Producing Viscose Rayon from Sustainable Cellulose

Emma Lenderink and Sharon Ideguchi

Bellarmine Preparatory, Tacoma, Washington
Teacher: Mr. DeGroot

Abstract

In an expired patent Production of High Strength Cellulose Fiber Using Zinc

Chloride, Organic Solvents and Aqueous Solution, Dr. Li Fu Chen outlines an alternative
way of making rayon. Using this patent and building upon it, this paper describes a
process to create a sustainable and cost effective viscose rayon fiber. This alternative
method of producing rayon can benefit the environment and the rayon industry, due to
the processs use of abundant sustainable materials and its simplified methods. Our
process uses water, zinc chloride solution, and cornstalk cellulose in a new ratio, not
described in the patent. It creates rayon fibers through heating then extrusion into a
coagulation medium. These fibers were tested for tensile strength with a range of .012
g/den to .216 g/den. Although these tensile strengths are less than previously reported
values, this process shows promise. With the proper equipment this new process could
be applied as a viable and favorable alternative to current rayon production methods.

Statement of Outside Assistance

Many research advisors helped with the making of this project. Dr. Armstrong from the
University of Oklahoma was the first person contacted about this project as an inquiry into
sustainable textiles, she then put us in contact with Dr. Ruppert-Stroescu who helped further with
the formation of our project. Dr. Ruppert-Stroescu from the University of Oklahoma helped us
find the patent, on which our experiment is based. The patent is discussed in the background
below. Dr. Hang Lui at Washington State University assisted us by answering our questions on
the science behind textile formation. Dr. Yakelis at Pacific Lutheran University met with us, and
answered questions we had about the chemistry of cellulose extraction. Dr. Xu at Purdue
University helped us by answering questions about the patent, as she was the colleague of the
late Dr. Li Fu Chen. Mr. Kuykendall at the University of Washington, allowed us to use the
Universitys Instron Tensile Testing machine at their mechanical engineering lab. The teacher,
who oversaw our project and its progress, was Mr. DeGroot. All original work was carried out
by us, the students, under the guidance of Mr. DeGroot. This is an original project.

Background
Viscose Rayon is an artificial silk material
commonly used in making clothes. Rayon was the first
man-made fiber ever produced, invented in 1894.
Originally created as a cheap alternative to silk, its
advantageous qualities contain, taking well to dyes,
wrinkle resistance, and a silk like sheen. Due to these
qualities it is used heavily in many markets from textile
industries to pharmaceutical packaging companies. From
its initial invention to todays markets, the process for
making rayon has not changed in any drastic way. The
same process that was published in 1894 is still being
used to make rayon today (Jones).
Rayon is commonly made by treating dissolving
pulp with aqueous sodium hydroxide and carbon disulfide
to create fibers for spinning. The undesirable chemicals
that go into making the fibers include caustic soda, or
sodium hydroxide, sulphuric acid, zinc, and sodium
sulfate. Each of these chemicals have detrimental effects
Figure 1
on the environment and are not sustainable, unsustainable
The 18 step process used for
meaning that the use of these chemicals and the rampant
current production on (regular)
deforestation cannot be maintained at its current rate.
viscose rayon.
Sulfuric acid for instance can enter the air during
production and dissolve into clouds, fog, and rain, then reappear in the form of acid rain. Along
with the use of harmful chemicals, traditional rayon processes also requires the harvest of 53-75

