Title:
Method of heat-setting twisted polycarbonamide yarn
United States Patent 3872558
Abstract:
The improved method of this invention omits autoclaving and substitutes tumbling of the yarn as skeins at a selected temperature between 120° and 240°F. for a period of 2 to 10 minutes in the heat-setting of twisted polycarbonamide yarn. The process gives a product carpet with locked tuft tips.
US Patent References:
Artificial fiber and process of producing same
Kagi - October 1935 - 2019185
Treatment of artificial silk filaments
Bouhuys - May 1936 - 2039279
Method of setting the twist of rayon yarn
Hood - August 1936 - 2050325
/2251962.html
Sommaripa - August 1941 - 2251962
Crepe thread and method of making same
Schneider et al. - December 1941 - 2265202
Artificial fiber and process of producing same
Kagi - October 1935 - 2019185
Treatment of artificial silk filaments
Bouhuys - May 1936 - 2039279
Method of setting the twist of rayon yarn
Hood - August 1936 - 2050325
/2251962.html
Sommaripa - August 1941 - 2251962
Crepe thread and method of making same
Schneider et al. - December 1941 - 2265202
Inventors:
Gomez, Climaco Alberto (Colonial Heights, VA)
Lewis, Marvin Dennis (Richmond, VA)
Twilley, Ian Charles (Chester, VA)
Lewis, Marvin Dennis (Richmond, VA)
Twilley, Ian Charles (Chester, VA)
Application Number:
05/421207
Publication Date:
03/25/1975
Filing Date:
12/03/1973
View Patent Images:
Export Citation:
Assignee:
Allied Chemical Corporation (Petersburg, VA)
Primary Class:
Other Classes:
57/282, 28/169, 28/166
International Classes:
D02G1/20; D02G1/02
Field of Search:
57/34HS,157TS,164,14R 28/72R,75WT,76R,75R,74R,74P
US Patent References:
Primary Examiner:
Petrakes, John
Claims:
We claim
1. The method of heat-setting twisted polycarbonamide continuous filament carpet yarn comprising
2. The method of heat-setting twisted polycaprolactam continuous filament carpet yarn comprising
3. The method of claim 2 wherein said tumbling temperature is selected from a range of from about 150° to 200°F. for about 6 to about 8 minutes.
4. The method of claim 2 wherein the heating medium for the tumbling step is steam.
5. The method of claim 2 wherein the heating medium for the tumbling step is hot air.
1. The method of heat-setting twisted polycarbonamide continuous filament carpet yarn comprising
2. The method of heat-setting twisted polycaprolactam continuous filament carpet yarn comprising
3. The method of claim 2 wherein said tumbling temperature is selected from a range of from about 150° to 200°F. for about 6 to about 8 minutes.
4. The method of claim 2 wherein the heating medium for the tumbling step is steam.
5. The method of claim 2 wherein the heating medium for the tumbling step is hot air.
Description:
BACKGROUND OF THE INVENTION
This invention relates to an improved method to heat set twisted polycarbonamide yarn.
Twisted and heat set polycarbonamide (nylon) bulked continuous filament yarn is extensively used in cut pile and frieze style carpets and other fabrics. The prior art method of producing this yarn from bulked continuous filament yarn consisted of twisting, skeining, tumbling and autoclaving followed by drying if necessary conditioning and backwinding from skeins onto a carrier to form a package of yarn. Autoclaving was considered essential in the prior art since it was believed that autoclaving the twisted yarn in high pressure steam for relatively long periods set the twist in the yarn structure. It is known in U.S. Pat. No. 2,695,509 to heat set twist in yarn by running a single end of yarn through a heating chamber, however, this yarn is not tumbled and not skeined.
