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DEMONSTRATION OF LARGE DEMONSTRATION OF LARGE SCALE PRODUCTION OF OLIGO SCALE PRODUCTION OF OLIGO CHITOSAN CHITOSAN GATOT TRIMULYADI REKSO GATOT TRIMULYADI REKSO E-mail: [email protected] E-mail: [email protected] CENTER FOR THE APPLICATION OF ISOTOPE CENTER FOR THE APPLICATION OF ISOTOPE AND RADIATION TECHNOLOGY AND RADIATION TECHNOLOGY NATIONAL NUCLEAR ENERGY AGENCY NATIONAL NUCLEAR ENERGY AGENCY (Augustus 4th – 8 th - 15th, 2008) 1 Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected] email:[email protected]

Pilot plant oligo chitosan-dr gatot trimulyadi

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GATOT TRIMULYADI REKSOE-mail: [email protected] FOR THE APPLICATION OF ISOTOPE AND RADIATION TECHNOLOGYNATIONAL NUCLEAR ENERGY AGENCYDEMONSTRATION OF LARGE SCALE PRODUCTION OF OLIGO CHITOSAN

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Page 1: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 2: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 3: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 4: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 5: Pilot plant  oligo chitosan-dr gatot trimulyadi

6050403020100

1600

1400

1200

1000

800

600

400

200

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

1200

1000

800

600

400

200

0

Irradiation Dose (kGy)

Vis

co

sit

y (C

ps

)

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]

Page 6: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 7: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 8: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 9: Pilot plant  oligo chitosan-dr gatot trimulyadi

During mixing processDuring mixing process

99Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]

Page 10: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 11: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 12: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 13: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 14: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 15: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 16: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 17: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 18: Pilot plant  oligo chitosan-dr gatot trimulyadi

PACKINGPACKING

1818Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]

Page 19: Pilot plant  oligo chitosan-dr gatot trimulyadi

1919Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]

Page 20: Pilot plant  oligo chitosan-dr gatot trimulyadi

At Nippon Express Indonesia, CengkarengAt Nippon Express Indonesia, Cengkareng2020

Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]

Page 21: Pilot plant  oligo chitosan-dr gatot trimulyadi

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]

Page 22: Pilot plant  oligo chitosan-dr gatot trimulyadi

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

--

Rp 500.000,- /batchRp 500.000,- /batchCo-60, Electron BeamCo-60, Electron Beam

--

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]

Page 23: Pilot plant  oligo chitosan-dr gatot trimulyadi

2323Dr.Ir.Gatot Trimulyadi Rekso- Dr.Ir.Gatot Trimulyadi Rekso- email:[email protected]:[email protected]