CA1154215A - Self crimping yarn and process - Google Patents
Self crimping yarn and processInfo
- Publication number
- CA1154215A CA1154215A CA000309498A CA309498A CA1154215A CA 1154215 A CA1154215 A CA 1154215A CA 000309498 A CA000309498 A CA 000309498A CA 309498 A CA309498 A CA 309498A CA 1154215 A CA1154215 A CA 1154215A
- Authority
- CA
- Canada
- Prior art keywords
- streams
- filament
- filaments
- cross
- sectional area
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002788 crimping Methods 0.000 title claims abstract description 9
- 229920000728 polyester Polymers 0.000 claims abstract description 15
- 238000010791 quenching Methods 0.000 claims abstract description 10
- 230000000171 quenching effect Effects 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims description 19
- 150000002148 esters Chemical class 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 2
- 230000002301 combined effect Effects 0.000 claims 2
- 230000002844 continuous effect Effects 0.000 claims 1
- 238000009987 spinning Methods 0.000 description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/32—Side-by-side structure; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Artificial Filaments (AREA)
- Multicomponent Fibers (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE This invention provides a process for producing a variable denier filament. The process comprises the steps of generating two individual streams of molten polyester of fiber-forming molecular weight travelling at different velocities; converging the individual streams side-by-side to form a combined strem; quenching the combined stream to form a combined filament and withdrawing the filament from the combined stream at a rate of speed in excess of 2500 meters per minute. Also provided is a self-crimping yarn which comprises a plurality of polyester continuous filaments. The filaments of the yarn have non-round cross-sectional areas which vary substantially regularly along the lengths of the filaments from regions of large cross-sectional area to regions of small cross-sectional area, the variation in cross-sectional area being mole than ? 10% about a mean value. The regions of large and small cross-sectional area are out of phase from filament to filament to thereby form the self-crimping yarn and the polyester continuous filaments of the yarn are formed by the above process.
Description
C- 54-0288 ~ Zl~
SELF CRIMPING YARN AND PROCESS
SPECIFICATION
The invention relates to novel processes for making polyester self-texturing yarns, and to the resulting yarns. ~--~Iore particularly, the process invention relates to such a ~ ;
spinning process wherein two molten streams of the same~
polyester polymer are combined and spun to give novel and useful yarns.
It is known to make~self-crimp~ing yarns by combining converging streams~ of dlfferent~jet stretch and cooling the combined streams into a filament, followed by a drawing ~ operatlon. Such prlor art proc~esses are di~scl~osed in U.S.
;~ patents 3,387,327;to Privott et al and 3,4g7,585 to Chapman et al.
It has~been dlscovered that,~by operating at speeds far in excess of those dis~closed in t~e Privott et al and Chapman et al patents, an~improved process and uniquely useful products are~provLded.
Accordlng~to a~flrst ma~or aspect of the mventlon, ~ ;;
there is provided a;~process~for~producing~a seIf-crlmp~ing~
filament, comprising generating two individual streams of~
molten polyester of flber-formlng~molecular weight,~the individual streams travelling at dlfferent velocities, con-verging the individual streams side-by-side to form a combined stream, quenching the comblned str;eam to form a combined filament, and withdrawlng the comblned filament from the combined stream at~a rate of speed ln excess of 2500 meters per ,, minute and selected such that an individual filament quenched from one of the individual streams would have a shrinkage at least ten percentage points hi:gher than that of an lnd~ividual ~ B
. .
~ . . .
- ~154~-15 C~ 54-0288 filament quenched from the other of the individual streams.
According to another aspect of the invention, one of the individual streams has a velocity between 2.0 and 7 times as high as the velocity of the other of the streams. According to another aspect of the invention, one of the individual streams has a velocity between 3.5 and 5.5 times as high as the velocity of the other of the streams. According to another aspect of the invention, one of the individual streams has a smaller cross-sectional area than the other of the streams.
According to another aspect of the invention, the rate of s~eed is selected such that the combined filament has a shrinkage less than 30%. According to another aspect of the invention, the rate of speed is selected such that the combined filamerlt has a shrinkage less than 10%.
