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Characterization of natural rubber cup coagula

maturation and its effect on dry rubber properties

Jutharat Intapun

Prof. Eric Dubreucq, Assoc. Prof. Dr.Varaporn Tanrattanakul,


Dr. Laurent Vaysse, Dr. Jérôme Sainte-Beuve, Dr. Frédéric Bonfils
Introduction
• Natural rubber (NR) is one of the major exported
products of Thailand.
• Standard Thailand Rubber (STR), STR 20
• Raw materials : field coagula
• Low consistency of the delivered raw material
Scope of work
Physico-chemical environment
-temperature
- oxygen content
-relative humidity

Maturation during storage


Biochemical Reactions
(microorganisms, enzyme)

Consequences on
dry rubber properties?
Po, PRI and
mesostructure
Objective
1. Characterization of industrial maturation conditions

2. Scaling down : labscale maturation box and


mini-process

3. Effect of microorganisms on cup coagula properties


Experimental
1. Characterization of industrial
coagula pile maturation

1.1 Maturation conditions inside cup


coagula pile

1.2 Cup coagula properties


Drilled stainless steel tubes
(external diameter 5.1 cm, thickness 2mm, 5mm-diameter holes,
3000 holes/m2)

7m
3m
Cup coagula pile

20m

depth
0cm
RH %
Temp °C
50cm
3m 100cm Digicon HT765232
Humidity/temperature
20cm 150cm meter

200cm
probe

Figure1. Coagula maturation pile equipped with two drilled stainless steel tube
10kg

Delivery day 10 kg
baskets
0 cm
10kg Creping of 10 kg Drying of crepe
50 cm 10kg sample

100 cm 10kg

150 cm 10kg
Po,
Po PRI and
200 cm 10kg mesostructure

Processing After 24 days

Figure 2. Cup coagula sampling for rubber properties determination


2. Scaling down : mini-process
and labscale maturation box
2.1 Setting up of the mini-process
Aim:
Setting up a mini process leading to a dry
rubber with properties comparable with
the one produced by industrial process
Adjusted parameters :
1. Number of passes in mini-creper
2. Temperature and duration of drying
Sampling 10kg
of cup coagula
Drying in Lab
120°C, (2,2.5,3h)
Industrial Creping Or 125°C, (2,2.5,3h)
130°C, (1.25,1.5,2h)
Minicreper Creping

6 passes +7,11,12, or 16 passes

Drying in Factory
129°C, 3h

21 passes
Figure 3. Cup coagula Processing
2.2 Maturation device at labscale
factory pile maturation
-conditions
-rubber properties

Factory to laboratory

laboratory maturation
- Monoclonal coagula
-T°, RH, O2 controlled and
recorded
3. The effect of micro-organisms on cup
coagula properties
Clean Latex
- Microorganisms controlled
by antibiotic adding or
various inoculum added

A:inoculum B:inoculum C:antibiotic


adding (Acid
(Auto coag.) (Acid coag.) coa.
Coagula Coagula Coagula

Maturation boxes
At 40C for 34
days

Processing and measure of properties


Results and
discussion
Results and discussion

1. Industrial coagula pile maturation

1.1 Physico-chemical parameters


50 100 20
(a)
90 (c)
45

Relative humidity (%)

Oxygen content (%)


80 15
Temperature ( C)
o

40
70
35 60 10
50
30
40 5
25 (b)
30
20 20 0
0 50 100 150 200 0 50 100 150 200 0 50 100 150 200
Depth of coagula pile (cm)
Depth of coagula pile (cm) Depth of coagula pile (cm)

Figure 4. Temperature, Relative humidity and oxygen content with depth of the pile
Measurements were performed at 8 AM ( ), 12 AM ( ) and 4 PM ( )
1.2 Properties of cup coagula from maturation pile
Po (Po Unit)
PRI (%)
0 5 10 15 20 25 30 35 40 45
0 5 10 15 20 25 30 35 40 45 50

0 25.9
0 25.9

31.3
Depth of pile (cm)

-50 21.1

Depth of pile (cm)


-50

-100 36.9 -100 36.5

-150 38.7 -150 41.6

-200 41.6 -200 45.8

Gel (% w/w) Mw (kg/mol)


25 30 35 40 45 50 55 600 700 800 900 1000 1100 1200 1300 1400 1500

0 41.0 0 869.7
Depth of pile (cm)

