interest, as one seems preferable on nylon while the other is The detailed results of the Alum/FeCl, study are
are summarized
better on leather. In the meantime, we have synthesized an
analog of these dyes that possesses improved water solubility,
and will be evaluating its fastness properties soon.
In recent weeks, we elected to turn our attention to a family
of less commonly used complex-forming monoazo dyes as
targets for the synthesis of new I:2 Iron complexes. The re-
sult has been the formation of blue and violet colors for nylon
and wool, in addition to brown and black shades. Needless to
say, this is an exciting and quite promising turn of events.
We are planning to synthesize a group of mixed complexes,
with the goal of fine tuning some of the present shades. Ob-
viously, the next step is to assess the fastness properties of
this new family of dyes. The results of this determination
will be outlined in our next report.
Preliminary results from the mutagenicity testing of the met-
allized dyes prepared so far indicate that the Fe complexes
are either non-mutagenic or significantly less mutagenic than
both the corresponding Co and Cr analogs and the unmetal-
lized precursors. Laura will have more definitive results for
the next report.
Diazotization of Heteroaromatic Amines
We completed our investigation of the utility of FeCl, as a co-
agulant for the removal of phosphate ions from disperse dye
wastewater. Using filtrates derived from the synthesis of Dis-
perse Red 177, we found that phosphate removal at a level of
99.999+% can be achieved when an Fe:P ratio of 2: 1 is used.
This means that either Alum or FeCl, can be used as long as
the proper pH is employed. For Alum the pH should be 5-6,
and for the pH should be 3-4. In the coming months we will
conclude the present aspect of our work in this area with a
determination of the utility of the collected phosphate as a
component for commercial fertilizers. This is envisioned as
an alternative to either incineration or landfilling the
coagulants.
Technical Papers and Other Communications
A manuscript entitled “Premetallized Acid Dyes Based on
Environmental Considerations” has been prepared for the
Book of Papers for the upcoming AATCC International Con-
ference (October, 1993). This paper outlines the results to be
presented during the conference delivery, and focuses on the
fastness properties and genotoxicity of the black Fe com-
plexes synthesized as potential non-chromium alternatives to
commercial premetallized acid black dyes containing Cr.
The manuscript mentioned in our last report as having been
submitted to Textile Research Journal has been reviewed, and
was found acceptable pending our consideration of 3 points.
These were handled by us immediately, and the editor has
sent the revised manuscript to the reviewer for final
consideration.
National Textib Center Quarterly Report: April - June 1993
in a manuscript recently prepared and entitled Chemical Re-
moval of Phosphate Ions$rom Wastewater Derived from the
Synthesis of C. I. Disperse Red 177.
Electrotechnology Applications In Textile
Manufacturing
S92C6
Principle Investigators:
W. Carr (Georgia Tech); T. Clapp, P. L. Grady, H. Hamouda,
G. L. Hodge, G. Mock, L. Moser, B. Smith (NC State); W.
Perkins (Auburn) [reported by Mike Cato]
Objective:
1. Characterize basic dielectric infrared and ultrasound
properties of textile material for a database to be used
to develop these energy sources in fiber, textile, and ap-
parel manufacturing.
2. Develop textile processing utilizing electrotechnologies
for improvement in productivity and environmental
safety; includes IR absorption studies; dielectric prop-
erties studies; RF fixation mechanisms; and ultrasonic
dyeing.
3. Develop economic analysis of existing energy intensive
manufacturing technologies; expansion of existing en-
ergy models to include economic analysis; develop
non-traditional economic models (multiattribute deci-
sion) of electrotechnologies.
4. Develop new processing techniques such as an acceler-
ated process for dyeing short runs of polyester/cotton
fabric. Develop a process to quickly and economically
dye short runs of polyester/cotton blend fabrics; process
based on radio frequency energy.
5. Develop entirely new processes using combinations of
electrotechnologies such as ultrasonic dyeing and RF
drying.
Summary:
Joint research involving all three universities is being done to
determine the effects of washing efficiency on dielectric prop-
erties and RF drying of yarn packages. Warren Perkins has
determined common residuals in bleached and dyed yarn
packages. With Warren’s recommendations, experiments are
being designed and conducted at Georgia Tech using a net-
work analyzer which measures the dielectric properties of
materials. Different solutions typically found in textile dye-
ing have been prepared and analyzed to determine their di-
electric properties. Different types of salt had significantly
different loss factors. Data is being analyzed and a final re-
port will be compiled within two months. NC State is plan-
ning to use the information learned at Georgia Tech to design
pilot plant drying studies. To better understand the network
analyzer, Mike Cato, from NC State, worked at Georgia Tech
for a day.