According to another major aspect of the invention, the invention comprises extruding molten polyester polymer through two spinneret passageways converging to merge substan-tially coincident with the face of the spinneret to define a combined orifice, the passageways being of different cross-sectional areas at least in the vicinity of the face, q~enchingthe resulting merged stream to form a filament, and withdrawing the filament from the merged stream at a rate of speed in excess of 3000 meters per minute and selected such that a filament spun solely from the larger of the passageways at the same jet stretch for the larger of the passageways would have a shrinkage at least ten percentage points lower tha~ that of a filament spun solely from the smaller o~ the passageways at the same jet stretch for the smaller of the passageways.
According to another major aspect of the invention, there is provided a process comprising generating a pair of streams of molten polymer of fiber-forming molecular weight travelling at different speeds to converge at a point below a C-14-54-0288 l~S~5 spinneret face, the speeds and momenta of the streams and the angle at which the streams converge being selected such that the first of the streams is slower and travels in substantially a straight line after the point at which the streams first touch and the second of the streams is fas~er and forms sinuous loops back and forth between successive points of attachment with the first of the streams.
According to another major aspect of the invention, there is provided a process for producing a variable denier filament, comprising generating a pair of streams of molten polymer of fiber-for~Ling molecular weight travelling at differ-ent speeds to converge at a point below a spinneret face, the speeds of the streams and the angle at which the streams converge being selected such that the first of the streams is slower and travels in substantially a straight line àfter the point at which the streams firs~ touch and attach and the second of the streams is faster and orms sinuous loops back and forth between successive points of attachment with the first of the streams; attenuating the first of the streams whereby the sinuous ~loops become straightened and the second of the streams is brought into continuous contact with the first of the streams; and quenching the resulting combined stream into a filament. According to a further aspect of the invention, the first of the streams is larger in cross section than the second of the streams. According to a further a.spect of the invention, there is provided a process for prod~Lcing a multi-filament variable denier yarn comprising simultaneously performing the process referred to above using a plurality of combined orifices in a common spinneret and supp~lied by a common poly~Ler source, the geometries of the combined orifices and the spinning conditions being selected such that the resulting ~ilaments have successive thick and thin regions which are out of phase from filament to filament.
According to another major aspect of the invention there is provided a yarn having a plurality of filaments comprising non-round cross-sections which repe~itively vary in area by more than ~ L0% along the lengths of the filaments, and alternating S-twisted and Z-twisted helically crimped sections, the variations in cross-sectional area being out of phase from filament to filament and the helically crimped sections being out of phase from filament to filament. Accord-ing to another aspect of the invention, the cross-sec~ions repetitively vary in area by more than ~ 25% (preferably more than ~ 30%) along the length of the filaments. According to another aspect of the invention, the yarn has a Uster une~en-ness of at least 2~5~/o U.
According to another major aspect of the invention there is provided a multifilament yarn comprising a plurality of continuous filaments comprising non round cross-sectional areas which vary repetitively along the lengths thereof, and variable pitch S-twisted and Z-twisted helically cailed sections, the sections being less tightly coiled in regions of large cross-sectional areas than in regions of small cross-sectional areas. According to another aspect of the invention, each of the filaments is formed ~rom a single molten polymer.
According to another aspect of the invention there is provided a spi~neret plate comprising a combined orifice, the combined orifice co~lprising a capillary having a large cross-sectional area and a capillary having a small cross-sectional area, the capillaries providing communication between the ILS~15 face of the plate and the opposite side of the plate and converging toward one another as the capillaries approach the face, the lengths of the capillaries being selected such that the capillary having a small cross-sectional area has less resistance to polymer flow than the capillary having a large cross-sectional area.
Other aspects of the invention will in part be obvious and will in part be disclosed in the following description taken in connection with the accompanying drawings, wherein:
FIGURE 1 is a vertical sectional view of the preferred embodiment of a spinneret usable according to the invention;
C-14-54-0~88 ~S~
FIGURE 2 is a bottom plan view of the FIGURE 1 spinneret, looking up;
FIGURE 3 is a graph of shrinkage versus spinning speed used in explaining the principles upon which certain aspects of the invention are based;
FIGURE 4 is a cross-sectional view of a filament according to certain aspects of the invention;
FIGURE 5 is a side elevation view of ~he molten streams issuing from the FIGURE 1 spinneret according to certain aspec~s of the invention;
FIGURE 6 is a graph illustrating the variation in denier along a representative filament according to certain aspects of the invention; and FIGURE 7 is a graph illustrating the distribution of the fluctuations illustrated in FIGURE 5 for a representative multiple oriice spinnere~ according to certain aspects of the invention.