SUMMARY OF THE INVENTION
The method of this invention omits autoclaving. The yarn is simply twisted, skeined and tumbled as skeins at a selected yarn temperature of between 100° and 240°F. preferably between 120° and 200°F. and even more preferably between 150° and 200°F. for a period of 2 to 30 minutes, preferably 2 to 10 and even more preferably 6 to 8 minutes. It has been found that no autoclaving is necessary when these conditions are used. The selected temperature during tumbling should be controlled to within ± 15°F. The yarn is then conditioned as skeins and backwound into a package of yarn. By conditioned is meant the yarn is cooled and/or dried or allowed to cool and/or dry at ambient conditions. Any of the polycarbonamide yarns can be used such as polycaprolactam (nylon 6) or polyhexamethylene adipamide (nylon 6,6). The heating medium can be either steam or hot air. Surprisingly, yarn which is twisted and heat set in this manner when tufted into a fabric such as a carpet and subsequently dyed with hot, wet agitation has excellent twist retention and entangled locked tuft tips when the tufts have been cut. The yarn made by the process of this invention also has greater bulk, ozone resistance, wear resistance and is more economical to produce. The excellent twist retention is uniform along the entire length of each tuft. The amount of agitation during tumbling is not critical and can be varied by the speed of agitation of the tumbler and by the amount of yarn agitated per tumbler load. The following tables contrast the prior art with the method of this invention and set forth the advantages over the prior art.
TABLE I ______________________________________ Prior Art Method of This Invention ______________________________________ Twisting Twisting Skeining Skeining Tumbling Tumbling Autoclaving Drying (optional) Cooling Cooling Backwinding Backwinding ______________________________________
TABLE II ____________________________________________________________ ______________ Greater Bulk The bulk of tumbled only yarn is greater than tumbled and autoclaved yarn. The linear density of tumbled only yarn is less than autoclaved yarn. Autoclaving "kills" bulk and raises linear density. Yarn made - by the process of this invention produces carpets with 20% greater bulk than comparable carpets produced with an equal amount of prior art yarn. Better Twist Because of higher residual yarn and crimp shrinkage of tumbled yarn, these Retention shrinkages in hot wet processing (dyeing) result in filament entanglements that lock the twist of the structure at the tip end of the cut tuft. Autoclaved yarns are not locked nearly as well and therefore have a - tendency to untwist. Better Walk-out Because of the locked tips with tumbled only yarn, the twisted structure Performance is much more stable upon floor wear. The autoclaved tips are unstable and the individual yarn components of the twisted structure separate resulting in flared or bursted tufts which is most undesirable. Improved Since lower temperatures and shorter exposure times are used for tumbled Atmospheric only yarn, the ozone resistance of the tumbled only dyed yarn is much Gas Fading and greater than for autoclaved dyed yarns. Dyeing uniformity is also improved. Dyeing Uniformity More Economical Since the autoclaving step is eliminated, the cost of throwing twisted Process structures is reduced because of less labor, less capital, and less floor space ____________________________________________________________ ______________
DESCRIPTION OF THE PREFERRED EMBODIMENTS
EXAMPLE I
A. A bright, amine terminated, bulked continuous filament polycaprolactam (nylon 6) 1,300 denier 70 filament yarn was twisted in a conventional manner to 3 turns per inch Z by 3 turns per inch S, skeined, and tumbled in steam at the yarn temperature given in the following tables. This acid dyeable yarn was then dried, if necessary, conditioned and the skeins were backwound into a conventional yarn package. The tumbling was carried out in a 100 No. Hubsch Commercial Dryer for about 7 minutes.
B. An identical yarn except for being produced from acid terminated polymer was processed in the same manner.
C. Yarns identical to those above were processed using hot air as the heating medium instead of steam.
EXAMPLE II
Method of Setting Twist in Control, Prior Art Yarn
A. Autoclaved -- The yarn of Example IA was processed by the prior art method by twisting to 3 tpi Z by 3 tpi S, skeining, tumbling with live steam at a yarn temperature of 140°F. for about 7 minutes, autoclaving for approximately 60 minutes at the cycle of vacuum and temperature conditions standard in the industry (maximum steam temperature during the cycle of 280°F.) conditioning to room temperature and backwinding into a conventional yarn package.
