PREPARATION OF SPINNABLE DOPE FROM SUNFLOWER KERNEL PROTEIN

FOR TEXTILE FIBER PRODUCTION

A Thesis Paper

Presented to the Faculty of

College of Engineering, Architecture and Fine Arts

Batangas State University

Alangilan, Batangas City

In Partial Fulfilment of the Requirements for the Degree in

Bachelor of Science in Chemical Engineering

Aluan, Everlette C.

Fabregar, Noel Christian M.

Reyes, Marjorie B.

December 2016
 CHAPTER I

THE PROBLEM AND ITS BACKGROUND

INTRODUCTION

The growing consumer demand of textile and significant depletion of crude oil

reserves have driven the textile industries into continuous quest of finding a renewable

and sustainable raw material in the production of man-made fiber. Through the years,

numerous efforts have been made to redirect the production of textile from petroleum-

derived products, a non-renewable source, to agricultural-based products and even

wastes which can be renewed. Thus, producing a man-made fiber from available

agricultural sources worldwide has been the focus of the researchers in recent years.

Regenerated protein is one of the promising raw materials in the production of

man-made fiber nowadays. Azlon is the generic term for the commercially manufactured

fibers from regenerated naturally occurring proteins (Federal Trade Commission, 2011).

The fact that proteins are renewable and biodegradable materials has gained the

interest of many researchers in the area of textile fiber. According to the study conducted

by T. Rijavec and Z. Zupin in 2011, the fabrics made from protein-based fibers were soft,

lustrous, durable as well as possess good hand and thermal resistance. In addition, the

application of regenerated protein fibers became increasingly prominent in the

development of lightweight functional materials because of its exceptional mechanical

properties. (N. Reddy and Y.Yang, 2014).

Over the past years, sunflower (Helianthus annuus) became a remarkable

industrial crop globally and is cultivated on over 21 million hectares worldwide (Skoric et

al., 2007). Aside from being valued for its high edible oil content, sunflower kernels
contain significant amount of protein that can be regenerated to produce textile fiber.

The kernels of sunflower contain 20.8% protein (Gopalan et al.,1982) whereas

considerable similarities of techno-functional properties between sunflower protein, soy

protein and other leguminous products was investigated. Likewise, sunflower kernels

contain 18 amino acids and storage globulins, a predominant protein material crucial in

the production of fiber. In 2001, the study conducted by Gonzalez-Perez and Vereikjken

reported that globulin constitute most of the sunflower proteins, ranging from about 40-

90%.

The wet spinning is one of the commercially known processes in the production

of textile fiber from both cellulose-based and protein regenerated sources. In this

process, the oil must be first extracted from the kernels to obtain oil-free meal. The

process also involves isolation of protein from kernels with dilute alkaline solutions,

precipitation from the solution with acids and salts, washing, dissolving in an alkaline

solution, aging and spinning into acid bath (Hartman, 1970).

Consequently, this study will utilize sunflower kernel protein by extracting its

protein content via solvent extraction to produce a spinnable dope for textile fiber

production.

STATEMENT OF THE PROBLEM

The main objective of this study is to prepare a spinnable dope of sunflower

kernel protein for textile fiber production. Specifically, it aims to answer the following

questions:

1. What is the yield of sunflower kernels per kilogram of seeds?

2. What is the yield of oil-free meal obtained by using hexane for oil extraction?
 3. What is the yield of protein-rich material from the oil-free meal considering the

following solvents for extraction:

2.1. ethanol, and

2.2. sodium chloride solution?

4. Are these protein-rich material : NaOH : water ratio formulations aged for one

hour and two hours suitable for wet spinning process:

4.1 Protein-rich material : NaOH : water ratio (percent by weight)

4.1.1 10 : 0.85 : 89.15

4.1.2 10 : 0.90 : 89.10?

5. Is there a significant difference before and after post-treatment of the spun fibers

with glutaraldehyde in terms of:

5.1 Fiber fineness, and

5.2 Tensile strength?

HYPOTHESES

1. There is no significant difference between the yields of protein-rich material

obtained at varied sodium chloride concentrations (7.5%, 10% and 12%).

2. There is no significant difference before and after treatment of the spun fibers

with glutaraldehyde in terms of fiber fineness and tensile strength.

SIGNIFICANCE OF THE STUDY

The study focuses on the utilization of sunflower kernel protein by preparing a

spinnable dope from the protein-rich material obtained via solvent extraction and

subsequent dissolution of the meal in alkali solvent which will be subjected to wet

spinning process for textile fiber production.

 With this study, the proponents will be able to justify that sunflower kernel is not

only used for the production of cooking oil but can also serve as a raw material in the

production of textile fiber because of its significant protein content.

Specifically, this study will contribute in the establishment of economically

feasible methodology for preparation of spinnable dope from sunflower kernel protein. It

will also generate new markets for textile industry and meet the market demands of

quality products these days with further development.

The study will also provide solution for companies dealing with issues concerning

industrial waste particularly the sunflower oil manufacturers. The meal extracted from the

sunflower kernel in producing oil were considered as a waste and aside from being used

as ruminants for cows, pigs, and many others, the usage of the protein content of the

sunflower kernels will be maximized by converting it into regenerated protein fiber.

In addition, this study will also benefit the farmers as well as the farm industry

since it will provide them numerous opportunities and greater profit for the reason that

cultivation of sunflower plants is certainly needed not only for the production of sunflower

oil but also as a raw material for textile fiber.

Furthermore, the study will help the environment because it focuses mainly on

sustainable products that meets the environmental and social aspects. This study will

utilize and lessen the sunflower kernel wastes, thus, shall uphold an environment free

from unnecessary industrial waste.