42.5 1038.2

Depth of pile (cm)


-50 -50

-100 47.3 -100 1158.3

-150 51.1 -150 1439.7

-200 -200 1458.7


50.6

Figure 5. Po, PRI, Gel content and Molar mass of cup coagula with depth of the pile
Results and discussion

2.1 Scaling down : the mini-process condition

in laboratory
Results and discussion

Sampling 10kg Drying in


Drying in Lab
Lab
of cup coagula 120°C, (2,2.5,3h)
Or 125°C, (2,2.5h,3h)
125oC for 2 hr
Industrial Creping 130°C, (1.25,1.5,2h)
Minicreper Creping

6 passes 1616passes
+7,11, and 18 passes

Drying in Factory
129°C for 3hr

21 passes
50

45

40
Po (median)

35

30

25

20

120-2 120-2.5 120-3 125-2 125-2.5 130-1.25 130-1.5 control

Drying conditions

Po and PRI of cup coagula under various processing conditions


35

30

25
PRI

20

15

10
120-2 120-2.5 120-3 125-2 125-3 control
125-2.5
Drying conditions
2.2 Scaling down : Maturation boxes

Nitrogen Tank Dry Air

Maturation box

Humid air Data logger

Figure 6. Maturation device in Laboratory


3. Cup Coagula after maturation in
labscale device
A. Physical aspect

Microorganisms Microorganisms Microorganisms (killed)


No formic acid Formic acid Formic acid
No antimicrobial agent No antimicrobial agent Antimicrobial agent
(A) (B) (C)
B. Initial Plasticity P0 and PRI of cup coagula
60 60 50
(A) (B) (C)

Po (red) P30 (green)

Po (red) P30 (green)

Po (red) P30 (green)


50 50 40
40 40
Po 30
30 30

P0 / P30
20
20 20
10
10 P30 10

0 0 0
0 4 15 28 34 0 4 15 28 34 0 4 15 28 34

maturation time (days) maturation time (days) maturation time (days)

125 125 125

100 100 100

75 75 75
PRI

PRI

PRI
50 50 50

PRI 25 25 25

0 0 0
0 4 15 28 34 0 4 15 28 34 0 4 15 28 34

maturation time (days) maturation time (days) maturation time (days)

Microorganisms Microorganisms Killed microorganisms


No formic acid formic acid formic acid
No antimicrobial agent No antimicrobial agent Antimicrobial agent
110
With antibiotic
100
90
80
Effect of
70
60 microorganisms on
PRI

50
40
30 PRI
20
10
With micro-organism
0
N+F+M+ N+F+M- N-F+M+ N-F-M+ Each Pair
Student's t
code 0.05

Effectof microorganisms initial concentration on PRI

120.0
3x104 CFU/ml
The drop of PRI is 100.0

proportional to the
initial quantity of 5x105 CFU/ml
80.0

PRI

microorganisms in 60.0 PRI Na azide (3E+4 cfu/ml)


2x10 CFU/ml
6 PRI Clean (5E+5 cfu/ml)
latex 40.0
PRI M (2E+6 cfu/ml)
PRI 2M (9E+6 cfu/ml)
PRI 4M (2E+7 cfu/ml)
20.0
2x107 CFU/ml

0.0
0 1 2 3 4 5 6
Maturation time (days)

Figure 7. The effect of microorganism activity on cup coagula properties


Conclusions (1)

1.Characterization Maturation conditions


• Temperature and relative humidity of the air
increased with depth. In contrast, oxygen
content of the air within the pile decreased
as depth increased.

• Initial plasticity (P0), plasticity retention


index (PRI), gel content and Mw were higher
at the bottom of the pile.
Conclusions (2)

2. Setting up of the maturation box and


mini-process

• Crepping : 16 passes on mini-creper

• Drying : 2 hr at 125°C
Conclusions (3)

3. The role of micro-organism on cup


coagula properties
• Po, PRI decreased with microorganism
content and maturation time (antibiotic
prevent those drops)
• It was proven that the drop of PRI was
proportional to initial quantity of
microorganisms in the latex
Perspectives
1. Identify precisely the mode of action of
this microorganisms during maturation :
pure enzyme testing, isolation and test of
specific strains
2. Study the microbial activity and its effect
on rubber properties under various
controlled conditions
3. Recommandations to improve the
maturation on industrial site
Thank you for your
attention

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