B. Autoclaved -- The yarn of Example IB was processed as above.
C. Single End Treatment -- The yarn described in Example IA and IB was processed as follows. A Relset 20 position machine with a 50 foot coil was run at 250 yards per minute to heat each end of yarn with hot air at 230°C. using a 170°C. band heater. The pressure was 30 psi in and 2-3 psi out. The band heater is located above the coils to heat them. The air is heated to temperature in the air storage tank with electrical resistance heaters or other heating means.
TABLE III ______________________________________ Carpet Tuft Tip Coherency ______________________________________ Yarn Yarn from Temperature After Wear Example in Tumbling Before Wear and Cleaning ______________________________________ IA 140°F. 16.6 21.0 IB 140°F. 16.9 33.7 IIA 5.5 12.0* IIB 5.2 18.7* ______________________________________ *Increase in force due to entanglements below the tip in spite of excessive opening at the tip, tip flare was noticeable.
These values are an average of 40 test observations of yarn from a tufted carpet before and after 10,000 treads test as described below. The "10,000 treads" means the carpet had 10,000 footsteps of actual persons walking on the carpet in a hallway as counted by a counter under a mat in the same hallway.
DESCRIPTION OF TIP COHERENCY TEST
Purpose:
The tip coherency test measures the degree of filament bonding of shag carpet tufts at their tips.
Principle:
This test measures the force in grams required to separate the tip of a shag carpet tuft composed of two yarns twisted together.
Procedure:
1. Cut a tuft from the carpet.
2. Separate the yarns at the base of the tuft and continue the separation up to about one-fourth inch from the tip.
3. Grip the two yarn ends in an Instron Tensile Tester.
4. Start the Instron with a cross-head speed of 5 inches per minute.
5. Record the force in grams required to completely separate the two twisted yarns.
6. Test a representative number of tufts and report Tip Coherency as the average force required. Table IIIa shows visual appearance before and after wear. Results show carpet in low weight carpet made of yarn of this invention is superior after wear.
TABLE IIIa ______________________________________ Visual Appearance Before And After Wear (10,000 Treads) ______________________________________ High Weight Carpet Low Weight Carpet Yarn from (24 oz/yd 2 ) (9-14 oz/yd 2 ) Example Before After Before After ______________________________________ IA & B 1 1 1 1 (140°F. Tumbling) IIC 1 2 1 2 IIA & B 2 4 2 5 ______________________________________ (Scale: 1 - 5 Best to Worst)?
TABLE IV ______________________________________ Bulk Test Yarn from Bulk in Example cc/gram ______________________________________ IA (Tumbled yarn 17.9 (average of two observations) temperature - 140°F.) IIA 15.3 (average of two observations) ______________________________________
Yarn processed on the Relset machines has about the same bulk as IA.
Bulk Measurement
Purpose:
To measure the volume occupied by a known mass of yarn.
Principle:
This test measures the volume in ml. occupied by 1 gram of yarn in a 1 inch diameter tube under a stress of 150 gm/in 2 .
Procedure:
1. Weigh out exactly one gram of yarn. The yarn may be from packages, skeins, or carpets.
2. Cut the yarns into three-fourth inch lengths and allow to fall into a 100 ml. graduated cylinder (1 inch inside diameter).
3. Place a 1 inch drill rod weighing 118 grams (150 gm/in 2 ) into the cylinder and allow to compress the yarn for 30 seconds.
4. Read the volume in ml. of the 1 gram of yarn.
Significance:
Results obtained with above bulk measurement test have been correlated with a bulk measurement in carpets as shown in Table IV.