Lastly, this study can provide an efficient basis for future researchers who are

interested in pursuing the study about the preparation of spinnable dope from the

sunflower kernel protein in the production of textile fiber.

SCOPE AND DELIMITATIONS OF THE STUDY

The focus of this study is to investigate on the preparation of a spinnable dope

from sunflower kernel protein for textile fiber production.

The first part of the study covers the obtainment of a protein-rich material from

the seeds. The seeds are hulled and ground until flour-like consistency of sunflower

kernels is achieved. To obtain the meal needed, the solvent utilized is limited to the use

of hexane only. Ethanol solution (70% by volume) is utilized to reduce the phenolic

content of the meal. Sodium chloride solution of varying concentration (7.5%, 10% and

12%) shall then be used to obtain a protein-rich material from the oil-free meal.

The second part of the study covers the preparation and syringe testing of the

spinnable dope. Prior to wet spinning is the dissolution and aging of the protein-rich

material in dilute sodium hydroxide solution. Syringe testing of the formulated dope shall

be conducted in a coagulation bath of acidic sodium chloride solution. Acidic sodium

chloride solution is prepared by mixing 10 parts of salt to 90 parts of 4% hydrochloric

acid solution.

The third part of the study covers the comparison of untreated spun fibers and

fibers treated with glutaraldehyde in terms of fiber fineness and tensile strength.

Sunflower seeds will be purchased from Dupay Seeds Trading, Quezon City.

The experiments will be conducted at the chemical laboratory of Batangas State

University Main Campus II. Laboratory tests for fiber fineness and tensile strength shall

be performed at Philippine Textile Research Institute Department of Science and

Technology, Taguig City.

CONCEPTUAL FRAMEWORK

The conceptual framework for the study outlines the concept and context of the

research investigation. The framework incorporates and defines the significant variables

in the study as well as the relationships among them. The researchers constructed the

following conceptual framework to synthesize a literature necessary in assessing and

realizing the objectives of the research.

The conceptual paradigm of the study is shown in the figure below:

Input
- Sunflower seeds
- Hexane
- Ethanol
- Sodium chloride
solution
- Sodium hydroxide
solution
- Sodium chloride
- Hydrochloric acid
solution
- distilled water
- glutaraldehyde
Process
Output
- Dehulling
- Sunflower kernels
- Grinding
- Ground kernels
- Solvent extraction
- Oil-free meal
- Vacuum filtration
- Protein-rich material
- Dissolution and
- Spinning dope
aging
- Untreated fiber
- Syringe testing
- Post-treated fiber
- Post treatment
-Fiber fineness
- Freeze drying
-Tensile strength
- Laboratory testing
- Statistical results
- ANOVA
- t-test

Fig.1 Conceptual Paradigm of the Study

Purchased sunflower seeds are hulled to obtain sunflower kernels. These kernels

are then ground until sunflower flour is achieved. Oil is extracted from the flour by using

hexane for 20 minutes at 40C with stirring every five minutes. To reduce the phenolic

compounds contained in the oil-free meal, it is treated with 70% ethanol solution at room

temperature. It will be performed by batch extractions with solvent to flour ratio of 5:1. A

protein-rich material will be acquired through treatment of the meal with sodium chloride

solution of varying concentration (7.5%, 10% and 12.5%) at 40C for 60 minutes. The

protein-rich material is separated from the solvent by vacuum filtration. One way analysis
of variance shall determine the validity of the hypothesis. Preparation of the spinnable

dope follows by dissolution and aging of the protein-rich material in dilute sodium

hydroxide solution. Dope formulations enlisted in the statement of the problem shall

undergo syringe testing in a coagulation bath of acidic sodium chloride solution

maintained at 50C. Untreated spun fibers and post-treated fibers (soaked in 25%

glutaraldehyde) shall be freeze-dried and stored until further use.

Laboratory testing of the untreated and post-treated fibers in terms of fineness

and tensile strength shall be conducted and results shall be subjected to separate paired

t-tests to determine the validity of the hypothesis.

DEFINITION OF TERMS

The terms below are conceptually and operationally defined for better

understanding of the researchers.

Agricultural based products. These are the products nurtured from plants or

animals in order to improve human life (https://www.thebalance.com/what-is-an-

agricultural-product-2538211). In this study, these are products that are biodegradable

and renewable.

Azlon. It is the generic term of regenerated fiber which is composed

of protein material derived from natural sources (https://www.britannica.com/topic/azlon).

In this study, the textile fiber that will be produced can be marked as azlon.

Biodegradable Materials. It has the ability to decompose, safely and relatively

fast, by biological means, into the raw materials of nature and disappear into the

environment (http://www.greengood.com/terms_to_know/biodegradable_definitions.ht

m). The fiber produced from sunflower kernel protein is a biodegradable material.
 Coagulation Bath. A liquid bath used in wet spinning processes that functions to

harden viscous polymer threads into solid fibers after extrusion through a spinneret

(http://en.termwiki.com/EN/coagulation_bath). This is where the syringe test will be

performed.

Dope. It is a solution (spinning solution) of fibre-forming polymer as prepared for

extrusion through a spinneret (http://www.textileindonesia.com/content/dope). In this

study, it is a solution that must be attained from which textile fiber can be drawn.

Ethanol. It is also called ethyl alcohol which is a colorless volatile flammable

liquid used as solvent and in fuels (http://www.merriam-webster.com/dictionary/ethanol).

It was used on the oil-free meal to reduce the phenolic compounds it contains.

