite:




Hình 2. 4 H
[9]
 V
10



Hình 2.5  


Hình 2. 5 
[9]
zeolite

zeolite

).
2.1.4.1 
zeolite 

 
 V
11


+

M

2+
). Các cat
  : 2 ion Na
+


2+
, hay 1 ion Na
+

+


zeolite 

zeolitezeolite 

+

+
zeolite
NaA (d = 4Å  KA (có d= 3Å).
zeolite, cation Na
+

+
 
nh   
H
+


+
.
zeolite 




g 

 zeolite
+ 

zeolite 
  



zeolite 

zeolite.
2.1.4.2.
Do zeolite 

zeolite.
Các zeolite 
zeolite 

 V
12


zeolite
zeolite 
zeolite 
zeolite.

zeolite zeolite 
 

2
ONH
3

zeolite 

               
zeolite giàu Si.
zeolite 


2
, H
2
S f
  thiên nhiên; tách SO
2
, NO
2
       
H

2
SO
4
/HNO
3
.

acid  
sát 
acid 


gây ra theo g , polyme hoá , izome hoá , alkyl
hoá.




hòa bI, 
 proton trong zeolite.

 acid  
acid tâm acid Lewis). Các

a. Sự hình thành tâm acid Bronsted:

×