TABLE V ____________________________________________________________ ______________ Carpet Appearance Evaluation ____________________________________________________________ ______________ Yarn Yarn from Temperature Oz yarn per Tip Example In Tumbling Sq/Yd Carpet Bulk Flare Hand Resilience Hariness ____________________________________________________________ ______________ IIA & B -- 24 B - C+ C+ C+ C+ IA & B 165°F. 24 A - B+ C+ C+ C IA & B 185°F. 24 A - B+ C+ C+ C IIC -- 24 A - B+ C+ C+ C IC 150°F. 24 A - B+ C+ C+ C - IA & B 165°F. 21.5 B+ B+ C+ C+ C IA & B 185°F. 21.5 B+ B+ C+ C+ C IIC -- 21.5 B+ B+ C+ C+ C IC 150°F. 21.5 B+ B+ C+ C+ C - IA & B 165°F. 19 C+ B+ C+ C+ C IA & B 185°F. 19 C+ B+ C+ C+ C ____________________________________________________________ ______________ Carpets were tufted end and end (with acid terminated yarn and amine terminated yarn in alternating rows) and evaluated visually according to the following grading system: A -- Excellent B -- Good C -- Average D -- Poor
The method of testing for ozone fading is similar to the AATCC Test 129-1968 set forth on page 334/15 of The Journal of American Association of Textile Chemists and Colorists, July 30, 1969, Volume 1, No. 16, in an article entitled, "A New Test Method for Ozone Fading at High Humidity," by Victor S. Salvin.
The method and the means of measuring the loss of dye consists in dyeing the yarn with a selected dye or dyes, exposing it to ozone at a concentration of 20 parts per hundred million in a test chamber 104°F. and 90% relative humidity together with a control nylon sample which was dyed an avocado shade. The control sample is examined periodically until the resulting color corresponds to that of the Standard of Fading (one cycle). It has been found that one cycle is completed when the internal standard has faded sufficiently to give a ΔE of 2.8, compared to the unexposed standard.
ΔE is a measure of the change of color between two samples, a smaller ΔE being a closer match, or less fading of one sample compared to the second sample.
This color difference, ΔE, was measured with a Hunterlab Color Difference Meter. This instrument measures color as seen in average daylight in a manner similar to the way in which the human eye responds to the stimulus of color. Experimentation has shown that the eye can match any color with a combination of three "primary" colored lights, and therefore, that any color can be specified by a three dimensional identification. The Color Difference Meter measures the light reflected by a specimen through filters that correspond to the three "primary" lights. These measurements made correspond to the way the average human eye responds to light.
Δ E = √(ΔL) 2 + (Δa) 2 + (Δb) 2
where
ΔL is L 1 -L 2
Δa is a 1 -a 2
Δb is b 1 -b 2
and L, a, and b are readings on the Hunterlab Color Difference Meter. L is a 100 to 0 reading of white to black; a indicates redness when positive, gray when zero, and green when negative; b indicates yellow when positive, gray when zero and blue when negative.
TABLE VI ____________________________________________________________ ______________ Ozone Fading ____________________________________________________________ ______________ Exposure to 0 3 Yarn from 6 Hours 12 Hours 18 Hours Yarn Tumbling Example ΔL ΔE ΔL ΔE ΔL ΔE Temperature Dyed ____________________________________________________________ ______________ IA 1.6 2.1 3.1 4.0 4.9 6.3 100°F. Disperse Olive II IA 1.2 1.7 2.5 3.6 3.3 4.8 120°F. Disperse Olive II IA .9 1.4 2.4 3.6 3.3 4.7 140°F. Disperse Olive II IA .6 1.3 3.0 4.1 4.4 5.9 170°F. Disperse Olive II IA .9 1.4 2.8 3.8 4.0 5.4 190°F. Disperse Olive II IB .6 1.3 1.4 2.3 2.6 3.9 100°F. Disperse Olive II IB 1.1 1.6 2.0 3.0 2.9 4.3 120°F. Disperse Olive II IB 1.4 1.9 2.1 3.0 3.0 4.1 140°F. Disperse Olive II IB .4 1.0 1.6 2.6 3.4 4.0 170°F. Disperse Olive II IB .7 1.4 1.6 2.8 3.0 4.5 190°F. Disperse Olive II IIA 1.7 2.2 3.6 5.2 5.2 7.1 -- Disperse Olive II IIA .2 .6 1.5 1.9 2.0 2.5 -- Acid Moss Green IIB 1.1 1.8 4.1 6.1 5.9 8.5 -- Disperse Olive II IIB 1.4 2.0 3.5 5.7 5.5 9.2 -- Acid Moss Green IA .8 1.1 1.6 2.1 1.1 2.1 100°F. Acid Moss Green IA .7 .9 1.5 1.9 1.8 2.5 120°F. Acid Moss Green IA .9 1.2 1.3 1.8 2.0 2.8 140°F. Acid Moss Green IA .9 1.1 .5 1.3 1.5 2.3 170°F. Acid Moss Green IA .4 .6 .9 1.3 1.5 2.2 190°F. Acid Moss Green IB .9 1.3 2.3 3.4 2.6 4.1 100°F. Acid Moss Green IB 1.6 2.0 2.4 3.5 2.6 4.2 120°F. Acid Moss Green IB 1.2 1.6 2.1 2.9 3.1 4.7 140°F. Acid Moss Green IB 1.0 1.4 2.1 3.1 3.1 4.7 170°F. Acid Moss Green IB 1.4 1.8 2.1 3.3 3.5 5.3 190°F. Acid Moss Green ____________________________________________________________ ______________
The formulation of the moss green dyebath is given on page 7 of allowed U.S. Ser. No. 223,772, filed Feb. 4, 1973, hereby incorporated by reference.