Fiber Fineness. It determines the number fibers are present in the cross-section

of a yarn of given thickness (http://www.definetextile.com/2013/04/fiber-fineness.html). It

is one of the properties to be quantified in the spun fibers.

Freeze Drying. It is a dehydration technique, which enables liquid or slurry

products, which have previously been frozen to be dried under a vacuum

(http://freezedrying.com/freeze-dryers/general-principles-of-freeze-drying/). In this study,

it is will be used to preserve the spun fibers from sunflower kernels for further used.

Globulins. These are any group of proteins, as myosin , that occur in plant and

animal tissue and are soluble in salt solutions and coagulate by heat ((2001) Random

House Websters College Dictionary: Random House, Inc.). It is one of the main

components of the sunflower kernel.

Glutaraldehyde. It is characterized by a colorless, oily liquid with a sharp,

pungent odor generally used for sterilization and disinfection of equipment as well as

surfaces (https://pubchem.ncbi.nlm.nih.gov/compound/glutaraldehyde#section=Top). In

this study, it is the solvent to be used in the post-treatment of spun fiber.

 Hexane. It is used for extraction edible oils from seeds and vegetables, as a

special-use solvent, and as a cleaning agent that has a petroleum-like odor

(https://pubchem.ncbi.nlm.nih.gov/compound/hexane#section=Top). It is the solvent to

be used in the extraction of oil from sunflower kernels.

Kernels. It is soft and typically edible portion of a nut, seed, or fruit stone

contained within its shell (https://en.oxforddictionaries.com/definition/kernel). The

sunflower kernel is the main raw material in this study that will be utilized to generate

textile fiber.

Non-renewable source. It is a resource of economic value such as oil, natural

and coal that cannot be readily replaced by natural means on a level equal to its

consumption (http://www.investopedia.com/terms/n/nonrenewableresource.asp).

Oil-free meal. In this study, the oil-free meal means that oil was already

extracted from the sunflower kernel.

Two-way Analysis of Variance (ANOVA). It is used to determine whether there

are any statistically significant differences between the means of two or more

independent (unrelated) groups (https://statistics.laerd.com/spss-tutorials/two-way-

anova-using-spss-statistics.php). It is one of the statistical treatments used in this study

to test the validity of the hypothesis.

Paired Sample T-test. It is a statistical technique used in before-after studies to

compare two population means in case of two samples that are correlated

(http://www.statisticssolutions.com/manova-analysis-paired-sample-t-test/). It is one of

the statistical treatments used in this study to test the validity of the hypothesis.

Petroleum derived products. It is any commodity made from crude petroleum

or natural gas (http://www.iadclexicon.org/petroleum-products/). These are synthetic

products like synthetic fibers that are detrimental in our environment.

 Protein. It is one of numerous naturally occurring extremely complex substances

that consist of amino-acid residues linked by peptide bonds (http://www.merriam-

webster.com/dictionary/protein). In this study, it is the substance that will be isolated

from the oil-free meal of the sunflower kernel.

Solvent Extraction. It is a technique used to partially remove a substance from

a solution or mixture soluble (https://en.oxforddictionaries.com/definition/solvent-

extraction). In this study, ethanol and salt solution is used as solvents for solvent

extraction.

Sustainable products. These are the products that provide environmental

benefits (http://www.sustainableproducts.com/susproddef.html). In this study, these are

the products that are widely available.

Syringe testing. In this study, it will be used to test the formulated dope from

sunflower kernels.

Tensile Strength. It is the resistance of a material to a force tending to tear it

apart (http://www.thefreedictionary.com/tensile+strength). It is one of the significant

properties to be measured in this study.

Textile Fiber. It is a material generally spun from natural or synthetic sources

that can be further processed to produce textile yarns and fabrics

(https://textechdip.wordpress.com/contents/textile-fiber/). In this study, it is the product

that will be generated from the protein of sunflower kernels.

Vacuum Filtration. It is a technique by which the mixture is decanted through a

filter paper in a Buchner funnel to isolate a solid product from a solvent or liquid reaction

mixture (https://www.dartmouth.edu/~chemlab/techniques/vfiltration.html). It is a method

to be used in the separation of protein rich material from a solvent.

Wet spinning. It is a precipitation-based process where fibers are extruded

directly into a liquid bath (http://www.tikp.co.uk/knowledge/technology/fibre-and-filament-

production/wet-spinning/). In this method, the spinnable dope is subjected to wet

spinning and fibers will be drawn.

 CHAPTER II

REVIEW OF RELATED LITERATURE

This chapter presents both the conceptual and research literature in local and
foreign setting, which is crucial in information enrichment and better comprehension of
the study.

CONCEPTUAL LITERATURE

Textile Fibers
The term textile is derived from the Latin word textilis meaning woven

(Random House Websters College Dictionary, 2001). Accordingly, textile was generally

used to define a woven fabric as well as the processes concerning weaving. Through

the years, the term has taken on broad connotations including: (1) staple filaments and

fibers for use in yarns or preparation of woven, non-woven, tufted and knitted fabrics, (2)

yarns generated from natural and man-made fibers, (3) fabrics and other products made

from fibers or from yarns, and (4) apparel or other articles fabricated from the above

which maintain the flexibility and drape of the original fiber. This wide-ranging definition

will mostly cover all of the products manufactured by the textile industry directed for

intermediate structures or final product (Needles, 1986).

