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Synthesis of Cellulose Acetates from banana (Musa acuminata) Fiber

Jennelie E. Caya, and Zailla P. Flores

Abstract

Cellulose diacetate (CA) and cellulose triacetate (CTA) are two of the most industrially utilized derivatives of cellulose. Recent studies have demonstrated the potential of electrospun CA nanofiber membrane - a nonwoven texttile material, for biomedical applications including tissue engineering and nutraceutical delivery. In this study, CA and CTA were produced from local banana (Musa acuminata) fibers extracted from the banana pseudo-stem. The esterificationreaction of the cellulose pulp from banna fiber was carried out with acetic acid and acetic anhydride with the aid of sulfuric acid. The yield of the oven dried product and degree of substitutions (DS) are 62.08% and 70.04 %, 2.44 and 3.15 for CA and CTA, respectively. fourier transform infrared (FTIR) spectra indicate the succesful introduction of an acetyl group the cellulose backbone as evidenced by the presence of carbonyl stretch at around 1700 cm -1 for the esterified products. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) revealed the thermal stability of the CA, having more hydroxyl groups, is a Thermally more stable derivative.

 

β-Cyclodextrin Microencapsulation of Peppermint (Mentha piperita) Essential Oil for Antibacterial Finishing of Cotton Fabrics

C. Abendanio, L. Labaclado, E. Manalang, and J. Leaño, Jr.

Abstract

β-cyclodextrin (β-CD) microcapsules containing peppermint (Mentha piperita) oil were prepared via co-precipitation method using the optimized β-cyclodextrin-oil mass ratio and stirring time of 3:1 and 8 h, respectively. DSC analysis confirmed effective encapsulation of the peppermint oil as evidenced by the disappearance of an exothermic peak in the thermogram of the microcapsules which was observed in the thermogram of the pure peppermint oil. The FTIR spectra of the β-CD-oil microcapsule showed major peaks corresponding to O-H (3220-3500 cm-¹), C-H (2927 cm-¹) and C-O (1150), which were identical to that of pure β-CD. It also showed that the characteristic peaks of the peppermint oil are no longer observed in the spectra of the microcapsules. The SEM images revealed the sizes of the microcapsule to be in the range of 1-20 µm and the structures are cube-like. The microcapsules were applied on knitted cotton via pad-dry cure method with 1,2,3,4-butanetetracarboxylic acid (BTCA) as cross -linking agent. SEM analysis of the treated fabrics showed the presence of microcapsules on the fabric. Further, FTIR spectra of the treated cotton showed peaks around 1716 cm-1, corresponding to an ester carbonyl formed between BTCA and cotton and BTCA and microcapsules proving effective cross-linking. The use of BTCA enhances the scent retention of the microcapsules. Antibacterial property assessment (AATCC 147-2004: Parallel Streak Method) showed that the treated fabrics did not exhibit antibacterial activity which was construed as a proof of the effective encapsulation of the antibacterial peppermint oil that was protected by the β-CD capsule. Durability to laundering was assessed, and the results revealed that washing enhances antibacterial activity of the treated fabric due to facilitated rupture of β-CD microcapsules, hence release of the peppermint oil and thus the observed scent and antibacterial activity. Further, the synergistic effect of BTCA in cross linking and stabilizing the microcapsules was also observed.

 

Cellulose Nanocrystals (CNCs) from Abacá (Musa textilis Nee)

Joshua DQ. Olindan, Benson A. Roxas, Regina S. Gatmaytan, Julius L. Leaño Jr.

Abstract

Cellulose nanocrystals (CNC's) were isolated from abaca (Musa textilis Nee) fibers through sulfuric acid (H2SO4) hydrolysis. One-bath scouring and bleaching method performed three tomes yielded 98.89% total cellulose content which is suitable for the production of cellulose nanocrystals. From a series of trial isolation of CNCs, hydrolysis condition (acid concentration, acid-to-fiber ratio and temperature) was optimized at 50 % H2SO4, 20 mL acid per gram of fiber at 24°C. Hydrolysis time of scoured/bleached abaca fibers was performed from 30 - 180 min optimum time of CNC isolation (CNC90). Infrared spectra of raw abaca fibers (RAF), scoured/bleach abaca fibers (SBAF) and CNC90 were evaluated and decrease in the peaks associated with lignin and hemicelluloses was noted SBAF and CNC90 proving sufficient removal of said components. Morphological properties of the RAF and SBAF microfibrils after purification were observed through SEM imaging. The X-ray diffraction patterns confirmed the presence of crytalline domains in the cellulose. Crystallinity Index (Crl) values were calculated for RAF, SBAF, CNC60, CNC90, CNC120 and CNC180 with CNC90 exhibiting the highest crystallinity region of 74.21%. The further decrease in Crl values at prolonged hydrolysis time of 120 and 180 min indicated the destruction of the crystalline phase of cellulose. Hence, the optimum hydrolysis of SBAF was effective in isolating cellulose with particle sizes in the nanometer range (at least one dimension equal or less than 100 nm). Particle sizes of the isolated nanocrystals decreased with longer acid hydrolysis with an average length of 110.50 nm and width of 19.48 nm for CNC90.

