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Republic of the Philippine

BATANGAS STATE UNIVERSITY


BatStateU Alangilan
Alangilan, Batangas City
College of Engineering, Architecture, and Fine Arts
https://batstate-u.edu.ph/, Tel No. (043) 425-0139 loc. 118/2121

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

October 20, 2021

DR. REYNATO A. GAMBOA


Dean, CEAFA
This University

Dear Sir:

Greetings of Peace!

The undersigned are 4th-year Chemical Engineering students of Batangas State University who
are currently conducting the thesis entitled “Electrical Insulating Epoxy-based Composite Reinforced
by Cellulose Nanofibers Derived from Carrot Peel Waste”. This research aims to recycle and reuse
agricultural losses such as carrot peel wastes and contributes to the development and enhancement
of the components used for power transmission systems.

We would like to request your good office to allow us to conduct the experiment utilizing the
materials and equipment available in the Unit Operations and Chemical Engineering Laboratory
with the supervision of their Thesis Adviser. The experiment will be conducted on the following
dates:

Date Time
October 28, 2021 8:00 AM - 5:00 PM
November 3, 2021 8:00 AM - 5:00 PM
November 16, 2021 8:00 AM - 5:00 PM
November 22, 2021 8:00 AM - 5:00 PM
December 6, 2021 8:00 AM - 5:00 PM
December 7, 2021 8:00 AM - 5:00 PM
December 9, 2021 8:00 AM - 5:00 PM

The following materials and equipment will be the ones to be requested for use in the conduct
of the said experiment. Attached is the procedure of the experiment for validation.
1. Oven 6. Graduated Cylinder 10. Erlenmeyer Flask
2. Analytical Balance 7. Hot plate 11. Centrifuge
3. Pipette 8. Mechanical 12. Desiccator
4. Fume Hood Balance 13. Vacuum pump
5. Beaker 9. Mechanical Stirrer 14. Ultrasonic Bath

Rest assured that we will take good care of the equipment that we will be using and ensure the
cleanliness of the laboratory adhering to the safety policies of the laboratory. With the approval of
this request, completing the experiment intended for the completion of the research study will be
possible. Thank you and God bless.

Respectfully yours,

BUNQUIN, MARIA ROSELYN N. HERNANDEZ, KRIZZETE M.


Proponent Proponent

MACATANGAY, LAYRA ALEXIS MACATANGAY, RICHMOND RAFAEL C.


Proponent Proponent
Republic of the Philippine
BATANGAS STATE UNIVERSITY
BatStateU Alangilan
Alangilan, Batangas City
College of Engineering, Architecture, and Fine Arts
https://batstate-u.edu.ph/, Tel No. (043) 425-0139 loc. 118/2121

Noted by:

ENGR. NANETH J. AGUADO


Thesis Adviser

Recommending Approval:

ENGR. RHONALYN V. MAULION ENGR. REJIE C. MAGNAYE


Program Chair, ChE/FE Department Department Head, ChE/FE

Approved by:

DR. REYNATO A. GAMBOA


Dean, CEAFA
Republic of the Philippine
BATANGAS STATE UNIVERSITY
BatStateU Alangilan
Alangilan, Batangas City
College of Engineering, Architecture, and Fine Arts
https://batstate-u.edu.ph/, Tel No. (043) 425-0139 loc. 118/2121

PROCEDURE
Drying (October 28)
The carrot peels will be dried in the oven to remove moisture content for easier
isolation of fibers.

Bleaching (November 3)

Following alkali treatment, the samples will be bleached with acetate buffer (which is
27 g NaOH and 75 mL glacial acetic acid diluted to 1 L distilled water) and aqueous NaClO
(1.7 wt%). The bleaching process will be repeated two times to remove the lignin and
hemicellulose and until the color of the bleached sample appeared to be white.

Drying (November 16)

The carrot peels will be dried in the oven to remove moisture content for easier
isolation of fibers.

Bleaching (November 22)

Following alkali treatment, the samples will be bleached with acetate buffer (which is
27 g NaOH and 75 mL glacial acetic acid diluted to 1 L distilled water) and aqueous NaClO
(1.7 wt%). The bleaching process will be repeated two times to remove the lignin and
hemicellulose and until the color of the bleached sample appeared to be white.

Ultrasonic Fibrillation (December 6)

The chemically filtered and purified cellulose fibers (PCFs) extracted from carrot peel
wastes will be then soaked in distilled water (1% by weight). The cellulose suspensions that will
be obtained will be then sonicated for 30 min using an ultrasonic processor specifically an
ultrasonic bath to isolate the cellulose nanofibers. The ultrasonic treatment will be carried out
in an ice bath to prevent overheating.