Numerous terms are associated with the word textile. The majority of the fabrics

we use every now and then are woven, thus, constructed by intertwining sets of yarns

that run along lengthwise and crosswise directions. Basically, yarn is composed of fibers

and a fiber is defined as any material capable of being interwoven, if not made into

fabric. It is the smallest visible unit of textile product. Fibers have very small diameter

and often described as pliable hair like strand. Further, fibers are fundamental units of
the building blocks used in the production of textile yarns and fabrics (Textile

Technology, 2010).

Types of Fibers

Textile fibers are customarily divided into two broad classes according to their

chemical origin. These two classifications include: natural fiber and man-made fiber

(Needles, 1986).

Natural fibers are those came from natural sources such as plants and animals.

This classification is further divided into protein fiber which is wool and silk, cellulose

fiber such as cotton and linen, and the mineral fiber like asbestos (Needles, 1986).

Natural fiber has a polymer-based, thus, characterized by a regular and repeating

structure. All natural fibers have a fixed length associated with them, varying from about

5 to 20 cm. This could be the length of the hair on the sheep (wool) or the length of a

cotton filament in a cotton plant (Weinberger, 1996).

Man-made fiber, on the other hand, are fibers in which either the basic chemical

units have been formed by chemical synthesis followed by fiber formation or the

polymers from natural sources have been dissolved and regenerated after passage

through a spinneret to spun fibers (Needles, 1986). Under this classification is synthetic

and regenerated fiber. Synthetic fibers are those made by chemical synthesis, usually

from coal, petroleum, nitrogen, carbon and hydrogen. (Needles, 1986 and Gioello,

1982). They are also based on a regular polymeric structure. Most of the synthetic fibers

are from polymers produced by step polymerization (usually, condensation polymers)

but many are manufactured from polymers produced by chain polymerization (addition

polymers). Synthetic fibers can be made into continuous filaments, which are

considerably infinite in length. (Weinberger, 1996). Conversely, regenerated fibers are

those generated from natural polymer sources and often called natural polymer fibers

(Needles, 1986).

Primary Properties of Fibers

Fibers have various properties considered by the textile and polymers industry as

crucial criteria in the formation, fabrication and assembly of fibers in the textile

substrates (Huang, 1994).

Fiber Length to Width Ratio. The length/width ratio of the units is a more

straightforward parameter, ranging from infinity for very long fibrils down to unity for

cubic micelles and to zero (or minus infinity on a logarithmic scale) for extensive flat

sheets. It is tacitly assumed here that the length refers to the direction of the chain axis.

Moreover, the ratio would be more usually regarded as thickness/width in lamellar

(Hearle and Morton, 2008).

Fiber Uniformity. The sufficient uniformity of fiber is the basis for the formation

of yarn. Only fibers uniform in shape and size are process into yarns and fabric. If the

fibers are not uniform enough, it may resulted to a yarn that is weak, rough, irregular in

size and unsuitable for textile usage (Needles, 1986).

Fiber Strength and Flexibility. The strength of a fiber is known as fiber tenacity.

It is defined as force per unit linear density necessary to break a sample of fiber. The

breaking tenacity of fiber may be expressed in grams per denier (g/d) or grams per tex

(g/t). Both denier and tex are units of linear density (mass per unit of fiber length) and

are defined as the number of grams of fibers measuring 9000 meters and 1000 meters

respectively (Needles, 1986).

Flexibility, on the other hand, allows freedom of movement and ability to shape

fabrics.The flexibility of fibers is directly linked to the flexibility of the textile product;
therefore, fabric adaptation to the end use and fabric durability are crucial and closely

related to evaluating fibers for particular uses (Joseph, 1988).

Fiber Extensibility and Elasticity. An individual fiber must be able to undergo

slight extensions in length (less than 5%) without fiber breakage and be able to recover

almost completely following slight fiber deformation. Thus, the extension deformation of

the fiber must be practically elastic (Needles, 1986).

Fiber Fineness. Fiber Fineness is the measure of the crosswise dimension of

textile fibers; included in this definition are fibers which have various forms and cross-

sectional shapes. The significance of fiber fineness focused on considering its effect on

yarn irregularity. The average number of fibers in the cross-section of a yarn of specific

linear density is dependent on the fineness of the fibers being used; the finer the fiber,

the greater the number of fibers which can be packed into the yarn. Moreover, this

property also determines the spinning value or spinnability of fibers (Textile Sizing,

2004).

Fiber Cohesiveness. It refers to the ability of the fiber to adhere to one another

when spun into a yarn. This property of the fiber may due to the shape and contour of

the individual fibers. Moreover, long-filament fibers by virtue of their length can be

entwined together to give stability without true cohesion between fibers. Often the term

spinning quality is used to state the overall attractiveness of fibers for one another

(Tufted Carpet: Textile Fibers, Dyes, Finishes and Processes, 2014). Natural fibers

possess unique structures that allow them to bind together. In synthetic fibers, on the

other hand, cohesiveness can be improved by reducing the diameter of the fiber,

increasing the aspect ratio, introducing the crimp shape to longitudinal section and

modifying the cross-sectional are into a more complex structure (Fundamentals of Fiber

Science, 2014).
Regenerated Protein Fiber

Regenerated fibers from proteins are called azlons (Brooks, 2009). These fibers

are made from globular proteins and known sources include soy, corn, peanut and even

milk. (Handbook of Textile Fiber Structure, 2009 and Brooks, 2009). The commercial

production of regenerated protein fiber dated back in early 1930s. In 1940, a variety of

proteins were used in the laboratory experiments and the small production of soya bean

fiber production was established. Further, fibers composed of casein from mill and zein

from corn and groundnut proteins were produced in the 1950. The poor quality of the

fibers produced and the advent of economical regenerated cellulose and synthetic fibers

lead to the decline and eventual eliminations of the azlons. However, recent advances in

biotechnology are being employed to develop novel methods and improve the fiber

properties (Reddy and Yang, 2015).