 

Spent Liquor for Degumming Pineapple (Ananas comosus Linn.) Fiber

Eduardo M. Marin

Abstract

The PTRI established degumming condition for pineapple was used in the first batch degumming of pineapple fiber. Spent liquor of sodium hydroxide was collected, measured and made-up to its original alkaline strength and volume and was used for second batch degumming. Same procedure was followed for the spent liquor from second batch degumming which was utilizedfor third batch degumming. Degummed fibers were analyzed for their physical and chemical properties to assess the effect of using spent liquor for degumming. Results showed that made-up solutions from spent liquor were as effective as the original solution as far as gum removal is concerned. Moisture content and total cellulose of the fibers degummed with new solution and spent liquor are also comparable. Utilization of spent liquor for second and third batch degumming resulted to lower chemical inputs and consequently, reduced waste, thereby reducing the processing and wastewater treatment costs.

 

Small-Scale Natural Fiber Degumming Machine

Ronald S. Pechera and Roberto O. Casero

Abstract

The invention relates to a simplified degumming machine that can process one to five kilograms of natural fibers such as pineapple, abaca, and banana, simulating the PTRI established technology without eliminating the degumping parameters of pressure, volume and temperature as customarily applied in the pilot scale processing. This invention can also be utilized as dyeing vessel for texttile-based micro enterprises. The machine consists of two stainless steel tanks using a closed system for complete circulation and penetration of chemical solution and through rinsing of the fibers. Heat source is provided by burners for the degumming and rinsing purposes and all accessories are placed in a movable platform for ease of transfer. Processing of natural fibers is simplified and made less laborious with the aid of a pump and gate valves for liquid circulation and another gate valve for the transfer of liquids from stock tank to the main tank. Improvements were noted in processing time of 36.5%for the three fibers, increase in fiber recovery of 2.8% for pineapple, 2.5% for abaca and 2.2% for banana. A reduction of residual gum by 22.4%, 13.9% and 20.7% and fineness property improved by 7.9%, 10.6% and 8.12% for pineapple, abaca and banana, respectively. Tensile strength was significantly improved for pineapple and reduced for abaca and banana, all within the desired range if tensile strength of natural fibers for textile application at 23 to 30 Kgf for pineapple, 29 to 38 KGf for abaca and 19 to 30 Kgf for banana.

*Note:
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Color Quality and Colorfastness of Textiles Dyed Using Young Cocos nucifera (Coconut) Husk with Copper Sulfate-Alum Mordant System

Julius L. Leaño Jr.

Abstract

Crude aqueous extract of young coconut (Cocos nucifera) husk was used to dye fabrics made of Musa Textilis (Abaca), knitted cotton, Ananas comosus (pineapple), pineapple-silk, fine (21D) silk and coarse (360D) silk. Colorimetric evaluation revealed that generally alum lightens the color, while CuSO4 tends to darken it. The use of CuSO4/alum mordant system revealed the almost equal influence of each mordant in the resulting L value except in the case of fine silk and M. textilis fabrics where the darkening effect of CuSO4 predominated. Incremental changes caused by varying the mordants were observed in the corresponding a and b values. Higher color strength, K/S values were obtained on fabrics using alum mordant compared to pure CuSO4 or their combination. Further, colorfastness to laundering (AATCC 61-2003) ratings are in the range of 3-4, although predominantly, the laundered samples all turned darker and qualifying the observed change not due to fading but to darkening. The corresponding staining ratings were in the range of 3.5-4.5 using multi-fiber No. 1. The colorfastness to perspiration (AATCC 15-2002) ratings were in the range of 3.5-4.5 with observed yellowing. The staining ratings were in the range of 3-4.5, but ratings of 2 were mostly on cotton mordanted with CuSO4. All the other ratings of the dyed fabrics comply with the minimum staining ratings specified by Oeko Tex 100. The use of CuSO4/alum mordant system further diversified the colorway of C. nucifera as it generally maintained the performance of the dyed fabrics compared when using either pure 5% CuSO4 or 5% alum as mordants.