The formulation of the Olive II dyebath is as follows:
0.082% Latyl Cerise Y (DuPont)
0.44% Celliton Yellow GA (C. I. 11855)
0.143% celanthrene Blue CR (DuPont)
2% trisodium phosphate
0.5% Triton X-100 (ethoxylated nonylphenol)
This invention relates to an improved method to heat set twisted polycarbonamide yarn.
Twisted and heat set polycarbonamide (nylon) bulked continuous filament yarn is extensively used in cut pile and frieze style carpets and other fabrics. The prior art method of producing this yarn from bulked continuous filament yarn consisted of twisting, skeining, tumbling and autoclaving followed by drying if necessary conditioning and backwinding from skeins onto a carrier to form a package of yarn. Autoclaving was considered essential in the prior art since it was believed that autoclaving the twisted yarn in high pressure steam for relatively long periods set the twist in the yarn structure. It is known in U.S. Pat. No. 2,695,509 to heat set twist in yarn by running a single end of yarn through a heating chamber, however, this yarn is not tumbled and not skeined.
SUMMARY OF THE INVENTION
The method of this invention omits autoclaving. The yarn is simply twisted, skeined and tumbled as skeins at a selected yarn temperature of between 100° and 240°F. preferably between 120° and 200°F. and even more preferably between 150° and 200°F. for a period of 2 to 30 minutes, preferably 2 to 10 and even more preferably 6 to 8 minutes. It has been found that no autoclaving is necessary when these conditions are used. The selected temperature during tumbling should be controlled to within ± 15°F. The yarn is then conditioned as skeins and backwound into a package of yarn. By conditioned is meant the yarn is cooled and/or dried or allowed to cool and/or dry at ambient conditions. Any of the polycarbonamide yarns can be used such as polycaprolactam (nylon 6) or polyhexamethylene adipamide (nylon 6,6). The heating medium can be either steam or hot air. Surprisingly, yarn which is twisted and heat set in this manner when tufted into a fabric such as a carpet and subsequently dyed with hot, wet agitation has excellent twist retention and entangled locked tuft tips when the tufts have been cut. The yarn made by the process of this invention also has greater bulk, ozone resistance, wear resistance and is more economical to produce. The excellent twist retention is uniform along the entire length of each tuft. The amount of agitation during tumbling is not critical and can be varied by the speed of agitation of the tumbler and by the amount of yarn agitated per tumbler load. The following tables contrast the prior art with the method of this invention and set forth the advantages over the prior art.