Azlon is generated by dissolving proteins such as casein from milk, soy protein,

or zein from corn in dilute alkali and forcing the solutions through spinneret into an acid

formaldehyde coagulation bath. (Brooks, 2009). Considering the structure, protein fiber

is the most complex of fibers. In addition to the complexity along the polymer molecule,

many composed of a mixture of proteins, in contrast to the single chemical compounds

that dominate the composition of other fibers. Likewise, multicellular fibers such as wool

and hair have structural features at multiple level on a coarser scale. Except possibly

from some difference in a surface skin, these fibers have a homogenous structure with

no differentiation above the atomic level (Handbook of Textile Fiber Structure, 2009).
Molecular Structure of Proteins

Proteins, originated from the Greek word proteios meaning holding first place

or of prime importance, are the most prolific of biological materials (Khan and Saxena,

2006 and Physical Properties of Textile Fibers, 2008). They are formed by the

condensation reaction of amino acids, NHCHRCOOH, with the production of a

peptide bond, NHCO and the elimination of H2O (Physical Properties of Textile

Fibers, 2008). In this way, proteins are characterized as very large and complex linear

chains consisting of a sequence of 20 amino acids in different combinations linked

exclusively by peptide bonds (Introduction to Biotechnology and Engineering, 2008).

The twenty amino acids present in proteins are named and denoted by three or

one letter designations. They consist of different side groups (R1, R2, etc.). It is the

distinction in the order and amount of these groups that determines the properties of the

material and gives rise to the large number of natural proteins that play a vital part in

animal and plant life (Physical Properties of Textile Fibers, 2008).

The successive levels of structure in a protein are categorized according to a

convenient, but possibly too rigid, terminology introduced by Linderstorm-Lang. The

linear sequence of residues in a peptide chain constitutes the primary structure of the

chain. Secondary structures are formed by regular local folding of certain sections of the

chains and stabilized by hydrogen bonds between NH and CO groups, while

other section exists in a random coil state (random in a sense of the absence of a

definite structural regularity) ( Chemistry of Natural Protein Fibers by R. S. Asquith,

2012). Tertiary structure is the overall three-dimensional shape of the entire protein

molecule. The protein molecule will bend and twist in such a way as to achieve

maximum stability or lowest energy state. Meanwhile, the quaternary structure refers to
how protein subunits interact with each other and arrange themselves to form a larger

aggregate protein complex. Thus, the final shape of the protein complex is stabilized by

various interactions, including hydrogen-binding, disulfide bridges and salt bridges.

(Particle Sciences, 2009).

Fig. 2 Protein Structures (Pearson Education, Inc., 2010)

Further, there are several sorts of crosslinks that can form between neighboring

protein molecules. The first one is hydrogen bonds which can form between the NH

and CO groups, associating neighboring main chains together. They may also form

between hydroxyl groups present in the side chains. Salts can form between basic and

acidic side chains by electrovalent forces. The cysteine linkage, on the other hand, is a

covalent crosslink between adjacent chains which turns numerous chain molecules into

a single network molecule. Globular proteins, for example, are a single long chain

molecules folded up into a compact ball held together by internal crosslinks. Globular

proteins may be unfolded, or denatured, by heat or other chemical treatments and can

then be drawn into fibres. Conversely, fibrous proteins are molecules more or less

extended and linked to their neighbor (Physical Properties of Textile Fibers, 2008).
Sunflower

Fig. 3 Sunflower (www.almanac.com) Fig. 4 Sunflower kernels (www.anuts.com)

Sunflower (Helianthus annuus L.) is one of the few plant species that originated

in North America (mostly originated in the Fertile Crescent, Asia or South or Central

America. The sunflower is a tall annual crop having a broadleaf structure with strong

taproot and prolific horizontal spread of roots (Department of Agriculture, Forestry and

Fishery, 2010). Leaves are described as dark green, roughly heart-shaped and have a

wrinkled surface together with prominent veins (UK Sunflower Association, 2003). Those

leaves that are invidually stalked and assembled in circumference of the stem are

phototropic. (UK Sunflower Association, 2003; Department of Agriculture, Forestry and

Fishery, 2010) Most often, sunflower plant reaches various heights ranges from 1.52 to

2.1 cm tall while dwarf varieties are only 0.91 to 1.22 cm high. The diameter of the

sunflower heads is usually between 7.62 and 15.42 cm; however, there also are

varieties with diameter measures more than 30 cm. Sunflowers exhibit heliotropism

which defines as the tendency for their flowering heads to follow the movement of the

sun during the daylight. This phenomenon has the advantage of decreasing damage

from birds and preventing the development of disease (Food and Agriculture

Organization of the United Nations, 2010).

 In terms of cultivation, sunflower is propagated by seeds only and can hybridize

spontaneously with various wild or weedy relatives (Burke et al., 2002). The process of

seed development proceeds when the individual flowers became pollinated during the

growing season. Seed development moves from the outer rim of the flower towards the

center. When the seeds are ready to harvest, their heads turn black or brown and their

moisture content varies from 10-12%. It normally takes 30 days after the last flower is

pollinated for the plant to mature (Food and Agriculture Organization of the United

Nations, 2010).