million trees a year in order to get the wood pulp necessary to make fibers. Canopy founder and
executive director, Nicole Rycroft, says around 30% of the rayon and viscose going into clothing
comes from dissolvable pulp sourced from endangered and ancient forests(McCullough, 2014).
The unfortunate result of deforestation and the prevalence of harmful chemicals, in the
process for making rayon, has led to researchers becoming increasingly aware of the
environmental detriment of rayon production. Now most of these researchers believe that the
process is no longer sustainable.
To combat these effects, researchers have made strides to change the process for making
rayon. They have developed such processes as Lyocell, in which rayon is made from bamboo
cellulose. While Lyocell is made of bamboo, which grows at a much faster rate than trees, it is
still detrimental to the environment. The vast bamboo fields must be harvested in order to
acquire the cellulose for production. Corn is mass-produced and is used for various purposes,
such as ethanol fuel, food, and livestock feed. The farms used to grow bamboo for Lyocell on the
other hand, are used solely for the purpose of growing and harvesting. Compared to cornstalks, a
byproduct of producing corn, bamboo is not as sustainable.
Due to the shortcomings of current methods for making sustainable rayon, other sources
have been researched. We found an expired patent from the 1980s by a researcher named Li Fu
Chen. His patent, Production of High Strength Cellulose Fiber Using Zinc Chloride, Organic
Solvents and Aqueous Solution, (Purdue Research Foundation, West Lafayette, Ind., 1991)
investigates the benefits of creating rayon from sustainable cellulose and an alternative
production process. The sustainable cellulose would come from corn stalks, sugarcane bagasse,
and recycled paper; all of these materials being byproducts of other processes themselves. The
process in question involves cooking the cellulose with zinc chloride and coagulating it to make
the rayon fibers. These fibers would be stronger than traditional fibers and more eco-friendly.
The cellulose itself is also sustainable. In theory this process is more sustainable, saves time and
has more eco-conscious qualities. Yet, it has never gone into production. When Dr. Chen created
it in the 1980s, many sources cited it as being the next big textile breakthrough in the coming
years but, after 1993, it fell off the grid. One possible reason for this may be the vague nature of
the patent. The process described in the patent is only an outline with a variety of possible ratios,
between water, cellulose, and zinc chloride solution, that could produce fibers of varying tensile
strengths. Therein lies the problem of finding a ratio that can create viable fibers.

Research Problem
Can rayon fibers be created from cellulose using water and a zinc chloride solution?
What is the tensile strength of these fibers and how do they compare to commercially created
rayon fibers?

Research Design
To find the process to create testable fibers, many trials were run to determine a
successful ratio and then were tested for tensile strength.

Variables
Independent Variables include heat, and the ratio between water, zinc chloride solution,
and cellulose. Dependent Variables include the resulting tensile strength of individual rayon
fibers.

Data Collection Procedures

Fiber Creation:
Cellulose (Avicel pH 101) was pre-wet with distilled water in a ratio
of 1:2 (Refer to Appendix 1 to see the process for finding the ratio). A 73%
ZnCl2 solution was then added in a water to solution ratio of 2.94 to 4. The
reaction temperature was kept no higher than 60-70 degrees Celsius for at
least an hour, until the solution turned clear. The solution was put into a 22gauge hypodermic needle and extruded into a coagulation medium of ethyl
alcohol. Fibers were allowed to coagulate. After 15 minutes the fibers were
removed from the coagulation medium and air-dried. The drying fibers were
weighted down at the ends so as the fibers dried they stretched to orient their
molecules. After the fibers stretched and dried, they were dipped in a water
bath to crystallize the fiber. The fiber was then dried to finish the production
of the viscose rayon fiber. After 5 successful trials about 25, 10cm long,
fibers were produced.

Figure 2
Dried fibers.

Testing Tensile Strength:

A collection of fibers was taken to the University of Washington Seattle to the
Mechanical Engineering lab to be tested on an Instron 5585H tensile tester machine. Each fiber
was cut into 7 cm segments. Individual fibers were loaded into the Instron. The grips to hold the
fiber were equipped with sandpaper tabs to better grip the fibers. To load a fiber the top of the
fiber was lined up with the middle of the top grip then clamped. The top grip was then adjusted
in relation to the bottom grip in order to fit the length of the fiber. The bottom of the fiber, which
was now in line with the middle of the bottom grip, was then clamped. The length was adjusted
with a fine-tuning knob until the fiber was taut. The Instron was connected to a computer
program that was set up to graph continuously at a rate of one millimeter stretched per minute,
until failure. This meant that when the Instron started, it pulled the fiber at this rate until it broke.
24 fibers were tested total, with 6 fibers not included in the resulting data due to slipping errors
with the machine. When the fiber broke, the graph stopped and showed the graph of the
elongation versus the load strength (gf/mm). To get the tensile strength (g/den), or grams per

denier, from gf/mm, the linear density first had to be calculated. The linear density was found by
dividing the mass of a fiber by the length. The linear density was then multiplied by 9000 to find
denier, denier being a unit of weight by which the fineness of rayon is determined. From there
the grams of force of the load strength for each fiber was divided by the denier, in order to find
the tensile strength.