TABLE I ______________________________________ Prior Art Method of This Invention ______________________________________ Twisting Twisting Skeining Skeining Tumbling Tumbling Autoclaving Drying (optional) Cooling Cooling Backwinding Backwinding ______________________________________
TABLE II ____________________________________________________________ ______________ Greater Bulk The bulk of tumbled only yarn is greater than tumbled and autoclaved yarn. The linear density of tumbled only yarn is less than autoclaved yarn. Autoclaving "kills" bulk and raises linear density. Yarn made - by the process of this invention produces carpets with 20% greater bulk than comparable carpets produced with an equal amount of prior art yarn. Better Twist Because of higher residual yarn and crimp shrinkage of tumbled yarn, these Retention shrinkages in hot wet processing (dyeing) result in filament entanglements that lock the twist of the structure at the tip end of the cut tuft. Autoclaved yarns are not locked nearly as well and therefore have a - tendency to untwist. Better Walk-out Because of the locked tips with tumbled only yarn, the twisted structure Performance is much more stable upon floor wear. The autoclaved tips are unstable and the individual yarn components of the twisted structure separate resulting in flared or bursted tufts which is most undesirable. Improved Since lower temperatures and shorter exposure times are used for tumbled Atmospheric only yarn, the ozone resistance of the tumbled only dyed yarn is much Gas Fading and greater than for autoclaved dyed yarns. Dyeing uniformity is also improved. Dyeing Uniformity More Economical Since the autoclaving step is eliminated, the cost of throwing twisted Process structures is reduced because of less labor, less capital, and less floor space ____________________________________________________________ ______________
DESCRIPTION OF THE PREFERRED EMBODIMENTS
EXAMPLE I
A. A bright, amine terminated, bulked continuous filament polycaprolactam (nylon 6) 1,300 denier 70 filament yarn was twisted in a conventional manner to 3 turns per inch Z by 3 turns per inch S, skeined, and tumbled in steam at the yarn temperature given in the following tables. This acid dyeable yarn was then dried, if necessary, conditioned and the skeins were backwound into a conventional yarn package. The tumbling was carried out in a 100 No. Hubsch Commercial Dryer for about 7 minutes.
B. An identical yarn except for being produced from acid terminated polymer was processed in the same manner.
C. Yarns identical to those above were processed using hot air as the heating medium instead of steam.
EXAMPLE II
Method of Setting Twist in Control, Prior Art Yarn
A. Autoclaved -- The yarn of Example IA was processed by the prior art method by twisting to 3 tpi Z by 3 tpi S, skeining, tumbling with live steam at a yarn temperature of 140°F. for about 7 minutes, autoclaving for approximately 60 minutes at the cycle of vacuum and temperature conditions standard in the industry (maximum steam temperature during the cycle of 280°F.) conditioning to room temperature and backwinding into a conventional yarn package.
B. Autoclaved -- The yarn of Example IB was processed as above.
C. Single End Treatment -- The yarn described in Example IA and IB was processed as follows. A Relset 20 position machine with a 50 foot coil was run at 250 yards per minute to heat each end of yarn with hot air at 230°C. using a 170°C. band heater. The pressure was 30 psi in and 2-3 psi out. The band heater is located above the coils to heat them. The air is heated to temperature in the air storage tank with electrical resistance heaters or other heating means.
TABLE III ______________________________________ Carpet Tuft Tip Coherency ______________________________________ Yarn Yarn from Temperature After Wear Example in Tumbling Before Wear and Cleaning ______________________________________ IA 140°F. 16.6 21.0 IB 140°F. 16.9 33.7 IIA 5.5 12.0* IIB 5.2 18.7* ______________________________________ *Increase in force due to entanglements below the tip in spite of excessive opening at the tip, tip flare was noticeable.
These values are an average of 40 test observations of yarn from a tufted carpet before and after 10,000 treads test as described below. The "10,000 treads" means the carpet had 10,000 footsteps of actual persons walking on the carpet in a hallway as counted by a counter under a mat in the same hallway.
DESCRIPTION OF TIP COHERENCY TEST
Purpose:
The tip coherency test measures the degree of filament bonding of shag carpet tufts at their tips.
Principle:
This test measures the force in grams required to separate the tip of a shag carpet tuft composed of two yarns twisted together.