Furthermore, the sunflower has relatively short growing season compared to

some major crops around the world. Early maturing varieties can be readily harvested 90

to 120 days after planting while the late maturing varieties require 120 to 160 days to be

harvested. Undesirable changes in oil quality and an increase in free fatty acid content

will be notice if the harvesting will be delayed (Food and Agriculture Organization of the

United Nations, 2010).

The sunflower is cultivated primarily because of its seeds (Canadian Food

Inspection Agencys Plant Biosafety Office, 2005). Sunflower seeds are typically four-

sided and flat having a dimension 0.6 cm long and 0.3 cm wide. The seed coat or hull,

which surrounds the sunflower kernel, is generally black with dark and grey stripes.

Analysis of the kernel shows that it is composed of about 20% protein and 30% lipids. It

also contains a significant amount of linoleic acid that makes the kernel prone to

rancidity, consequently, giving it a limited shelf life (Food and Agriculture Organization of

the United Nations, 2010).

Over the years, sunflower seeds yield one of the worlds most important sources

of edible oil. For every 100 kg of seed, about 40 kg of oil, 35 kg of high-protein meal and

20-25 kg of by-products are produced (Food and Agriculture Organization of the United
Nations, 2010). Sunflower seeds from the oil-type varieties and hybrids are commonly

utilized to produce cooking oil, margarine and salad dressing. Also, they can be used in

making soaps as well as detergents and has further applications in paints, varnishes and

plastics posed by good-semi drying properties without color modification (Department of

Agriculture, Forestry and Fishery, 2010) In addition, the meal left after oil extraction is

valuable livestock feed with 50-60% protein (Canadian Food Inspection Agencys Plant

Biosafety Office, 2005).

Manufacturing of Regenerated Protein Fiber

Regenerated protein fiber is complex and more difficult to generate than

cellulosic fibers. Over the past years, the methods have changed significantly.

Numerous animals and vegetables were explored as protein sources for manufactured

protein fiber. Many production processes were established and most of them involved for

steps: separation of protein, solubilization of protein, fiber spinning and insolubilization of

protein (Fundamentals of Fiber Science, 2014).

Protein Separation. Basically, proteins are not readily accessible and some

contains an enormous amount of oils and fats. Consequently, proteins were first isolated

from the source material into a suitable form for fiber formation. Proteins were also dried

and ground into granules in some cases (Fundamentals of Fiber Science, 2014).

Solubilization. In this process, proteins were dissolved in a solvent for the

purpose of obtaining a useful spinning solution. Some proteins are like gelatin are readily

dissolved in hot water and glacial acetic acid while some which are dried and grounded

required stronger solvent. The obtained spinning solution was then aged to obtain the

desired viscosity. Oxidation and bacterial activity are necessarily controlled in this

process (Fundamentals of Fiber Science, 2014).

 Spinning. It concerns with the extrusion of spinning solution through a spinneret

into a coagulation to form filaments. In general, coagulation bath contains salts and

acids which promote coagulation and minimizes the tendency of the filaments to clump

together (Fundamentals of Fiber Science, 2014). The several methods of spinning

include: dry spinning, gel spinning, melt spinning, phase-separation spinning, reaction

spinning and wet spinning (Complete Textile Glossary, 2001).

Insolubilization. The purpose of this step is to form networks between protein

chains. The process is usually carried out in a liquid bath and degree of cross-linking is

considered. When the cross-linking is too low, the filaments wound not have a sufficient

wet strength to be made into useful products, otherwise, the filaments would be brittle if

the degree of cross-linking is too high (Fundamentals of Fiber Science, 2014).

RELATED STUDIES

Foreign Settings

There were recent related studies on the utilization of different raw materials for

the production of textile fiber. Most of the concepts of the researchers were adapted and

considered from these existing studies. Presented here are some of the published

studies and literature about kernel protein.

In the study conducted by Hsin Chi Huang in 1994 at Iowa State University, the

soy protein was utilized as a potential source for the production of textile fibers. The

main objectives of the study were to re-examine the wet-spinning process and attempt to

apply extrusion technology in the production of textile fibers from soy protein. In addition

to that, the factors limiting the functional properties of soy protein fibers were observed

and the properties of these fibers were improved by chemical modification.

 The study found out that the extruded soy fibers made by soy protein isolate

alone with water tended to be quite brittle while the tenacity of finished-fibers increased

as the concentration of acetaldehyde, acetic anhydride, glyoxal or glutaraldehyde

increased. Wet-spun soy fibers were successfully produced in 4% HCl baths containing

various inorganic salts. Among these salts tested in the coagulating bath, a combination

of sodium chloride, zinc chloride and calcium chloride improved fiber tenacity the most.

The results suggest that soy protein might be modified by molecular genetics to improve

their fiber-producing properties by decreasing the number of polar groups and increasing

the number of points for cross-linking.

The spinning of peanut protein fibers was the focused of the study accomplished

by D.L.Fletcher and E.M.Ahmed. In this study, Raw Altika peanuts were blanched,

partially defatted, ground and the protein was removed using an aqueous alkaline

extraction, precipitated at pH 4.0 and freeze dried to yield a protein concentrate with

85.5% protein, 3.1% fat and 2.0% ash on a dry weight basis. Most procedures report the

use of a simple acid salt combination for use as the coagulation bath in the spinning

process.It was found out that the viscosity of dope solutions increased rapidly with

increases in protein concentration from 11 to 14 and concentrations above 15% would

usually result in gelation during the mixing process while the 15% concentration would

usually form a gel shortly after mixing. Investigations have shown that dope viscosity can

also be influenced by holding time and/or age of the dope solution.

