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Nano. C. Overview of Carbon Group Research Program. NC100 - Local AC. -Rostam [Science Officer] -Zairy [Science Officer]. Characterization. Acid Base Titration. -Rostam [science Officer] -Salamiah [Science Officer]. CARBON GROUP. Iodine / CCL 4. -Azman [Science Officer]. - PowerPoint PPT Presentation
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Overview of
Carbon GroupResearch Program
Nano C
CARBON GROUP
-Rostam [Science Officer] -Zairy [Science
Officer]
-Norly [PhD student] -Imran [PhD
student] – Ali [PhD student]
-Rostam [science Officer] -Salamiah [Science
Officer]
-Azman [Science Officer]
NC200 Commercial AC KD Tech
NC100 - Local AC
Characterization
Acid Base Titration
Iodine / CCL4
NC100Objective
Achievement
• Succeed in producing activated carbon with low production cost.
• Succeed in producing of homogenous mesopores distribution but still shallow of pore features ( measured via pore volume) surface area 475m2/g, meso 0.04cc/g, total pore 0.2 cc/g.
• Low production cost of Activated carbon.• To get high mesopore distribution.
Solution vs weakness
An existance of Si and Fe and others inorganic compound will be removed by using Nitrate acid as an alternative .
Nitrate acid is helping breaking the micropores to mesopores features.
Flow Chart of NC100 Preparation Process ( For KD Replacement )
Palm kernel
Dry & wash
Deionized water by usingUltrasonic for 6 hours at 60oC
dried
Dry by using conventional oven at 60oc Overnight
carbonization
Gas CO2At 900C for 4 hours
Activation
Carbonized with N2 from room temp.
to 900C
Carbonized with N2 from room temp to
900oC
Soak with 17MNaOH /
12hrs/ dry 120oC 12hrs
NC100 – Preminalary Results
Element Weight% Atomic%C K 87.86 90.8O K 11.62 9.02Si K 0.29 0.13Fe K 0.22 0.05Totals 100
870 nm
737 nm
716 nm
816 nm
708 nm
I. Support modification
Objective : Oxidative treatment of activated carbon to obtain mesoporous carbon
II. Synthesis of CNT/CNF on AC supported Fe catalyst
Objective : to get high dispersion and homogeneous of nanocarbon on AC
NC200 – current work
Support Modification – Meso program
Raw AC-KD
475oC 500oC 525oC 550oC
Physisorption measurement
Heat 10K/min, hold 3hrs, synthetic air flow rate 25ml/min in UTP
575oC
Support Modification – Meso program
Raw-HT475 475 1568 0.502 0.557 0.055
Raw-HT500 500 1313 0.621 0.5389 0.0821
Raw-HT525 525 1217 0.5612 0.5264 0.0348
Raw-HT550 550 1203 0.5535 0.4855 0.068
Raw-HT575 575 1229 0.5859 0.5345 0.052
AC-Raw - 1124 0.441 0.399 0.042
Sample TOC SBET (m2g-1) Total pore V Vmicro (cc/g) Vmeso (cc/g)
0.0 0.2 0.4 0.6 0.8 1.0150
200
250
300
350
400
450
RAW HT475 HT500 HT525 HT550 HT575
cc /
g
P / Po0 5 10 15 20 25 30 35 40 45 50 55
-0.01
0.00
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
0.09
0.10RAW HT475 HT500 HT525 HT550 HT575
Dv/
Dr
(cm
3/g
A)
Pore radius A
isotherm BJH
mesopore
Support Modification – Meso program
Pre-treatment [heat 200oC, 2hrs, wash 5M HNO3 / 24hrs/ RT]
