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Oasis Work Update-1
Oasis Work Update-1
2024-02-1
Set the gelatinization of starch with carrageenan.
Experiment 1
- Starch 5 g, carrageenan 5 g, calcium propanoate 1 g, glycerol 2.5 g, and water 100 mL was
mixed in a Erlenmeyer flask. The mixture was heated to about 100 C using water bath for
about 20 min and the starch became dissolved.
- The mixture was poured into the mole and gel was formed immediately.
Experiment 2
- Same composition as in Experiment 1.
- During heating, detergent was added to the mixture and vigorously stirred to make foam.
- When the temperature was low enough and the foam is about to set and not settle down, the
mixture was poured into the mole.
- Got white gel.
Experiment 3
- Same composition as in experiment 1 but more water is added (about 200 mL total volume)
- Generate the form as in Experiment 2.
- Got white gel.
Results:
This is the Photo of experiment set up.
After pouring into the mole and gel was generated.
จากข้อมูล
- Crosslink ที่เกิดจากการใช้คาราจิแนนจะไม่ค่อยดีและเหมาะสมที่จะเป็ น Floral foam เนื่องจาก
เป็ นการจับกันของสายโซ่คาราจิแนนแต่ละสายด้วยพันธะไอออนิกเท่านั้น ส่วนแป้งไม่ได้เกิด
ปฏิกิริยาอะไรต่อเลย แต่อาจจะมี Glycerol ที่เข้าไปเกิดพันธะ hydrogen แทรกอยู่ระหว่างสายโซ่
เท่านั้น นี่คือภาพแสดงการจับกันของ carrageenan
- นำมาสู่การใช้Crosslink ที่เป็ น ester จาก citric acid
การทดลอง
- ทำการ vary ปริมาณต่างๆ ตามตาราง
- Mix all solid component.
- Add water.
- Add Glycerol solution.
-Heat at about 80-90 C (water bath). About 15 min.
For the ex without carageenan, the product will be added to the tube for freeze dry.
Discussion
- เจลจะเกิดได้ดีและแข็งจะต้องมี carageenan
- in the presence of calcium propanoate and citric acid, there is smell of acid assumed to be propanoic
acid that get protonated to get its acid form and evaporated out from the mixture.
- In ex 1 and ex4 that have one CP or citric acid, respectively, there is not that bad smell.
- From the ex 3 and 4, there reason why ex 3 can form gel better might be because of the absence of
glycerol or the presence of CP.
- As seen in ex8, if Glycerol and citric acid were not included, the solution is more viscous indicated that
there might be more crosslink from using HCHO.
WS-24-033 _Oasis work
Try to form the crosslink between starch and citric acid first and then the crosslink carbohydrate
will blow with NaHCO3 and high temperature.
Component amount
Cassava starch 20 g
Glycerin 1 mL
Citric acid 4g
H2O 50 mL
Procedure:
- The ingredients from the above table were mixed together.
- Heat to about 100 C and then the viscous gelatin like material. This takes about 3-5 minutes
to complete. The starch suspension became more viscous and solid.
- Because the mixture contains citric acid, NaHCO3 can not be added. So, about 2 volumes of
EtOH was added and the solid was collected via filtration. The solid was blend with some
NaHCO3 which is used as a blowing agent at high temperatures. (NaHCO3 decomposes to
form CO2 at more than 80 C.)
- The material was put in the oven and the temperature was set to 150 C.
Result:
- The material can be expanded because of the generation of CO2 from heating. However, the
material is too hard and inside it is just empty space. So it is like a ball from blowing from the
inside not actually the foam.
- Some soy protein is blend with the material and put to the oven. The result is the same that
the material is very hard.
-
ลักษณะจะเป็ นเหมือนข้าวเกรียบกุ้งเหนียวๆ แข็งๆ และเมื่อโดนน้ำก็จะยุ่ย
Try to use diethyl ether and 30% H2SO4 as blowing agent. Still not OK
จากผลการทดลองพบว่าสามารถทำให้เกิดฟองได้เพราะ Et2O จุดเดือดต่ำ และเดือดเมื่ออุณหภูมิที่
สูงขึ้น แต่เนื่องจากในสารผสมแป้งมีส่วนประกอบที่เป็ นน้ำอยู่ด้วย ทำให้ฟองที่ได้ไม่จับตัวเป็ นของแข็งเมื่อ
ปล่อยให้เย็นลง และแน่นอนเมื่อนำมาจุ่มกับน้ำ มันก็ยุ่ยและเปื่ อยละลายหายไป แสดงว่าไม่ค่อยมี crosslink
เกิดขึ้นเท่าใดนัก
สรุปการทดลองการใช้แป้งสำหรับทำให้เป็ น foam
This is after remove water in the oven. Got white solid that is quite hard.