Results of the study revealed that the best conditions for the spinning of peanut

protein fibers were 13.0% protein concentration, pH 11.4, maturation time 10 hours at

1C, coagulating bath conditions of 2N acetic acid: 20% NaCl and dope extrusion

pressure of 15 psi.
 Another study with the title Production of Textile Fibers from Zein and a Soy

Protein-Zein Blend was conducted by Zhang, et.al. In this study, Zein fibers were

successfully prepared by a wet-spinning technique from a suspension formulated with

15% zein, 60% water, 22% 0.4 N Sodium Hydroxide and 3% urea by weight. It was

found out that after spinning, the tenacity of the zein fibers was improved by modification

with several agents such as acetic anhydride for acetylation, glutaraldehyde and

dialcohols for cross-linking and physical stretching. The researchers concluded that the

zein-soy protein mixture could be extruded, but properties of wet-spun fibers of zein-soy

blends were not much improved.

Local Setting
Numerous studies concerning production of textile fibers from cellulosic

renewable sources have been established locally. However, studies about regenerated

protein fiber which continues to advance and renews interest are indeed insufficient.

A study conducted by De Leon et al. in 2012 entitled Water Hyacinth (Eichhornia

crassipes) for Yarn Manufacture. In the study, the potential of water hyacinth as a

source of fiber for yarn manufacture was investigated. The fibers were extracted from

fresh stalks of water hyacinth using fiber decorticating machine and yielded 1.7% dry

fiber. The researches then found that 58.8% of the decorticated water hyacinth fiber is

gum with tensile of 8.07 kgfm/g and fineness of 68.8 denier. Numerous treatments were

carried out to convert fiber into it spinnable form. Results of the study revealed that the

yarn from the combined woolenization-degumming treatment exhibited acceptable

technical properties with less breakages and higher yarn realization.

Another study conducted entitled Mechano-Physical Properties of Enzyme-

Treated Musa textilis (Abaca) Fibers by Cabansag et al. in 2012. In this study, knotted

abaca (Musa textilis) was treated with enzymes to remove the non-cellulosic impurities
such as pectin, fats, waxes, lignin and xylans. The enzymes used include pectinase,

protease and xylanase at varying pH, temperature, surfactant and enzyme

concentrations and treatment duration. Physio-mechanical properties of the treated fiber

evaluated in terms of % weight loss, whiteness and tensile strength. Thus, the enzyme-

treated fiber was compared to with alkaline scoured fiber. The study found out that the

effectiveness of enzyme treatment on the fibers were comparable with the mechanical

properties of alkaline treated fibers and possessed better tensile strength. Likewise, the

researchers concluded that the use of enzymes offers a greener alternative to the

conventional alkaline pre-treatment for M. textilis fibers.

SYNTHESIS

The substantial studies discussed above are the justified literatures that were

used as the basis and reference for the preparation of spinnable dope from sunflower

kernel protein for textile fiber production.

In terms of raw materials, the researchers will also utilize a renewable source to

produce textile fiber. Sunflower kernels will be used as a raw material which is different

from the commonly attributed protein sources like soy beans, corn zein, peanuts and

milk casein and far more different from the cellulosic sources.

The study will used the same method mentioned above in producing textile fiber

from regenerated protein fiber. However, sunflower kernels will be grounded to achieve

flour which is solid in form other than the usual liquid form used. Hexane will be used to

extract the oil at the temperature condition of 40C for 20 minutes. Likewise, the study

will be using ethanol for reducing the phenolic compounds of the oil-free meal.

Researchers will vary the concentration of sodium chloride solvent to 7.5%, 10% and

12.5% at 40C. Before the spinning process, spinnable dope must be first attained like
what mentioned in the cited studies. In this study, syringe test will be employed in the

process. Also, the comparative analysis between the untreated spun fiber and post-

treated fibers (sprayed with 25% glutaraldehyde while the fibers are stretched) will be

carried out. Meanwhile, neither enzymes nor polymeric materials will be used in this

study.
 CHAPTER III

RESEARCH DESIGN AND METHODOLOGY

This chapter covers the research design, materials and methodologies proposed

by the researchers for the conduct of the study.

Research Design

The study utilizes the experimental method factorial design. Spinning dope

formulations and maturation time parameters are evaluated to determine its suitability for

the preparation of a spinnable dope and its effects on fiber fineness and tensile strength.

Preparation of Materials

Sunflower seeds are purchased from Dupay Seeds Trading, Quezon City. The

chemical reagents used: hexane, ethanol, hydrochloric acid, sodium hydroxide pellets,

and glutaraldehyde are obtained from JEFCOR Laboratories, Inc., Dasmarias, Cavite.

Extraction of Protein

Purchased sunflower seeds are washed, dried, weighed and hulled. Kernels are

then ground in a blender for one minute at maximum speed to achieve coarse flour-like

consistency. Oil is extracted twice from the meal by using hexane for 20 minutes at 40C

with meal to solvent ratio of 1:1 and with stirring every five minutes. The meal is then

cooled and treated with 70% ethanol solution at room temperature. It will be performed

by batch extractions with solvent to flour ratio of 5:1 (utilizing fresh solvent in every

stage). A protein-rich material will be acquired through treatment of the meal with sodium

chloride solution of varying concentration (7.5%, 10% and 12.5%) at 40C for 60

minutes. The protein-rich material are labelled X, Y, and Z, respectively, according to the

concentration of sodium chloride used. The proteins are precipitated by salting out and
are separated from the solvent by vacuum filtration. Among X, Y and Z, the one with the

highest precipitate yield shall be used for the preparation of spinnable dope.