400oC 450oC 480oC 500oC
Physisorption measurement
5K/min, static air flow in small furnace
Raw AC-KD
Holds time : 1hrs, 3hrs, 5 hrs, 7hrs
0.0 0.2 0.4 0.6 0.8 1.0150
200
250
300
350
400
450
500
550
Vo
lum
e (
cc/g
)
Relative Pressure (P/Po)
RAWACAWA009_B ACAW5001HR_B ACAW4507HR_B ACAW4505HR_B ACAW4503HR_B ACAW4505HR20_B
0 10 20 30 40 50 60
0.00
0.02
0.04
0.06
0.08
0.10
Po
re V
olu
me
(cc
/A/g
)
Pore width (A)
Micropore Mesopore
isotherm
BJH
Sample TempTime
HoldRate/min
% Yield Decreased
Surface Area (m2/g)
Pore volume (cc/g)
Average pore width (nm)
Total Pore Volume (cc/g)
Pore volume [mesopore]
(cc/g)
ACAW50020HR 500 20 5 Ash X X X X X
ACAW60020HR 600 20 5 Ash X X X X X
ACAW5001HR 500 1 5 51.19 1224 0.6529 4.805 0.7538 0.1009
ACAW6001HR 600 1 5 Ash X X X X X
ACAW5003HR 500 3 5 Ash X X X X X
ACAW5005HR 500 5 5 Ash X X X X X
ACAW4001HR 400 1 5 6.19 1182 0.4889 3.749 0.5671 0.0782
ACAW4501HR 450 1 5 11.81 1372 0.6079 3.980 0.6786 0.0707
ACAW4003HR 400 3 5 8.75 1194 0.5023 3.873 0.5775 0.0752
ACAW4503HR 450 3 5 26.13 1280 0.5985 4.392 0.6982 0.0997
ACAW4005HR 400 5 5 7.93 1311 0.5617 3.900 0.6513 0.0896
ACAW4505HR 450 5 5 37.60 1340 0.6755 4.619 0.7955 0.1200
ACAW4507HR 450 7 5 63.52 1037 0.5600 4.728 0.6646 0.1046
ACAW4509HR 450 9 5 69.43
ACAW4505HR20 450 5 20 35.53 1299 0.6492 4.447 0.7614 0.1122
ACAW4505HR1 450 5 1 56.84
ACAW4801HR 480 1 5 27.41
ACAW4805HR 480 5 5
A009 Norly Ali
- - 1122 0.4598 3.469 0.5210 0.0612
Raw ACAW (A009)
- - 1234 0.5063 3.536 0.5827 0.0764
Future Plan
• Compare the highest mesopore volume method with UTP+synthetic air method– Rotating UTP – the burning process more
homogen
• The best method use to create a mesopore based substrate for impregnation process
Schematic diagram for mesoporous program
Raw AC-KD
450oC 475oC 500oC 525oC
Heat 10K/min, hold 3hrs, 5%O2 in N2 flow rate 100ml/min, ToC is based on Meso2
BET=Meso 1A
BET=Meso 1B
A009
Heat 10K/min, 5%O2 in N2 flow rate 100mil/min, ToC
Impregnate with Fe
BET = Meso2
BET=Meso 2A
1K/min 3K/min 5K/min
D080-1 D080-2 D080-3
Heat 10K/min, hold 3hrs, 5%O2 in N2 flow rate 100mil/min,
ToC is based on Meso1B [xxxOc]
BET = Meso 1C
Further Calcine 120C, 5%O2 in N2,Wash with 5M HNO3, RT, 24hrs
Heat 10K/min, hold 3hrs, 5%O2 in N2 flow rate 100mil/min
Synthesis CNF/CNT on AC/Fe
Big Raw AC Wash 5M HNO3 24hrs
Grain / seive <50µm
Wet impregnation 1wt% Fe-nitrate/Fe-acetate
Ultrasonification / 30min
Calcination
• 250oC
• Hold 1hrs
• 5%O2 in N2
Reduction
• 300oC
• Hold 1hrs
• 5%H2 in N2
Growth
• 700oC
• Hold 2hrs
• 200ml H2 / 30ml C2H4
SEM images – iron nitratecal250, red300, growth700
Element Weight% Atomic%C K 90.03 92.51O K 9.50 7.33Si K 0.23 0.10Fe K 0.24 0.05Totals 100.00 100.00
SEM images – iron acetate,
cal250, red300, growth700
Element Weight% Atomic%C K 85 88.52O K 14.39 11.25Si K 0.39 0.17K K 0.07 0.02Fe K 0.15 0.03Totals 100
Acknowledgement
Combicat & NanoC team
FHI team
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