 

Simple and Effective UV-assisted Synthesis of Silver Nanoparticles in Polymethacrylic Acid

Evangeline Flor P. Manalang and Jeannie Lynn J. Cabansag

Abstract

A simple, inexpensive, and intrinsically non-toxic method of preparing silver nanoparticles via UV- include reduction of silver ions using polymethacrylic acid (PMA) is reported. Parameters such as source of radiation, concentrations of AgNO3 and PMA and duration of irradiation were optimized to establish a technique of synthesizing silver nanoparticles with minimized aggregation. The radiation sources, mechanical action, reactant concentration, and irradiation time have significant effect on the preparation of Ag NPs; and they can be varied to control its size, shape and distribution. Results revealed that 10:1 millimolar ratio of AgNO3 and PMA and 1 h UV irradiation using 8 W UV C lamp with continuous stirring are the optimized condition for the preparation of Ag NPs. Using the optimized parameters, characteristic SPR band at 430 nm wavelength was observed via UV-Vis spectroscopic technique. This confirmed the effective conversion of Ag+ to Ag0 and the formation of spherical Ag NPs with minimized agglomeration. This method has great potential for scaled-up production of Ag NPs for various industrial applications.

 

Synthesis and Grafting of Monochlorotriazinyl-?-cyclodextrin (MCT-?-CD) on Knitted Cotton and Cotton-Polyester Fabrics

Gilbert V. Gomez, Francis M. dela Rosa, Argentina T. Cariño, and Julius L. Leaño Jr.

Abstract

Monochlorotriazinyl-?-cyclodextrin (MCT-?-CD), 4 was synthesized from cyanuric chloride, 1 and ?-cyclodextrin, 3. The synthesized MCT-?-CD was applied to cotton and cotton-polyester (50/50 and 65/35) by pad-dry-cure method. Subsequent characterization of the grafted fabrics through Fourier Transform Infrared-Attenuated Total Reflectance (FTIR-ATR) Analysis revealed the successful grafting of MCT-?-CD, 4 into cotton and cotton-polyester fabrics with the appearabce of characteristic peaks at 1489 cm-1 and 1404 cm-1. Further, the grafted fabrics through Energy Dispersive Spectroscopic (EDS) Analysis revealed the presence of Nitrogen, indicative of the presence of the synthesized MCT-?-CD, 4 on the surface of cotton and cotton-polyester fabrics, Durability test revealed that MCT-?-CD-grafted cotton and cotton-polyester fabrics can withstand at least one washing cycle.

 

Total Phenolic Content and Textile Dye Performance of Dried Coffea robusta (Coffee) Mesocarp

Julius L. Leaño Jr., Neil Jhon G. Tadeo, and Evangeline Flor P. Manalang

Abstract

The total phenoloc content (TPC) of the Robusta coffee (Coffea robusta) pulp was successfully determined using Follin-Ciocalteu assay. Different factors, such as extraction methods, sample to solvent ratio, solvent system, temperature, rate, and duration, effect the amount of TPC extracted. Based on the result, refluxing with 50:50 EtOH-H2O is the best extraction solvent-system and approach. The crude coffee pulp extracts were freeze dried and was found to have the highest powder yield of 54.6% from extraction by boiling in water. The powdered extract was characterized using FTIR-DRS and UV-Vis Spectroscopy. FTIR spectrum showed the presence of peak corresponding to alcoholic O-H, alkyl C-H and aromatic C=C vibrations. UV-Vis spectrum showed a maximum peak at 312 nm corresponding to the electronic transitions of ? electronics in the benzene ring of the polyphenolic compounds. Results confirmed the presence of polyphenolic compounds as earlier detected by Folin-Ciocalteu assay. Dye potential of the coffee pulp powder was investigated and was found to impart light brown color to pineapple (Ananas comosus), abaca (Musa textilis), silk (Bombyx mori) and pineapple-silk) fabrics. Results further revealed that the dyed fabrics, whether pre-mordanted or not, showed satisfactory performance to colorfastness laundering and perspiration tests and these colorfastness properties proved that C. robusta mesocarp is a promising textile dye source.

 

Mechano-Physical Properties of Enzyme-Treated Musa textilis (Abaca) Fibers

Jeannie Lynn J. Cabansag and Julius L. Leaño Jr.