The invention will be specifically exemplified using polyester polymer, it being understood that certain aspects of the invention are applicable to the class of melt-spinnable polymers generally. "Polyester;' as used herein means fiber-forming polymers at least 85% by weight of which is formable by reacting a dihydric alcohol with terephthalic acid.
Polyester typically is formed either by direct esterification of ethylene glycol with terephthalic acid, or by ester inter-change between ethylene glycol and dimethylterephthalate.
FIGURES 1 and 2 illustrate the preferred embodiment of a spinneret design which can be employed for obtaining all aspects of the invention. The spinneret includes a large counterbore 20 formed in the upper surface 21 of spinneret plate 22. Small counterbore 24 is formed in the bottom of and at one side of large cou~terbore 20. A large capillary 26 C-14-54-02~8 ~ i S
extends from the bottom of large counterbore 20 at the side opposite small counterbore 24, and connects the bottom of large counterbore 20 with the lower surface 28 of plate 22.
Small capillary 30 connects the bottom of counterbore 24 with surface 28. Capillaries 26 and 30 are each inclined four degrees from the vertical, and thus have an included angle of eight degrees. Counterbore 20 has a diameter of 0.0625 inch (1.588 mm.), while counterbore 24 has a diameter of 0.031 inch (0.787 mm.). Capillary 26 has a diameter of 0.0165 inch (0.419 mm.) and a length of 0.150 inch (3.81 mm.), while capillary 30 has a diamete-r of 0.0102 inch (0.259 mm.) and a length of 0.0286 inch (0.726 mm.). Land 32 separates capillaries 26 and 30 as they emerge at surface 28, and has a wldth of 0.0056 inch (0.142 mm.). Plate 22 has a thickness of 0.554 inch (14.07 mm.). Capillaries 26 and 30 together with counterbores 20 and 24 constitute a combined orifice for spinning various novel and useful filaments according to the invention, as will be more particularly described hereinafter.
FIGURE 3 is a graph showing how polyester filament shrinkage varies with spinning speed for two illustrative cases of jet stretch. The curve in dotted lines shows tha~ the shrinkage falls from about 65~/o at 3400 ypm (about 3100 mpm) to about 5% at 5000 ypm (about 4500 mpm) when using spinneret capillaries having diameters of 0.063 inch (1.6 mm.) and when sirnultaneously spinning 34 such filaments to be false-twist draw-textured to yield a textured yarn having 150 denier. The solid curve shows that the shrinkage drops off at higher speeds when using spinneret capillaries having diameters of 0.015 inch (0.38 mm.) when similarly simultaneously spinning 34 such filaments to be false-twist draw-textured to yield a textured yarn having 150 denier. Using different capillary diameters produces a family of curves between, to the left, and to the ....
.... .. . ... . . ... . . . .. . ...
C-14-54-0288 ~5~ LS
right of those illustrated. The curves also can be shifted (for a given capillary diameter) by varying the polymer through-put. In other words, the curves can be shifted by varying the jet stretch, which is the ratio of yarn speed just after solidification to average speed of molten polymer in the capillary. It is thus possible to provide a combined orifice for spinning a composite filament of a single polymer wherein one side of the filament has a much higher shrinkage than the other side. This is done by selecting the individual capillaries to give different jet stretches, and also selecting the spinning speed within the range whereln an individual filament quenched from one of the individual streams would have a shrinkage at least ten percentage points higher than that of an individual filament ~uenched from the other o the individual streams. Under the spinning conditions illustrated in E'IGURE
3, at a spinning speed of 5000 yards per minute the individual streams would have shrinkages differing by about 25 percentage points. Combining these molten streams into a side-by-side configuration results in a highly crimped filament in its as-spun form, without the necessity of drawing the yarn to develop the crimp as in the Privott and Chapman patents noted above.
Such combining may be done uslng a spinneret design similar to that disclosed in FIGUR~ 1, or the spinneret may merge the two streams at or just prior to emergence of the streams from surface 28, In any event, the two streams merge substantially coincident with the face of the spinneret according to this aspect of the invention.
Advantageously, the spinneret is so designed that one of the individual streams has a velocity in its capillary between 2.0 and 7 times (preferably between 3.5 and 5.5 times) the velocity of the other of the streams in its capillary.