Figure 3
Instron 5585H Tensile
Testing Machine

Figure 4
Fiber placed in Instron for
testing.

Figure 5
Broken fiber after it was
tested in Instron.

Results

Figure 6
Dry fibers had the higher load capacity but a low level of elongation, which created a taller
curve. The damp fibers had a higher elongation but a low load strength, which is shown through
the long short curve. The breaking points are visible by where the lines sharply cut off, and move
downward.

Figure 7
Tensile strength of the tested damp fibers ranged from 0.012131 g/den to 0.091783 g/den.

Figure 8
Tensile strength of the tested dry fibers ranged from 0.104203 g/den to 0.216417 g/den.

Standard Deviations
Tensile Strength (g/den)

0.3
0.25
0.2
Damp Fibers Mean

0.15

Dry Fibers Mean

0.1
0.05
0
1

Figure 9
The standard deviation of the damp fibers was 0.035474085 g/den of the mean, 0.17671375
g/den. Of the dry fibers standard deviation was 0.024367977 of the mean, 0.03835477.

Discussion
The findings from this study demonstrate that making rayon fibers from sustainable
cellulose, like corn stalk cellulose, has the potential to be a viable alternative to traditional
processes for making rayon. The fibers produced in this experiment were made with the same
process as diagramed in Dr. Li Fu Chen's patent, Production of high Strength Cellulose Fiber
Using Zinc Chloride, Organic Solvents and Aqueous Solution, with an altered ratio. The process
for making the fibers utilized zinc chloride and a cellulose that closely imitates the cellulose of
corn stalk (Avicel pH 101), these two things coupled with water and ethyl alcohol produced the
rayon fibers and made up both a sustainable and effective way of making rayon.
Of the fibers tested, fibers 2, 4, 5, 6, 16, 17, 18, 19, 20, 22 were tested before the fibers
dried completely, and represent the tensile strength of damp fibers. These fibers experienced
more elongation but broke under a significantly smaller load than the dry fibers. Fibers 1, 3, 12,
13, 14, 15, 21, 24 were fibers that were completely dry when tested. These fibers had larger load
strengths and broke under a much higher force, but did not elongate as far as the damp fibers. A
statistical difference was found between the damp and dry fibers. These findings are consistent
with the characteristics of damp and dry traditional rayon (My Textile Notes, 2009).
Compared to the fibers described in the patent, the fibers made were weaker than those
cataloged in the patent. The fibers in the patent had tensile strengths ranging from 2.8 g/den to
4.5 g/den as compared to our .012 g/den to .216 g/den. Possible reasons for this discrepancy
could have been inconsistent pressure when extruding the solution into the coagulation medium.
The solution proved to be very viscous. Human hands were unable to keep a constant pressure
during the extrusion process because of the large amount of force required. This inconsistency of
pressure led to increased air bubbles within the fibers that formed in the coagulation medium.
Those air bubbles led to skinnier sections of the fiber, which made the fiber weaker in those
places. The compromised sections of the tested fibers led to decreased tensile strengths. To
combat this problem the use of a spinneret, which is a large industrial machine that extrudes
fibers into a coagulation medium at a constant rate and with constant pressure, is suggested. The
amount of air bubbles could be reduced and the tensile strength could be increased, through this
change in equipment.
When the tested fibers are compared to traditional fibers, whose tensile strength ranges
from 2.0 g/den to 2.6 g/den (My Textile Notes, 2009), these fibers proved to be weaker with
values of .012g/den to .216g/den. With more trials and the implementation of a spinneret, it is
believed that the tensile strength of the fibers could meet or even exceed the tensile strength of
traditional fibers as indicated in the patent. With this increased tensile strength, the new fibers
would be more effective than traditional fibers. The larger the tensile strength, the less likely the
fibers are to break when being used in practical applications. Based on these findings it can be
inferred that with the appropriate equipment, these new fibers could be a viable alternative to
traditional rayon fibers.