Abstract

Treatment of knotted abaca (Musa textilis) fibers with enzymes affording the subrate specific removal of noncellulosic impurities such as pectin, fats, waxes, lignin, and xylans was studied and compared with the conventional alkaline method of scouring. M. Textilis fibers were treated with commercially available pectinase, cellulase, protease, and xylanase at varying pH, temperature, surfactant and enzyme concentrations, and treatment duration. Physico-mechanical properties of treated fibers were evaluated in terms of % weight loss, whiteness, and tensile strength and compared with alkaline scoured fibers. Whiteness index was assessed using the CIE L*a*b* data expressing color in tri-stimuli values. Results showed that the efficiency of enzyme treatment on the fibers were comparable with the mechanical properties of alkaline treated fibers and exhibited better tensile strength. The use of enzymes in pre-treating M. textilis fibers offers a greener alternative to the conventional alkaline pre-treatment process.

*Note:
If you are interested to any of these scientific papers, send us an email at This email address is being protected from spambots. You need JavaScript enabled to view it. or at our google accountThis email address is being protected from spambots. You need JavaScript enabled to view it., with your full name, address and affiliation/institution.

 

1.) Synthesis of Cellulose Acetates from banana (Musa acuminata) Fiber

2.) β-Cclodextrin Microencapsulation of Peppermint (Mentha piperita) Essential Oil for Antibacterial Finishing of Cotton Fabrics

3.) Cellulose Nanocrystals (CNCs) from Abacá (Musa textilis Nee)

4.) Spent Liquor for Degumming Pineapple (Ananas comosus Linn.) Fiber

5.) Small-Scale Natural Fiber Degumming Machine

 

 

 

 

 

 

 

 

Synthesis of Cellulose Acetates from banana (Musa acuminata) Fiber

Jennelie E. Caya, and Zailla P. Flores

Abstract

Cellulose diacetate (CA) and cellulose triacetate (CTA) are two of the most industrially utilized derivatives of cellulose. Recent studies have demonstrated the potential of electrospun CA nanofiber membrane - a nonwoven texttile material, for biomedical applications including tissue engineering and nutraceutical delivery. In this study, CA and CTA were produced from local banana (Musa acuminata) fibers extracted from the banana pseudo-stem. The esterificationreaction of the cellulose pulp from banna fiber was carried out with acetic acid and acetic anhydride with the aid of sulfuric acid. The yield of the oven dried product and degree of substitutions (DS) are 62.08% and 70.04 %, 2.44 and 3.15 for CA and CTA, respectively. fourier transform infrared (FTIR) spectra indicate the succesful introduction of an acetyl group the cellulose backbone as evidenced by the presence of carbonyl stretch at around 1700 cm -1 for the esterified products. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) revealed the thermal stability of the CA, having more hydroxyl groups, is a Thermally more stable derivative.

 

 

β-Cyclodextrin Microencapsulation of Peppermint (Mentha piperita) Essential Oil for Antibacterial Finishing of Cotton Fabrics

C. Abendanio, L. Labaclado, E. Manalang, and J. Leaño, Jr.

Abstract

β-cyclodextrin (β-CD) microcapsules containing peppermint (Mentha piperita) oil were prepared via co-precipitation method using the optimized β-cyclodextrin-oil mass ratio and stirring time of 3:1 and 8 h, respectively. DSC analysis confirmed effective encapsulation of the peppermint oil as evidenced by the disappearance of an exothermic peak in the thermogram of the microcapsules which was observed in the thermogram of the pure peppermint oil. The FTIR spectra of the β-CD-oil microcapsule showed major peaks corresponding to O-H (3220-3500 cm-¹), C-H (2927 cm-¹) and C-O (1150), which were identical to that of pure β-CD. It also showed that the characteristic peaks of the peppermint oil are no longer observed in the spectra of the microcapsules. The SEM images revealed the sizes of the microcapsule to be in the range of 1-20 µm and the structures are cube-like.

The microcapsules were applied on knitted cotton via pad-dry cure method with 1,2,3,4-butanetetracarboxylic acid (BTCA) as cross -linking agent. SEM analysis of the treated fabrics showed the presence of microcapsules on the fabric. Further, FTIR spectra of the treated cotton showed peaks around 1716 cm-1, corresponding to an ester carbonyl formed between BTCA and cotton and BTCA and microcapsules proving effective cross-linking. The use of BTCA enhances the scent retention of the microcapsules.