Surface Modification of Isolated Cellulose Nanofibers (CNFs) (December 7)

Before the modification process, the cellulose nanofiber (2% w/v) derived from carrot
peels will be added with NaOH solution until the pH level reaches 10. To initiate the
modification, cetyltrimethylammonium chloride (CTAC) will be applied and mixed to the
samples as a cationic surfactant. The modification of the CNF’s surface will begin by putting
together the 2% w/v CNF and 2% cetyltrimethylammonium chloride (CTAC) drop by drop in
a ratio of 1:4. During this process, the temperature will be maintained at 60±5°C for 180
minutes. Then, this will continue at room temperature for 12 hours. And then, it will be subject
to a 2 times centrifugation process for 20 mins, at 4600 rpm to remove excess NaOH and CTAC.
Republic of the Philippine
BATANGAS STATE UNIVERSITY
BatStateU Alangilan
Alangilan, Batangas City
College of Engineering, Architecture, and Fine Arts
https://batstate-u.edu.ph/, Tel No. (043) 425-0139 loc. 118/2121

Production of Cellulose Nanofiber Reinforced Epoxy-based Electrical Insulating


Composites (December 9)
The isolated cellulose nanofiber from carrot peel wastes will be used as filler or
reinforcement in epoxy-based electrically insulating composite. Epoxy resin and epoxy curing
agent/hardener will be mixed as a matrix. Electrically insulating composite will be fabricated
using different cellulose nanofiber loading percentages of 0%, 0.5%, 0.7%, and 0.9% (w/w).
The cellulose nanofiber will be then added to the epoxy resin mixture at different concentrations
and stirred by using a mechanical stirrer for 30 minutes at room temperature. Bubbles from the
mixture will be removed by using a vacuum chamber for 30 minutes. Afterward, the epoxy
curing agent will be added to the mixture and then, it will be mechanically stirred for 10 minutes.
The mixture will be degassed again in the vacuum chamber for 15 minutes. Then, the solution
that will be obtained in this procedure will be cast into a mold. It will be then covered with
silicon oil as a releasing agent. Finally, the insulating composite will be cured at 85°C for 120
minutes and will continue for post-cure at 125°C for 180 minutes.
Republic of the Philippine
BATANGAS STATE UNIVERSITY
BatStateU Alangilan
Alangilan, Batangas City
College of Engineering, Architecture, and Fine Arts
https://batstate-u.edu.ph/, Tel No. (043) 425-0139 loc. 118/2121

SUMMARY OF PLAN OF ACTIVITIES

DATE ACTIVITIES

 Oven-drying of Carrot Peels


- Washing, cutting, and weighing carrot peel wastes
- Soaking into a sodium metabisulfite
- Oven drying for 6 hours at 80±5 °C
 Weighing of reagents
October 28,
- 175 grams of NaOH for pre-treatment
2021 - 17 grams of NaClO
- 20 grams of NaOH for alkali treatment
- 27 grams of NaOH for acetate buffer
 Transferring liquid reagents using a pipette
- 75 mL of HCl for acid hydrolysis
- 75 mL of acetic acid for bleaching

 Bleaching
 27 g NaOH and 75 mL glacial acetic acid diluted to 1 L distilled water for
acetate buffer
November  1.7 wt% aqueous NaClO as a bleaching agent
3, 2021  Mixing of acetate buffer and bleaching agent
 2 times pulp bleaching process at 70 °C for 1 hr

 Oven-drying of Carrot Peels (Batch 2)


- Washing, cutting, and weighing carrot peel wastes
- Soaking into a sodium metabisulfite
- Oven drying for 6 hours at 80±5 °C
 Weighing of reagents
November 16,
- 175 grams of NaOH for pre-treatment
2021 - 17 grams of NaClO
- 20 grams of NaOH for alkali treatment
- 27 grams of NaOH for acetate buffer
 Transferring liquid reagents using a pipette
- 75 mL of HCl for acid hydrolysis
- 75 mL of acetic acid for bleaching
 Bleaching
 27 g NaOH and 75 mL glacial acetic acid diluted to 1 L distilled water for
November 22, acetate buffer
2021  1.7 wt% aqueous NaClO as bleaching agent
 Mixing of acetate buffer and bleaching agent
 2 times pulp bleaching process at 70 °C for 1 hr
 Ultrasonic Fibrillation of CNF
December 6, - Sonicating for 30 min using an ultrasonic bath
2021 - Done in an ice bath to prevent overheating
 Surface Modification of CNF
- Modifying with cetyltrimethylammonium chloride (CTAC) as
December 7, a cationic surfactant
2021 - Mixing 2% w/v CNF and 2% cetyltrimethylammonium
chloride (CTAC) drop by drop in a ratio of 1:4
- Mixing at 60±5°C for 180 minutes
Republic of the Philippine
BATANGAS STATE UNIVERSITY
BatStateU Alangilan
Alangilan, Batangas City
College of Engineering, Architecture, and Fine Arts
https://batstate-u.edu.ph/, Tel No. (043) 425-0139 loc. 118/2121

 Continuation: Surface Modification of CNF


- Subjecting to a 2 times centrifugation process for 20 mins at
4600 rpm
 Production of CNF-reinforced Composite
December 9, - Fabricating using different cellulose nanofiber loading
percentages of 0%, 0.5%, 0.7%, and 0.9% (w/w)
2021
- Mixing epoxy resin with a mechanical stirrer for 30 minutes at
room temperature
- Removing bubbles by using a desiccator with a vacuum pump
for 30 minutes
- Curing at 85°C for 120 minutes
- Post-curing at 125°C for 180 minutes

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