In addition to practical applications, this alternative process could also possibly be

implemented on a large scale due to its cost effectiveness. The process itself is able to produce
large batches, as long as the ratio of water, zinc chloride and cellulose stays the same. This
process also cuts out 12 of the 18 steps in the process of making traditional rayon. Comparing the
cost of traditional rayon materials to the materials of this experiment, corn stalks are more cost
effective. Wood pulp costs approximately $875 per ton (Indexmundi.com, 2016), with only 40%
of a tree becoming usable cellulose (Cassidy, and Ashton). On the other hand, this experiment
utilizes corn stalks which cost approximately $72 (www.extension.iastate.edu/agdm, 2016) a ton
and about 45% of the stalk is usable cellulose (Rymsza, 2016). From a cost and waste
perspective, this experiment uses more of the raw materials and at a lower cost.
Future steps to be taken with this process would be the implementation of a number of
different celluloses including sugarcane bagasse and recycled paper. Also the patent states that
the ZnCl2 can be recovered for further use, which would be an invaluable step, so finding a way
to recover the zinc chloride could be looked into further. Additionally, we found the process for
extracting the cellulose from the raw material to be a limitation for us due to our lab equipment
and experience. One process involved boiling strong acids while the other involved a specific
high-pressure oven that we could not acquire. In the future, when looking to implement other
sources of cellulose, this problem should be addressed.

Conclusion
The process of making rayon explored in this experiment sheds new light on an
alternative to the current environmentally harmful process. This research proves the possibility
and viability of employing byproduct cellulose as a main cellulose source for producing regular
rayon. Therefore, this new process would cut down on the chemical byproducts and wastefulness
traits of traditional rayon processes. It also shows the cost benefits of this new process. With the
correct equipment, to increase the tensile strength to the strength described in the patent, this
process is a viable alternative to the traditional rayon manufacturing process.

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Appendices
Appendix 1
Date

Method

Cohesion
Scale
(0-4)

4-20-15

- .335g cellulose into 10mL of ZnCl2

- heated to 60 degrees for 10 minutes

5-26-15

- 3.35g cellulose into 10mL of ZnCl2

- heated to 60 degrees for 20 minutes

6-15-15

- 33.5g of cellulose to 100mL of solution

- heated solution to 60 degrees for 30
minutes

6-16-15

continuation of mixture made 6-15-15

- dried overnight

NA

Qualitative Result

Determined ZnCl2 was of poor quality

7-14-15

- 1.75 grams of cellulose

- made white cloudy

measured out 50ml of new 69% ZnCl2

solution
- heated the solution to 62 degrees
Celsius
- then added cellulose
heated cellulose until opaque
- added to ethyl alcohol
7/15/15

- heated 50mL of 69% ZnCl2 solution

with 1.75g of cellulose at approx 90
degrees for 90 minutes
- while hot the solution was put the pipet
and extruded into the Erlenmeyer flask
full of ethyl alcohol

substance

- not clear
- stuck to itself
- not stretchy
- Fragile broke when lifted
from medium
8-11-15

- .335g of cellulose with 1.35ml of water

to pre-wet it
- poured that into test-tube set up
- added 2mL of 76% ZnCl2 solution
- stirred for approximately 3 hours
- solution never turned clear
- water temperature approximately 70
degrees Celsius for the duration of time

NA

8-17-15

- .335g of cellulose into the test-tube

- added 1.35ml of water to test-tube
- added 2mL of 76% ZnCl2 solution to
test-tube
- stirred continuously with bean for 3
hour
- never turned clear

NA

8-18-15

- .335g of cellulose with 2 mL of 76% -

Fiber too weak to pick up

ZnCl2 solution and 1.35ml of water

together
- stirred for 15 minutes, didn't turn clear
- let heat for 23 minutes

from medium

8-18-15

- .335g of cellulose with 2mL of 69%

ZnCl2 solution
- stirred with magnetic bean for 1 hour,
never turned clear
- .67g of cellulose with 2.7mL of water
and 4ml of 76% ZnCl2 solution
- stirred for 1 hour
- never turned clear
- extruded into coagulation medium

NA

fibers didn't form

8-18-15

- .335g of cellulose with 3.35g of

cellulose with 2mL of 69% ZnCl2
solution
- stirred with stirring bean for 2 hours
- never turned clear