Determination of Total Protein Content

Samples of seeds, kernels, oil-free meal, X, Y, and Z shall be taken for

determination of total protein content at the University of the Philippines Los Baos

Central Analytical Services Laboratory.

Preparation of Spinning Dope

Preparation of the spinnable dope follows by dissolution and aging of the protein

extract in dilute sodium hydroxide solution. Two formulations of the spinnable dope are

Formulation A, which consists of 10% protein extract, 0.85% NaOH, and 89.15% water

and Formulation B, which consists of 10% protein extract, 0.90% NaOH, and 89.10%

water. Each formulation is aged for 1 hour and 2 hours (labelled A1, A2, B1 and B2,

accordingly).

Formation of Sunflower Kernel Protein Fiber

Samples of centrifuged spinning dope are drawn by a 10mL syringe in a 100mL

coagulation bath of acidic sodium chloride solution (10% NaCl in 4% HCl solution)

maintained at 50C. Fresh coagulation baths are utilized for every spinning operation.

Drawn fibers are then soaked in 25% glutaraldehyde solution at room temperature for an

hour and are stretched afterwards. Fibers are washed with distilled water until neutral

pH, freeze-dried and stored for further use.

Evaluation of Protein Fiber

Tests for fiber fineness and tensile strength of the protein fibers are to be

conducted at the Department of Science and Technology Philippine Textile Research

Institute.
 Determination of Fiber Fineness. ASTM D 1577 method is used.

Determination of Tensile Strength. ASTM D 3822 method is used.

Fig. 5 Schematic Diagram of Protein Fiber Formation

Textile Production

Protein fibers and cotton fibers shall be woven as weft and warp, respectively.

Evaluation of Produced Textile

Blended woven fibers are tested for bow/skewness and bursting strength.

Determination of Bow/Skewness. ASTM D 3382 method is used.

Determination of Bursting Strength. ASTM D 3786 method is used.

Statistical Treatment of Data

Analysis of variance is used to compare the yield of protein extracts obtained by

varying the sodium chloride concentration in the solvent used for extraction. It is also

utilized to evaluate the effect of the dope formulations used and maturation time to the

fineness and tensile strength of the protein fibers as they are treated individually.

Paired t-test is used to determine if there will be a significant difference in the

properties of the fibers before and after treatment with glutaraldehyde.

Pearsons correlation is used to show the positive or negative correlation of the

effect of dope formulations and maturation time to fiber fineness and tensile strength.
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 WORK PLAN

S.Y. 2016-2017
ACTIVITY AUGUST SEPTEMBER OCTOBER NOVEMBER DECEMBER
CONCEPTUALIZATION
CREATING TOPIC
AND ITS
BACKGROUND
CONCEPT PAPER
SUBMISSION OF
CHAPTER 1 AND
TITLE PAGE
REVISION OF
CHAPTER 1
GATHERING RELATED
STUDIES AND
LITERATURE
SUBMISSION OF
CHAPTER II
REVISION OF
CHAPTER II
SUBMISSION OF
CHAPTER III
REVISION OF
CHAPTER III
BIBLIOGRAPHY,
SCHEDULE, BUDGET
REVISIONS OF
CHAPTER I, II, III
PROPOSAL DEFENSE

S.Y. 2017-2018
ACTIVITY JANUARY FEBRUARY MARCH APRIL
PREPARATION FOR
LABORATORY WORKS
EXPERIMENTATION
DATA ANALYSIS
PRESENTATION,
ANALYSIS,
INTERPRETATION OF
RESULTS
SUMMARY, FINDINGS
AND CONCLUSION
CONSULTATIONS OF
CHAPTER 1-5
REVISIONS OF
CHAPTER 1-5
FINAL DEFENSE
ESTIMATED BUDGETARY REQUIREMENTS

Table 1. Materials and Reagents

SAMPLES QUANTITY PRICE (/UNIT) TOTAL ()

Distilled Water 24 L 81/6L 324
Sunflower Seeds 6 kg 150/kg 900
Hexane 10 L 100/L 1000
Ethanol 15 L 69/500mL 2070
Sodium chloride 500g 40/1000g 20

Sodium hydroxide
20 g 200/150g 26.67
pellets

Hydrochloric acid 100 mL 140/100 mL 140

Glutaraldehyde 100 mL 125/100mL 125

Syringe 12 pcs 35/pc 420
Filtering Film 3 boxes 200/box 600
Blender 1 1500/unit 1500
Ziplock Bag 1 pack 100/pack 100
Corkboard 1 150 150
Trough (100mL) 3 100/pc 300
Tissue 5 packs 40/pack 200
TOTAL 7875.67

Table 2. Test and Analysis

SAMPLES QUANTITY PRICE (/UNIT) TOTAL ()

Seeds 3 572.00 1716.00
Kernels 3 572.00 1716.00
Oil-free meal 3 572.00 1716.00
Extract 3 572.00 1716.00
Untreated fibers 6 545.00 3270.00
Untreated fibers 6 1100.00 6600.00
Post-treated fibers 6 420.00 2520.00
Post-treated fibers 6 570.00 3420.00
TOTAL 22674.00
 Table 3. Miscellaneous Payments

MISCELLANEOUS PRICE
Printing 2000.00
Binding and Cover 1200.00
Food 2000.00
Transportation 2000.00
Professional Fees 3500.00
TOTAL 10700.00

Table 4. Summary of Budget Allocation

PROPOSED
BUDGET ALLOCATION
BUDGET

Materials and Reagents 7875.67

Test and Analysis 22,674.00

Miscellaneous 10700.00
TOTAL 41249.67