The solid is quite stable when adding to water.
This is the product after removal of the unreacted vinyl acetate. However, this still has some water.
I tried to use the modified starch solution with sawdust. I think the amount of saw dust is too much and
final material is still now stable enough when adding some water to it.
I tried to set the reaction again but in this case, sawdust was added in the process of polymerization.
I found that the polymerization did not proceed very well and a lot amount of the monomer left. I think
the radical initiator might be destroy by phenolic group in sawdust that prevent the reaction to proceed.
WS-24-037_Oasis work Crosslinking with vinyl acetate
Freeze dry
2024-03-13
The starch mixed with the mixture of polymerization of vinyl acetate was subjected to freeze
drying to remove water.
Procedure:
- In water 100 mL has starch 5 g, glycerin 0.5 mL.
- The mixture was heated at about 80 C to gelatinize the starch. This process was done within 10
min.
- 5 g of vinyl acetate + 10 mg of benzyl peroxided was slowly added to the solution under reflux
condenser because vinyl acetate has the boiling point lower than that of water.
- The reaction mixture was heated at about 80 C for 3 h. The reaction became more white because
of formation of acetylated starch and polyvinyl acetate.
- The reaction mixture was cooled down and the remove the volatile component (mainly vinyl
acetate) by rotavap.
- Put to the freezer O/N and freeze dry the samples
Results:
- The following pictures is the sample after freeze dry to get the starch foam.
- The foam has the texture similar to polystyrene foam that it soft but after pressing it with a
pointing material of fingernails, the foam does not turn back to the original shape and the mark
remained in its surface.
This property is just like the Oasis in the dried form.
-
-
-
-
-
-
Discussion:
- The chemical structure of the foam needs to be modified to reduced the water absorption.
WS-24-039 Oasis using gellan gum, xanthan gum
Sample Cassava starch Tween 85 Additive
1 5% 0.5% No additive
4 5% 0.5% Chitosan
Procedure:
- There are 4 samples for this experiment as listed in the above table. The total volume is 20 mL.
The solution was prepared in falcon tubes.
- The samples were heated at about 90 C to let the starch gelatinized.
- The samples were cooled down to room temperature and put in the freezer -20 C for O/N.
- The samples were lyophilized for 2 days to get foam.
Results:
- The freeze dry process took two days to complete. There is still some water in the sample after 1
day.
The results after freeze drying
- I preliminarily tested PU foam B (PU-B) with starch suspension. At first I tried to gelatinize the
starch first but it is difficult to mix with PU-B because of the hard texture of gelatinized starch.
To do this, I need to increase the concentration of starch, not to have too much water because PU-
B is an isocyanate that it can react with water to form CO2 used for foaming agent. If there is too
much water, there will not be isocyanate groups left for doing crosslinking.
However, the first attempt was to directly mix the PU-B with the starch suspension, there is no
reaction because the absence of an amine catalyst.
- I then added some amount of catalyst (Et3N) to the mixture and the reaction occurred
-
- I increased the amount of Et3N and got the reaction occurring faster.
- For this experiment, the texture of Starch-PU foam is not rigid and broken so easily when
removed from the flask. However, the foam cannot be dissolved in water just like starch. So, the
crosslink reaction has changed the property of starch.
WS-24-041 Oasis using PU foam 2
2024-03-24
(The amount of the solvent There is no foam forming just like the first
2 and catalyst is increased) experiment.
Starch 6 g
The order of adding the ingredient might not be
1:1 H2O/PEG 10 mL suitable.
PU-B 10 mL
Mix and start the reaction
by adding
Et3N 200 uL
(The addition order was There is still no foam forming in the reaction.
3 changed)
This might be because the two phases, water and
PU-B are not mixed well so that the reaction can
Starch 6 g
not occur efficiently.
1:1 H2O/PEG 10 mL
Et3N 200 uL
During the reaction, we tried to add some Tween
Mix and start the reaction 85, acting as emulsifier, into the reaction mixture.
by adding We found that the reaction took place and CO2 gas
was generated immediately.
PU-B 10 mL
(Change the solvent by The gas was generated much more amount when
4 adding emulsifier) comparing to the previous experiments.
Starch 6 g
However, the material did not expand well and
1:1 H2O/PEG (5% after for a while, there was some moisture in the
Tween85) 10 mL product.
