DEMONSTRATION OF LARGE DEMONSTRATION OF LARGE SCALE PRODUCTION OF OLIGO SCALE PRODUCTION OF OLIGO
CHITOSAN CHITOSAN
GATOT TRIMULYADI REKSOGATOT TRIMULYADI REKSOE-mail: [email protected]: [email protected]
CENTER FOR THE APPLICATION OF ISOTOPE AND CENTER FOR THE APPLICATION OF ISOTOPE AND RADIATION TECHNOLOGYRADIATION TECHNOLOGY
NATIONAL NUCLEAR ENERGY AGENCYNATIONAL NUCLEAR ENERGY AGENCY
(Augustus 4th – 8 th - 15th, 2008)
11Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
DEMONSTRATION FOR 1000 L OLIGO-DEMONSTRATION FOR 1000 L OLIGO-CHITOSAN- LIQUID IRRADATION CHITOSAN- LIQUID IRRADATION
PROCESSPROCESS Raw materialRaw material - Chitosan 20 kg - Silver Nitrate 500 g- Chitosan 20 kg - Silver Nitrate 500 g - Lactic acid 20 L - NaOH pa 1 Kg- Lactic acid 20 L - NaOH pa 1 Kg - Demineral water 1000 L- Demineral water 1000 L MachineMachine - Mixing tank 1200 L - Raw mat storage- Mixing tank 1200 L - Raw mat storage - Irradiation tank 1500 L - Product storage- Irradiation tank 1500 L - Product storage - Liquid transfer system- Liquid transfer system Irradiator Irradiator ƴƴ – Co-60 – Co-60
22Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Preparation of 20 kg Preparation of 20 kg chitosanchitosan
MATERIALS :MATERIALS :- Wet fresh shrimp shell : 200 kgWet fresh shrimp shell : 200 kg- NaOH technical : 100 kgNaOH technical : 100 kg- HCl technical : 50 LHCl technical : 50 L- Demineral water : 100 LDemineral water : 100 L
33Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
4000.0 3000 2000 1500 1000 450.0
12.5
14
16
18
20
22
24
26
28
29.2
cm-1
%T
Laboratory Test Result
chitosan
3421.24
1650.53 1025.02
Deacetylation degree : 72.8 %
Molecular Weight : 1.574 104
44Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
6050403020100
1600
1400
1200
1000
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0
Irradiation Dose (kGy)
Vis
co
sit
y (C
ps
)
Irradiation of chitosan (2 %) in Lactic acid 2%
Fig 2. Irradiation dose(kGy) Vs Viscosity (Cps)
100806040200
1600
1400
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200
0
Irradiation Dose (kGy)
Vis
co
sit
y (C
ps
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Irradiation chitosan in solid conditions
Fig 1. Irradiation dose (kGy) Vs Viscosity (Cps)
Effect of irradiation on viscosity of chitosan
55Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Step for demonstration of Step for demonstration of preparing oligo-chitosanpreparing oligo-chitosan
Standardization of chitosanStandardization of chitosan Mixing processMixing process Transfer process to irradiation tankTransfer process to irradiation tank Irradiation ProcessIrradiation Process Finishing processFinishing process Preservation ProcessPreservation Process PackingPacking
66Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Standardization of chitosanStandardization of chitosan
Prepare of standard molecular weightPrepare of standard molecular weight
( Mw = 100 – 200 Da)( Mw = 100 – 200 Da) Irradiation methodIrradiation method Irradiation by Gamma ray : 25 kGy (48 hr)Irradiation by Gamma ray : 25 kGy (48 hr)
77Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
MIXING PROCESS ( 500 L)MIXING PROCESS ( 500 L)- Put a DM water 100 L to mixer tank - Add chitosan 10 Kg - Add DM water 100L - Keep for 1 hr - Add lactic acid 10 L - Stirr for 1 hr - Adding DM water up to 500 L (around 285 L)
Stirr for 3 hr until homogen
Chitosan lactic acid NaOH 2M Demineralized
water
88Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
During mixing processDuring mixing process
99Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Transfer process to irradiation Transfer process to irradiation tanktank
Using air pressure : Compressor
1010Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
MW of irradiated chitosan in solution (Dr Hien )
Table 1: The relationship of molecular weight of irradiated chitosan and absorbed dose
Molecular weight (Mw 103) of chitosan
Mw0 = 130,000
Dose, kGy 8 16
24 32 40
1% CTS 34.3 17.1 12.2 9.7 -
2% CTS
43.2 30.4 20.1 16.7 12.0
3% CTS
45.0 33.0 23.5 19.3 15.2
The suitable molecular weight (Mw) of oligochitosan for growth promotion and elicitation for plants is in the range of 10,000-20,000
Irradiation processIrradiation processDose : 35 kGy ( around 75 hr) At dose 12, 24, 30 and 35 KGy sample will be taken to be analyzed (± 2 L)
1111Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Irradiation Dose Vs ViscosityIrradiation Dose Vs Viscosity
403020100
60
50
40
30
20
10
0
Irradiation Dose (kGy)
Vis
co
sit
y (C
ps
)
35 kGy + Ag-Nano = 9.37 Cps
1212Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Preparation of Ag-nano/chitosan for utilization as preservative 1. Taking 10 litters of chitosan solution as above mentioned preparation 2. Adding 17 g AgNO3 (disolved in small volume of water) into chitosan
solution 3. Stirring about 15 minutes 4. Putting prepared Ag+/chitosan solution into plastic can 5. Irradiation at dose of 30 kGy 6. Ag-nano/chitosan colloid with concentration of 1.000ppm Ag.