Further advantages are obtained when the fas~er of the two C-14-54-0288 1 ~ 54 ~ 1~
streams has a smaller cross-sectional area than the slower of the streams, particularly in degree of crimp and spinning stability. Productivity is increased when the spinning speed is selected such that the combined filament has a shrinkage less than 30%, and is maximized when the shrinkage is less than 10/~, .
Further aspects of the inventionJ applicable to melt-spinnable polymers as a class, are achievable by use of spinnerets wherein the streams intersect outside the spinneret.
As a specific example, molten polyester polymer of norm~l textile molecular weight is metered at a temperature of 290C.
through a spinneret having 34 combined orifices as above specifically disclosed. The polymer ~hroughpu~ is adjusted to produce filaments of 4 average denier per filament at a spinning speed of 52~0 yards per minute, the molten streams being conventionally quenched into filaments by transversely directed quenching air.
Under these spinning conditions a remarkable phenomenon occurs, as illustrated in FIGURE ~. Due to the geometry of the spinneret construction, the polymer flowing through the smaller capillaries 30 has a higher velocity than that flowing through the larger capillaries. The speeds and momenta of the paired streams iSSUillg from each combined ori~ice and the angle at which the streams converge outside the spinneret are such that the slower streams 34 travel in substan-tiallv strai~ht lines a~ter the Doints at which the paired streams first touch and attach, while each of the smaller and faster of the streams 36 forms sinuous loops back and forth between successive points of attachment 38 with its associated larger streams. This action can be readily observed using a stroboscopic light directed onto`the streams immediately below the spinneret face 28. As the molten streams accelerate away _ 9 _ l:~S~ S
C~ 54-0288 rom the spinneret, the slower stream attenuates between the points of attachment 38 and the loops of the faster stream become straightened until the faster stream is brought into continuous contact with the slower stream. The slower stream attenuates more between than at the points of first attachment, so that the resulting combined stream has a cross-section which is larger at the points of first attachment than in the regions between these points. The resulting combined stream is then further attenuated somewhat until it is solidified into a filament 40 by the transverse quench air.
Each solidified filament 40 has non-round cross-sectional areas which vary repetitively along its length, and, a~ter being heated while under low tension, has variable pitch S-twisted and Z~twisted helically coiled sections, the sections being less tigh~ly coiled in regions of large cross-sectional area than in regions of small cross-sectional area. As illustrated qualitatively in FIGURE 6, when using the above spinning conditions, the filament cross-sectional area repetitively varies at a repetition rate of about one per meter, although this can be varied by modifying the spinning conditions and the geometry of the spinnere~ passages.
Due to minor differences between combined orifices, temperature gradations across the spinneret, and other like deviations from exactly the same treatment for each pair of streams, a multiple orifice spinneret will typically provide somewhat different repetition rates among the several resulting streams and ~ilaments. An example of this is qualitatively shown in FIGURE 7, wherein is shown that various orifices produce somewhat different repetition rates as determined by stroboscopic examination of the comhined streams just below the spinneret face. In the resulting multifilament yarn, the filaments have non-round cross-sections which vary by more C `4~54-0288 :~S~Z~
than + lO~o along the length of the filaments, and alternating -S-twisted and Z-twisted helically crimped sections, the variations in cross-sectional areas being out of phase from filament to filament and the helically crimped sections being out of phase from filament to filament.
The multifilament yarn has various applications and end uses. When woven into a fabric, the fabric has a pleasing novelty effect, resembling in some respects a fabric containing yarns spun from staple fibers. Other novelty effects can readily be obtained by minor variations of the spinneret and spinning conditions.
For certain of these effects, it is advantageous that the filaments vary repetitively along their lengths by more than + 25% (preferably more than ~ 30%~ in cross-sectional area. The effects are particularly pronounced when the yarn has a Uster unevenness of at least 2.5% U. The Uster measure-ment is made using the Uster*Evenness Tester, Model C, together with integrator ITG-101 for this instrument. The yarn speed is 182.8 meters per minute (200 ypm), the service selector is set on normal, and the sensitivity selector is set to 12.5%.
The /0 U is read from the integrator after a sample run time of 5 minutes.