Antibacterial property assessment (AATCC 147-2004: Parallel Streak Method) showed that the treated fabrics did not exhibit antibacterial activity which was construed as a proof of the effective encapsulation of the antibacterial peppermint oil that was protected by the β-CD capsule. Durability to laundering was assessed, and the results revealed that washing enhances antibacterial activity of the treated fabric due to facilitated rupture of β-CD microcapsules, hence release of the peppermint oil and thus the observed scent and antibacterial activity. Further, the synergistic effect of BTCA in cross linking and stabilizing the microcapsules was also observed.

Cellulose Nanocrystals (CNCs) from Abacá (Musa textilis Nee)

Joshua DQ. Olindan, Benson A. Roxas, Regina S. Gatmaytan, Julius L. Leaño Jr.

Abstract

Cellulose nanocrystals (CNC's) were isolated from abaca (Musa textilis Nee) fibers through sulfuric acid (H2SO4) hydrolysis. One-bath scouring and bleaching method performed three tomes yielded 98.89% total cellulose content which is suitable for the production of cellulose nanocrystals. From a series of trial isolation of CNCs, hydrolysis condition (acid concentration, acid-to-fiber ratio and temperature) was optimized at 50 % H2SO4, 20 mL acid per gram of fiber at 24°C. Hydrolysis time of scoured/bleached abaca fibers was performed from 30 - 180 min optimum time of CNC isolation (CNC90). Infrared spectra of raw abaca fibers (RAF), scoured/bleach abaca fibers (SBAF) and CNC90 were evaluated and decrease in the peaks associated with lignin and hemicelluloses was noted SBAF and CNC90 proving sufficient removal of said components. Morphological properties of the RAF and SBAF microfibrils after purification were observed through SEM imaging. The X-ray diffraction patterns confirmed the presence of crytalline domains in the cellulose.

Crystallinity Index (Crl) values were calculated for RAF, SBAF, CNC60, CNC90, CNC120 and CNC180 with CNC90 exhibiting the highest crystallinity region of 74.21%. The further decrease in Crl values at prolonged hydrolysis time of 120 and 180 min indicated the destruction of the crystalline phase of cellulose. Hence, the optimum hydrolysis of SBAF was effective in isolating cellulose with particle sizes in the nanometer range (at least one dimension equal or less than 100 nm). Particle sizes of the isolated nanocrystals decreased with longer acid hydrolysis with an average length of 110.50 nm and width of 19.48 nm for CNC90.

Spent Liquor for Degumming Pineapple (Ananas comosus Linn.) Fiber

Eduardo M. Marin

Abstract

The PTRI established degumming condition for pineapple was used in the first batch degumming of pineapple fiber. Spent liquor of sodium hydroxide was collected, measured and made-up to its original alkaline strength and volume and was used for second batch degumming. Same procedure was followed for the spent liquor from second batch degumming which was utilizedfor third batch degumming. Degummed fibers were analyzed for their physical and chemical properties to assess the effect of using spent liquor for degumming. Results showed that made-up solutions from spent liquor were as effective as the original solution as far as gum removal is concerned. Moisture content and total cellulose of the fibers degummed with new solution and spent liquor are also comparable.

Utilization of spent liquor for second and third batch degumming resulted to lower chemical inputs and consequently, reduced waste, thereby reducing the processing and wastewater treatment costs. 

Small-Scale Natural Fiber Degumming Machine

Ronald S. Pechera and Roberto O. Casero

Abstract

The invention relates to a simplified degumming machine that can process one to five kilograms of natural fibers such as pineapple, abaca, and banana, simulating the PTRI established technology without eliminating the degumping parameters of pressure, volume and temperature as customarily applied in the pilot scale processing. This invention can also be utilized as dyeing vessel for texttile-based micro enterprises. 

The machine consists of two stainless steel tanks using a closed system for complete circulation and penetration of chemical solution and through rinsing of the fibers. Heat source is provided by burners for the degumming and rinsing purposes and all accessories are placed in a movable platform for ease of transfer. Processing of natural fibers is simplified and made less laborious with the aid of a pump and gate valves for liquid circulation and another gate valve for the transfer of liquids from stock tank to the main tank. Improvements were noted in processing time of 36.5%for the three fibers, increase in fiber recovery of 2.8% for pineapple, 2.5% for abaca and 2.2% for banana. A reduction of residual gum by 22.4%, 13.9% and 20.7% and fineness property improved by 7.9%, 10.6% and 8.12% for pineapple, abaca and banana, respectively. Tensile strength  was significantly improved for pineapple and reduced for abaca and banana, all within the desired range if tensile strength of natural fibers for textile application at 23 to 30 Kgf for pineapple, 29 to 38 KGf for abaca and 19 to 30 Kgf for banana.