23
A summary of activities at each site follows: the tests. Sodium acetate is the primary chemical likely to be
found in bleached yarn packages. For aqueous solutions of
Auburn sodium acetate, loss factor varied linearly with concentration
Work was done on a short run, quick response dyeing process from approximately zero for 0.005 g/l to 3 1.4 for 0.5 g/l. Af-
based on the use of radio frequency (RF) energy to fix dyes. ter the dyeing process, the major residuals are acetic acid, lu-
Previous work concentrated on dyeing either polyester or cot- bricant, and auxiliaries. Acetic acid was the only component
ton. During this quarter, a study of simultaneous fixation of that significantly affected loss factor. At a concentration of
disperse and reactive dyes on polyester/cotton fabric was con- 0.5 g/l, the loss factor was found to be 24.0. Further tests
ducted. Simultaneous dyeing of polyester were conducted to determine the effect of
and cotton is difficult because optimum ion size and concentration on loss factor.
dyeing conditions for disperse dyes and re- Dielectric measurements were made on
active dyes are different. Special neutral- aqueous solutions of sodium chloride and
dyeing reactive dyes were used so that the several acids (acetic, chloroacetic, di-
dyeing could be done in a neutral medium. on polyester and ootton. chloroacetic, trichloroacetic and formic).
The alkali normally required in reactive For the same concentrations (moles/liter).
dyeing inhibits fixation of many disperse dyes. The process loss factor varied greatly for aqueous solutions of the various
consisted of applying the disperse and reactive dye in the chemicals. Tests are to be performed to determine if loss fac-
same pad formulation. The fabric was taken up on a roll and tor for the solutions can be correlated to solution
insulated with foam and cardboard. Then, the fabric was conductivity.
heated to 90°C in a radio frequency oven to fix the reactive
dye. The insulation was then removed, and the fabric was NC State
dried in the RF oven. After the fabric was dry, the package Research on the ultrasound-aided dyeing is progressing
was again insulated, and RF heating was continued until the steadily. On February 25, the ultrasound consortium met at
fabric reached a temperature of 200°C in order to fix the dis- NC State to review and discuss the ultrasound project. The
perse dye on polyester. Color yields using the RF-assisted consortium consists of Branson Ultrasonics, Blackstone Ul-
process were about 90% of that achieved using conventional trasonics, Cotton Incorporated, and Greenville Machinery.
two step procedures in which the polyester and cotton are The consensus of the group was that other areas in textile wet
dyed in separate dye cycles. Additional work is needed to op- processing should be investigated in addition to dyeing, such
timize the RF-assisted process. as washing, finishing, and water removal. Currently, the
most expensive and time consuming process is dyeing, so the
Georgia Tech main focus of the project will continue to be ultrasound-aided
Research to characterize the infrared spectral properties of dyeing.
textiles is continuing. Measurements have been delayed due
to FT-IR system problems which are currently being resolved. An ultrasound cleaning tank has been configured to emulate
Software for data analysis and calculations of important pa- an atmospheric beck. Current experiments are designed to
rameters is being written. compare a 100% cotton fabric dyed with direct dyes in a com-
mercial machine (Mathis JFO) to fabric dyed in the ultra-
A flow-through dryer has been designed, and construction of sound tank with and without the ultrasound. The trials are
the oven will begin as soon as equipment funds are available. designed to determine the effects of ultrasound on fastness
The oven will be used to study the effects of an acoustic field properties (in particular washfastness, lightfastness, and
at different humidity ratios on drying of tufted nylon carpet. crockfastness), rate of dye exhaustion, and reduced dyeing
temperature. By comparing the exhaustion curves of the dye-
Residual chemicals found in wet bleached or dyed yarn pack- ing cycles with and without ultrasound, the period in which
ages can greatly alfect the performance of RF dryers. In ultrasound affected the exhaustion can be determined.
some cases, high concentrations of certain chemicals can
cause arcing problems related to high loss factor. Studies are A final report on the first phase of the project to optimize a
being conducted to determine which chemicals in the bleach- radio frequency dryer by utilizing intelligent automated han-
ing and dyeing process may cause RF dryer performance dling and controls has been completed. The project focused
problems and the effect of chemical concentration, Professor on the design and development of a low cost robotic system
Warren Perkins has studied the yarn bleaching and dyeing capable of controlling and loading a radio frequency (RF)
processes and determined the chemicals most likely to be dryer to maximize energy savings and through-put, minimize
found in the yarn during drying. The dielectric properties processing time, and deliver a uniformly dried, undamaged
(dielectric constant and loss factor) of aqueous solutions con- package without extensive plant layout modifications. The
taining these residuals have been measured over a spectrum proposed system uses a gantry type manipulator to pick pack-
from 10 MHz to 3 GHz. Results were compared at 27.2 MHz, ages from a pallet and place them in an optimal configuration
on the RF conveyor belt based on the characteristics of the
package. Standard machine design engineering practices
24 National Tex&ile Center Quarterly Report: April - June 1993
were used to analyze the dynamic and static aspects of the
manipulator in order to design proper motor drives and feed-
back control loops. Building the proposed system would cost
approximately $72,000. An estimate from a robot manufac-
turer to build a similar system was $155,000.