Shrinkage is determined by the method disclosed in this paragraph. Generally speaking, a sample yarn's initial length Lo is determined while the yarn is under a tension of 0.1 grams per denier. The yarn is then subjected to a tension of 0.0025 grams per denier and placed in an oven at 120C. for five minutes. The yarn is then removed from the oven, again subjected to a tension of 0.1 grams per denier and its length L2 determined. Shrinkage percentage equals Lo~L2 X 100 Lo * Trademark
SELF CRIMPING YARN AND PROCESS
SPECIFICATION
The invention relates to novel processes for making polyester self-texturing yarns, and to the resulting yarns. ~--~Iore particularly, the process invention relates to such a ~ ;
spinning process wherein two molten streams of the same~
polyester polymer are combined and spun to give novel and useful yarns.
It is known to make~self-crimp~ing yarns by combining converging streams~ of dlfferent~jet stretch and cooling the combined streams into a filament, followed by a drawing ~ operatlon. Such prlor art proc~esses are di~scl~osed in U.S.
;~ patents 3,387,327;to Privott et al and 3,4g7,585 to Chapman et al.
It has~been dlscovered that,~by operating at speeds far in excess of those dis~closed in t~e Privott et al and Chapman et al patents, an~improved process and uniquely useful products are~provLded.
Accordlng~to a~flrst ma~or aspect of the mventlon, ~ ;;
there is provided a;~process~for~producing~a seIf-crlmp~ing~
filament, comprising generating two individual streams of~
molten polyester of flber-formlng~molecular weight,~the individual streams travelling at dlfferent velocities, con-verging the individual streams side-by-side to form a combined stream, quenching the comblned str;eam to form a combined filament, and withdrawlng the comblned filament from the combined stream at~a rate of speed ln excess of 2500 meters per ,, minute and selected such that an individual filament quenched from one of the individual streams would have a shrinkage at least ten percentage points hi:gher than that of an lnd~ividual ~ B
. .
~ . . .
- ~154~-15 C~ 54-0288 filament quenched from the other of the individual streams.
According to another aspect of the invention, one of the individual streams has a velocity between 2.0 and 7 times as high as the velocity of the other of the streams. According to another aspect of the invention, one of the individual streams has a velocity between 3.5 and 5.5 times as high as the velocity of the other of the streams. According to another aspect of the invention, one of the individual streams has a smaller cross-sectional area than the other of the streams.
According to another aspect of the invention, the rate of s~eed is selected such that the combined filament has a shrinkage less than 30%. According to another aspect of the invention, the rate of speed is selected such that the combined filamerlt has a shrinkage less than 10%.
According to another major aspect of the invention, the invention comprises extruding molten polyester polymer through two spinneret passageways converging to merge substan-tially coincident with the face of the spinneret to define a combined orifice, the passageways being of different cross-sectional areas at least in the vicinity of the face, q~enchingthe resulting merged stream to form a filament, and withdrawing the filament from the merged stream at a rate of speed in excess of 3000 meters per minute and selected such that a filament spun solely from the larger of the passageways at the same jet stretch for the larger of the passageways would have a shrinkage at least ten percentage points lower tha~ that of a filament spun solely from the smaller o~ the passageways at the same jet stretch for the smaller of the passageways.
According to another major aspect of the invention, there is provided a process comprising generating a pair of streams of molten polymer of fiber-forming molecular weight travelling at different speeds to converge at a point below a C-14-54-0288 l~S~5 spinneret face, the speeds and momenta of the streams and the angle at which the streams converge being selected such that the first of the streams is slower and travels in substantially a straight line after the point at which the streams first touch and the second of the streams is fas~er and forms sinuous loops back and forth between successive points of attachment with the first of the streams.
According to another major aspect of the invention, there is provided a process for producing a variable denier filament, comprising generating a pair of streams of molten polymer of fiber-for~Ling molecular weight travelling at differ-ent speeds to converge at a point below a spinneret face, the speeds of the streams and the angle at which the streams converge being selected such that the first of the streams is slower and travels in substantially a straight line àfter the point at which the streams firs~ touch and attach and the second of the streams is faster and orms sinuous loops back and forth between successive points of attachment with the first of the streams; attenuating the first of the streams whereby the sinuous ~loops become straightened and the second of the streams is brought into continuous contact with the first of the streams; and quenching the resulting combined stream into a filament. According to a further aspect of the invention, the first of the streams is larger in cross section than the second of the streams. According to a further a.spect of the invention, there is provided a process for prod~Lcing a multi-filament variable denier yarn comprising simultaneously performing the process referred to above using a plurality of combined orifices in a common spinneret and supp~lied by a common poly~Ler source, the geometries of the combined orifices and the spinning conditions being selected such that the resulting ~ilaments have successive thick and thin regions which are out of phase from filament to filament.