Procedure:
1. Cut a tuft from the carpet.
2. Separate the yarns at the base of the tuft and continue the separation up to about one-fourth inch from the tip.
3. Grip the two yarn ends in an Instron Tensile Tester.
4. Start the Instron with a cross-head speed of 5 inches per minute.
5. Record the force in grams required to completely separate the two twisted yarns.
6. Test a representative number of tufts and report Tip Coherency as the average force required. Table IIIa shows visual appearance before and after wear. Results show carpet in low weight carpet made of yarn of this invention is superior after wear.
TABLE IIIa ______________________________________ Visual Appearance Before And After Wear (10,000 Treads) ______________________________________ High Weight Carpet Low Weight Carpet Yarn from (24 oz/yd 2 ) (9-14 oz/yd 2 ) Example Before After Before After ______________________________________ IA & B 1 1 1 1 (140°F. Tumbling) IIC 1 2 1 2 IIA & B 2 4 2 5 ______________________________________ (Scale: 1 - 5 Best to Worst)?
TABLE IV ______________________________________ Bulk Test Yarn from Bulk in Example cc/gram ______________________________________ IA (Tumbled yarn 17.9 (average of two observations) temperature - 140°F.) IIA 15.3 (average of two observations) ______________________________________
Yarn processed on the Relset machines has about the same bulk as IA.
Bulk Measurement
Purpose:
To measure the volume occupied by a known mass of yarn.
Principle:
This test measures the volume in ml. occupied by 1 gram of yarn in a 1 inch diameter tube under a stress of 150 gm/in 2 .
Procedure:
1. Weigh out exactly one gram of yarn. The yarn may be from packages, skeins, or carpets.
2. Cut the yarns into three-fourth inch lengths and allow to fall into a 100 ml. graduated cylinder (1 inch inside diameter).
3. Place a 1 inch drill rod weighing 118 grams (150 gm/in 2 ) into the cylinder and allow to compress the yarn for 30 seconds.
4. Read the volume in ml. of the 1 gram of yarn.
Significance:
Results obtained with above bulk measurement test have been correlated with a bulk measurement in carpets as shown in Table IV.
TABLE V ____________________________________________________________ ______________ Carpet Appearance Evaluation ____________________________________________________________ ______________ Yarn Yarn from Temperature Oz yarn per Tip Example In Tumbling Sq/Yd Carpet Bulk Flare Hand Resilience Hariness ____________________________________________________________ ______________ IIA & B -- 24 B - C+ C+ C+ C+ IA & B 165°F. 24 A - B+ C+ C+ C IA & B 185°F. 24 A - B+ C+ C+ C IIC -- 24 A - B+ C+ C+ C IC 150°F. 24 A - B+ C+ C+ C - IA & B 165°F. 21.5 B+ B+ C+ C+ C IA & B 185°F. 21.5 B+ B+ C+ C+ C IIC -- 21.5 B+ B+ C+ C+ C IC 150°F. 21.5 B+ B+ C+ C+ C - IA & B 165°F. 19 C+ B+ C+ C+ C IA & B 185°F. 19 C+ B+ C+ C+ C ____________________________________________________________ ______________ Carpets were tufted end and end (with acid terminated yarn and amine terminated yarn in alternating rows) and evaluated visually according to the following grading system: A -- Excellent B -- Good C -- Average D -- Poor
The method of testing for ozone fading is similar to the AATCC Test 129-1968 set forth on page 334/15 of The Journal of American Association of Textile Chemists and Colorists, July 30, 1969, Volume 1, No. 16, in an article entitled, "A New Test Method for Ozone Fading at High Humidity," by Victor S. Salvin.
The method and the means of measuring the loss of dye consists in dyeing the yarn with a selected dye or dyes, exposing it to ozone at a concentration of 20 parts per hundred million in a test chamber 104°F. and 90% relative humidity together with a control nylon sample which was dyed an avocado shade. The control sample is examined periodically until the resulting color corresponds to that of the Standard of Fading (one cycle). It has been found that one cycle is completed when the internal standard has faded sufficiently to give a ΔE of 2.8, compared to the unexposed standard.
ΔE is a measure of the change of color between two samples, a smaller ΔE being a closer match, or less fading of one sample compared to the second sample.