Technical Papers and Other Communications
Mike Cato and Hechmi Hamouda (flC State) are going to at-
tend the 28th Microwave Power Symposium in Montreal
Canada July 12-14, 1993. Hechmi will present a paper titled
An Analytical Model for the Combined Convective and Ra-
diative (IR) Drying of Fabrics. Following is an abstract from
the paper:
The process of moisture removal is analyzed based on a
balance of the required and supplied thermal energies
during drying. The computations were implemented to
investigate the process limitations to achieve efficient
fabric dving or preheating. An illustrative example,
requiring the removal of 70% of the initial water con-
tent from a given fabric, was numerically treated for a
specific set of drying conditions.
Hechmi Hamouda and Mike Cato have submitted an abstract
to the Microwave and High Frequency 1993 International
Conference in Goteborg, Sweden, September 28-30. The title
of the abstract is A Precise Model for RF Drying of Yarn
Packages. The abstract is given below.
A mathematical model of the transport phenomena in-
volved in the radio frequency (RF) drying of yarn pack-
ages was developed to describe the simultaneousjlow of
heat, liquid, water and air. The model consists of mass
and energy balances of the process defined in terms of
a set of nonlinear equations; empirical relationships
are used to solve these equations. Evaluation and ap-
plications of the model was demonstrated through a in-
teractive spreadsheet program. The results of the
mathematical model are compared to a set of experi-
mental radio frequency drying tests of yarn packages.
These tests were investigated in terms of power, mois-
ture content and dving mechanism.
Coloration Systems for Quick Response
Manufacturing
G92C5
Principal Investigators:
W. C. Tincher, W. W. Carr, F. L. Cook, P. Desai (NC State)
Objectives:
The objective of this research is to develop new coloration
technologies that will allow the textile industry to practice
quick response manufacturing. In year two
the specific objectives are:
1. To continue development of computer
controlled dye delivery systems for con-
National T&de Center Quarter& Report: April - June 1993
tinuous dye ranges that will permit rapid color changes
and short production runs.
2. To develop compatible pigment-resin systems for xero-
graphic printing of textile substrates utilizing molecu-
lar modeling techniques for selection of systems and
prediction of properties.
3. To develop thermal and/or UV curable ink systems for
ink-jet printing of textile substrates.
4. To demonstrate on a laboratory scale uniform and re-
producible dyeing of woven fabrics in garment form.
Summary:
The computer modeling of polymer properties system consist-
ing of the Biosym software running on a Silicon Graphics
workstation has been used to predict properties for several
polyesters of interest as binders for xerographic printing of
textile substrates. The predictions are being checked by pre-
paring the polyesters and checking properties such as glass
transition temperature, melt viscosity and initial shear and
tensile moduli. Polyesters are being prepared by interfacial
polymerization of terephthaloyl chloride with a number of
both single and mixed dials.
A number of polymer films have also been prepared by UV
initiation of acrylic acid terminated monomers. Polyacry-
lates, polyesters, and polyurethanes have been prepared and
are currently being evaluated.
The initial results on the use of an HPLC pumping system
with spectroscopic detection for on-line analysis of the dye
stream being pumped to a continuous carpet dye range have
been completed. Results show that it is possible to dilute the
dye stream at least lo-fold with a gradient pumping system
with a high degree of precision. A range of dye concentra-
tions from approximately 0.001 g/L to 1 g/L can be analyzed
with no dilution of the dye stream and with dilution this
range is 0.001 to 1.0 g/L. This is a very conservative esti-
mate of the analytical range.
The low volume applicator for continuous dye ranges is func-
tional and initial runs are underway. We are now evaluating
the uniformity of wet pick-up and the influence of speed and
pressure on the wet pick-up. Based on these experiments,
conditions will be selected for uniformity and repeatability
studies. Detailed information is also being collected on all
existing low volume applicators to look at approaches others
have taken to solution of this problem and for comparison
with the system we are developing.
A trip is planned next quarter to visit the
Research Center in Valence, France.
is one of the leading companies in
printing technology and we are in-
terested in one of the Imaje units as a test
bed for our materials development effort.
25