NA

fibers didn't form

8-18-15

- .67g of cellulose with 2.7ml of water

and 4ml of 76% ZnCl2 solution
- stirred for 1 hour
- never turned clear
- extruded into coagulation medium

NA

fibers didn't form

8-26-15

- 1.5g Calcium Chloride

- 1.35ml water
- 2ml 76% ZnCl2
- .335g Cellulose
- add 1.5g of Calcium to 1.35ml of water
- add the calcium water to the cellulose
- add the calcium/water/cellulose to the
ZnCl2 solution
- heated at 70 degrees Celsius for 10
minutes

- substance turned goopy

before it turned clear and
proved impossible to put
into the syringe for
extrusion
- the bit that we did get
into the ethyl alcohol was
white and non-cohesive
new trial

8-26-15

- 2g Calcium Chloride
- 1.35mL water
- 2ml 76% ZnCl2
- .335g cellulose
- added 2g of Calcium to 1.35mL of
water
- added calcium water to .335g of

substance turned goopy

and clear but too high of a
viscosity to extrude
the bit that was put into the
ethyl alcohol was white
and non-cohesive

cellulose
- added calcium/cellulose/water to 2mL
ZnCl2
- heated at 65 degrees Celsius
for 20 minutes
9-11-15

- 73% ZnCl2 solution and mixed 2ml of

that with .07g of cellulose and 1.47ml of
water
- that was stirred and heated at about 65
degrees celsius for 30 minutes
- solution was opaque when we extruded
it into the ethyl alcohol

- got one strand

- not quite cohesive
- tried to stretch
- dunked in water
air drying under hood

9-15-16

- observed fibers made on 9-11-15

- brittle to touch
- shrank considerably

NA

9-15-16

- 4 mL of ZnCl2 with .14g of cellulose

NA
and 2.94ml of water
- heated at about 65 degrees celsius for 30

- accidentally got water

into the beaker
threw out experiment

9-17-15

- 4 mL of ZnCl2 with .14g of cellulose

and 2.94ml of water
- heated at 62 degrees Celsius
for 30 minutes

NA

- ran out of class time

before it turned clear and
had to leave it

9-29-15

- mixed 4 mL of ZnCl2 with .14g of

cellulose and 2.94ml of water
- heated at 68 degrees celsius
for an hour
- produced a totally clear mixture
was a bit too thick to extrude
- poured viscose liquid into medium

-tried pulling fibers, pulled

apart

9-29-15

- mixed 4 mL of ZnCl2 with .14g of

cellulose and 2.94ml of water
- heated at 68 degrees celsius
for an hour
- produced a totally clear mixture
was a bit too thick to extrude

10-15-16

- mixed 4mL of ZnCl2 with .14g of

cellulose and 2.94ml of water
- let heat at about 62 degrees celsius for
an hour
- heated until it was clear
- when it was clear it was extruded into
the coagulation medium

- extruded through the

syringe
- fibers thicker and more
white than the previous
fiber
- they were only a 3, they
were bendable but came
apart when we pulled

- were able to stretch fibers

successfully
11-19-15

replicated method from 10-15-16

- fibers stayed in longer

strands

11-18-15

replicated method from 10-15-16

successful

11- 22-15

replicated method from 10-15-16

successful

11-23-15

replicated method from 10-15-16

- successful
- Now have enough fibers
to do tensile testing

Cohesion Scale from 0 (non-cohesive) to 4 (completely cohesive)

The cohesiveness scale in Figure 1 is a representation of how well the fiber molecules
stick together to form a flexible fiber. This scale helps determine how successful the fibers in
quantitative data. The fibers that scored 0 on the scale did not stick together at all, flakes of
cellulose floated around in the ethyl alcohol. A 1 on the scale, visible fibers were formed when
extruded into the ethyl alcohol but broke when lifted out of the medium. On the scale a 2 is when
fibers are produced and successfully lifted out of coagulation medium but when stretched the
fiber broke apart with little force exerted. A 3 is the same as a 2 but it breaks when stretched to a
higher elongation. The fibers that scored a 4 on the cohesiveness scale were successfully
produced and stretched, then tested for tensile strength.