This color difference, ΔE, was measured with a Hunterlab Color Difference Meter. This instrument measures color as seen in average daylight in a manner similar to the way in which the human eye responds to the stimulus of color. Experimentation has shown that the eye can match any color with a combination of three "primary" colored lights, and therefore, that any color can be specified by a three dimensional identification. The Color Difference Meter measures the light reflected by a specimen through filters that correspond to the three "primary" lights. These measurements made correspond to the way the average human eye responds to light.
Δ E = √(ΔL) 2 + (Δa) 2 + (Δb) 2
where
ΔL is L 1 -L 2
Δa is a 1 -a 2
Δb is b 1 -b 2
and L, a, and b are readings on the Hunterlab Color Difference Meter. L is a 100 to 0 reading of white to black; a indicates redness when positive, gray when zero, and green when negative; b indicates yellow when positive, gray when zero and blue when negative.
TABLE VI ____________________________________________________________ ______________ Ozone Fading ____________________________________________________________ ______________ Exposure to 0 3 Yarn from 6 Hours 12 Hours 18 Hours Yarn Tumbling Example ΔL ΔE ΔL ΔE ΔL ΔE Temperature Dyed ____________________________________________________________ ______________ IA 1.6 2.1 3.1 4.0 4.9 6.3 100°F. Disperse Olive II IA 1.2 1.7 2.5 3.6 3.3 4.8 120°F. Disperse Olive II IA .9 1.4 2.4 3.6 3.3 4.7 140°F. Disperse Olive II IA .6 1.3 3.0 4.1 4.4 5.9 170°F. Disperse Olive II IA .9 1.4 2.8 3.8 4.0 5.4 190°F. Disperse Olive II IB .6 1.3 1.4 2.3 2.6 3.9 100°F. Disperse Olive II IB 1.1 1.6 2.0 3.0 2.9 4.3 120°F. Disperse Olive II IB 1.4 1.9 2.1 3.0 3.0 4.1 140°F. Disperse Olive II IB .4 1.0 1.6 2.6 3.4 4.0 170°F. Disperse Olive II IB .7 1.4 1.6 2.8 3.0 4.5 190°F. Disperse Olive II IIA 1.7 2.2 3.6 5.2 5.2 7.1 -- Disperse Olive II IIA .2 .6 1.5 1.9 2.0 2.5 -- Acid Moss Green IIB 1.1 1.8 4.1 6.1 5.9 8.5 -- Disperse Olive II IIB 1.4 2.0 3.5 5.7 5.5 9.2 -- Acid Moss Green IA .8 1.1 1.6 2.1 1.1 2.1 100°F. Acid Moss Green IA .7 .9 1.5 1.9 1.8 2.5 120°F. Acid Moss Green IA .9 1.2 1.3 1.8 2.0 2.8 140°F. Acid Moss Green IA .9 1.1 .5 1.3 1.5 2.3 170°F. Acid Moss Green IA .4 .6 .9 1.3 1.5 2.2 190°F. Acid Moss Green IB .9 1.3 2.3 3.4 2.6 4.1 100°F. Acid Moss Green IB 1.6 2.0 2.4 3.5 2.6 4.2 120°F. Acid Moss Green IB 1.2 1.6 2.1 2.9 3.1 4.7 140°F. Acid Moss Green IB 1.0 1.4 2.1 3.1 3.1 4.7 170°F. Acid Moss Green IB 1.4 1.8 2.1 3.3 3.5 5.3 190°F. Acid Moss Green ____________________________________________________________ ______________
The formulation of the moss green dyebath is given on page 7 of allowed U.S. Ser. No. 223,772, filed Feb. 4, 1973, hereby incorporated by reference.
The formulation of the Olive II dyebath is as follows:
0.082% Latyl Cerise Y (DuPont)
0.44% Celliton Yellow GA (C. I. 11855)
0.143% celanthrene Blue CR (DuPont)
2% trisodium phosphate
0.5% Triton X-100 (ethoxylated nonylphenol)