Et3N 200 uL
This could indicate that the amount of water is too
Mix and start the reaction
much that kill the isocyanate group preventing the
by adding
crosslink reaction.
PU-B 10 mL
(Reduce the amount of The formation of the foam was much better.
5 water)
Starch 6 g
1:2 H2O/PEG (5%
Tween85) 10 mL
Et3N 200 uL
Mix and start the reaction
by adding
PU-B 10 mL
Experiment 6 (Sorbitol)
- Sorbitol 6 g
- 1:2 H2O/PEG (5% Tween85) 10 mL
- Heat until sorbitol was dissolved to get a clear solution and cool down.
- Et3N 200 uL
- Mix and start the reaction by adding PU-B 10 mL
- Results: The foam texture is just like sponge. It can be cut by a knife.
However, the water absorption is not suitable for being floral foam yet.
o
o
Experiment 2 (Add CMC)
- Sorbitol 15 g
- 1:2 H2O/PEG (5% Tween85) 10 mL
- Heat until sorbitol was dissolved to get a clear solution and cool down.
- CMC 0.4 g (Slowly add. This is the minimum CMC amount. If too much CMC, the texture will
be too hard)
- Et3N 200 uL
- Mix and start the reaction by adding PU-B 10 mL
- Results:
o The foam is softer than the one having sorbitol alone even though the amount of sorbitol
is the same.
o This one can absorb water better than not including CMC but still not suitable for being
Oasis.
o The problem is how to add more CMC.
-
WS-24-043 Oasis using PU foam 4
2024-03-28
Partial hydrolysis of starch at room temperature and slightly heating the starch suspension.
(Cassava starch 100 g + water 100 g + H2SO4 1 mL)
No further experiments
WS-24-044 Oasis using PU foam 5
2024-03-31
Experiment 1 (KCl)
- Sorbitol solution 25 g
- KCl 5 g
- Et3N 200 uL
- *** In this experiment, after mixing those ingredients above together, the mixture was crashed
out to be solid and can not be mixed with the PU-B in the next step.
Try to form the crosslink between starch and citric acid first and then the crosslink carbohydrate
will blow with NaHCO3 and high temperature.
Component amount
Cassava starch 20 g
Glycerin 1 mL
Citric acid 4g
H2O 50 mL
Procedure:
- The ingredients from the above table were mixed together.
- Heat to about 100 C and then the viscous gelatin like material. This takes about 3-5 minutes
to complete. The starch suspension became more viscous and solid.
- Because the mixture contains citric acid, NaHCO3 can not be added. So, about 2 volumes of
EtOH was added and the solid was collected via filtration. The solid was blend with some
NaHCO3 which is used as a blowing agent at high temperatures. (NaHCO3 decomposes to
form CO2 at more than 80 C.)
- The material was put in the oven and the temperature was set to 150 C.
Result:
- The material can be expanded because of the generation of CO2 from heating. However, the
material is too hard and inside it is just empty space. So it is like a ball from blowing from the
inside not actually the foam.
- Some soy protein is blend with the material and put to the oven. The result is the same that
the material is very hard.
-
ลักษณะจะเป็ นเหมือนข้าวเกรียบกุ้งเหนียวๆ แข็งๆ และเมื่อโดนน้ำก็จะยุ่ย
Try to use diethyl ether and 30% H2SO4 as blowing agent. Still not OK
จากผลการทดลองพบว่าสามารถทำให้เกิดฟองได้เพราะ Et2O จุดเดือดต่ำ และเดือดเมื่ออุณหภูมิที่
สูงขึ้น แต่เนื่องจากในสารผสมแป้งมีส่วนประกอบที่เป็ นน้ำอยู่ด้วย ทำให้ฟองที่ได้ไม่จับตัวเป็ นของแข็งเมื่อ
ปล่อยให้เย็นลง และแน่นอนเมื่อนำมาจุ่มกับน้ำ มันก็ยุ่ยและเปื่ อยละลายหายไป แสดงว่าไม่ค่อยมี crosslink
เกิดขึ้นเท่าใดนัก
สรุปการทดลองการใช้แป้งสำหรับทำให้เป็ น foam
2024-04-03
Stock Solution
- 1:2 H2O/PEG (+ 5% Tween85) 150 mL
2024-04-04
Adding glycerol (+Varying the concentration of glycerol) to increase the foam’s water absorption ability.
Stock Solution
- 1:2 H2O/PEG (+ 5% Tween85)
Lock the proportion of water and vary the proportion between Glycerol : PEG
** linear = เหนียวขึ้น so adding glycerol (3 arms of OH) makes more branches and makes the foam more
hard and crumbly.