1313Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Treatment after irradiation (Finishing)Treatment after irradiation (Finishing)
NEUTRALIZATION
-Take 25 L oligo chitosan after irradiated
- Adding 250 mL , 2 M NaOH, little by little
- Keep the solution for 30 min
1414Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
PROSEDUR FINISHING OLIGO-CHITOSAN
Buat 1 batch 25 L sebanyak 6 batch untuk di kirim ke negara FNCA ; Peralatan :
1. Ember 25 -40 L = 6 buah 5. Jerigen 30 L = 6 buah
2. Ember 50 L = 2 buah 6. Penhisap cairan 2 bh
3. Saringan mesh 7. Penakar
4. Pengaduk kayu 8. Pengaduk listrik
ProsesNetralisasi :
- Masukan dalam ember 25 L oligo chitosan hasil iradiasi di IRKA
- Tambahkan 250 mL , 2 M NaOH sedikit demi sedikit dan diaduk, kalau terjadi
penggumpalan NaOH diencerkan sampai 500 L
- Biarkan sekitar 30 menit
Proses pengawetan oligo chitosan sengan Ag-nano ( hasil iradiasi IRPASENA)
- Oligo chitosan sekitar 25 L yang sudah dinetralisasi dengan NaOH.
- Tambahkan sekitar 500 mL Ag-nano sedikit-dikit sambil di aduk.
- Aduk selama 30 menit.
- Saring dengan saringan net
- Masukan kedalam wadah untuk duikirim ke FNCA country –export perdana.
1515Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Preservation of oligo-chitosan with Preservation of oligo-chitosan with Ag-Nano of 20 ppmAg-Nano of 20 ppm
Taking 25 L oligo-chitosan that already Taking 25 L oligo-chitosan that already neutralization by 2M NaOHneutralization by 2M NaOH
Adding 500 mL Ag-nano/chitosan little Adding 500 mL Ag-nano/chitosan little by little while stirringby little while stirring
Stir for 30 minStir for 30 min Filter with net mesh (# 100)Filter with net mesh (# 100) Move to plastic drum of 30 L for Move to plastic drum of 30 L for
sending to FNCA countrysending to FNCA country..
1616Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Adding of 500 mL AgNOAdding of 500 mL AgNO33- - NanoNano
1717Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
PACKINGPACKING
1818Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
1919Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
At Nippon Express Indonesia, CengkarengAt Nippon Express Indonesia, Cengkareng2020
Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
Application (Dr Hien experience)
1. For Rice : Dilution 1000 times with water (20ppm), spraying 3 times (20,30 and 40 days after sawing), 500 L diluted/ha it means 1.5 L (2% of original oligo chitosan)/ha Seedling : For rice seed treatment, dilution 100 times with water (1/100). Rice seed are dipped in oligo chitosan solution about 10 min
2. For other plants such as tea, potato, carbage, sugarcane, carrot, red peper, tomato and any kind flower : dilution 500 times with water (40 ppm) spraying 3 time up to haverst
2121Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
NNoo
ProcessProcess Liquid Liquid phasephase
Solid phaseSolid phase
11
22
33
44
55
66
77
88
ChitosanChitosan
SolventSolvent
StandardizationStandardization
Handling of materialsHandling of materials
NeutralizationNeutralization
Irradiation CostIrradiation Cost
PreservationPreservation
TransportationTransportation
20 kg20 kg
Lactic AcidLactic Acid
Chemical : HChemical : H22OO22
Irradiation (25 kGy), Irradiation (25 kGy), Rp 200.000,-Rp 200.000,-
Special equipmentSpecial equipment
10 L, 1 M NaOH10 L, 1 M NaOH
Rp 4000.000,-/ batchRp 4000.000,-/ batchCo-60Co-60
Ag-Nano-ChitosanAg-Nano-Chitosan
DifficultDifficult
20 kg20 kg
Acetic acid (Also act as Acetic acid (Also act as anti bacteria)anti bacteria)
--
Simple, Plastic bagSimple, Plastic bag
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Rp 500.000,- /batchRp 500.000,- /batchCo-60, Electron BeamCo-60, Electron Beam
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EasyEasy
COMPARISON PROCES FOR PREPARATION OF IRRADIATED CHITOSAN COMPARISON PROCES FOR PREPARATION OF IRRADIATED CHITOSAN
(1000 l)(1000 l)
2222Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]
2323Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]