According to another major aspect of the invention there is provided a yarn having a plurality of filaments comprising non-round cross-sections which repe~itively vary in area by more than ~ L0% along the lengths of the filaments, and alternating S-twisted and Z-twisted helically crimped sections, the variations in cross-sectional area being out of phase from filament to filament and the helically crimped sections being out of phase from filament to filament. Accord-ing to another aspect of the invention, the cross-sec~ions repetitively vary in area by more than ~ 25% (preferably more than ~ 30%) along the length of the filaments. According to another aspect of the invention, the yarn has a Uster une~en-ness of at least 2~5~/o U.
According to another major aspect of the invention there is provided a multifilament yarn comprising a plurality of continuous filaments comprising non round cross-sectional areas which vary repetitively along the lengths thereof, and variable pitch S-twisted and Z-twisted helically cailed sections, the sections being less tightly coiled in regions of large cross-sectional areas than in regions of small cross-sectional areas. According to another aspect of the invention, each of the filaments is formed ~rom a single molten polymer.
According to another aspect of the invention there is provided a spi~neret plate comprising a combined orifice, the combined orifice co~lprising a capillary having a large cross-sectional area and a capillary having a small cross-sectional area, the capillaries providing communication between the ILS~15 face of the plate and the opposite side of the plate and converging toward one another as the capillaries approach the face, the lengths of the capillaries being selected such that the capillary having a small cross-sectional area has less resistance to polymer flow than the capillary having a large cross-sectional area.
Other aspects of the invention will in part be obvious and will in part be disclosed in the following description taken in connection with the accompanying drawings, wherein:
FIGURE 1 is a vertical sectional view of the preferred embodiment of a spinneret usable according to the invention;
C-14-54-0~88 ~S~
FIGURE 2 is a bottom plan view of the FIGURE 1 spinneret, looking up;
FIGURE 3 is a graph of shrinkage versus spinning speed used in explaining the principles upon which certain aspects of the invention are based;
FIGURE 4 is a cross-sectional view of a filament according to certain aspects of the invention;
FIGURE 5 is a side elevation view of ~he molten streams issuing from the FIGURE 1 spinneret according to certain aspec~s of the invention;
FIGURE 6 is a graph illustrating the variation in denier along a representative filament according to certain aspects of the invention; and FIGURE 7 is a graph illustrating the distribution of the fluctuations illustrated in FIGURE 5 for a representative multiple oriice spinnere~ according to certain aspects of the invention.
The invention will be specifically exemplified using polyester polymer, it being understood that certain aspects of the invention are applicable to the class of melt-spinnable polymers generally. "Polyester;' as used herein means fiber-forming polymers at least 85% by weight of which is formable by reacting a dihydric alcohol with terephthalic acid.
Polyester typically is formed either by direct esterification of ethylene glycol with terephthalic acid, or by ester inter-change between ethylene glycol and dimethylterephthalate.
FIGURES 1 and 2 illustrate the preferred embodiment of a spinneret design which can be employed for obtaining all aspects of the invention. The spinneret includes a large counterbore 20 formed in the upper surface 21 of spinneret plate 22. Small counterbore 24 is formed in the bottom of and at one side of large cou~terbore 20. A large capillary 26 C-14-54-02~8 ~ i S
extends from the bottom of large counterbore 20 at the side opposite small counterbore 24, and connects the bottom of large counterbore 20 with the lower surface 28 of plate 22.
Small capillary 30 connects the bottom of counterbore 24 with surface 28. Capillaries 26 and 30 are each inclined four degrees from the vertical, and thus have an included angle of eight degrees. Counterbore 20 has a diameter of 0.0625 inch (1.588 mm.), while counterbore 24 has a diameter of 0.031 inch (0.787 mm.). Capillary 26 has a diameter of 0.0165 inch (0.419 mm.) and a length of 0.150 inch (3.81 mm.), while capillary 30 has a diamete-r of 0.0102 inch (0.259 mm.) and a length of 0.0286 inch (0.726 mm.). Land 32 separates capillaries 26 and 30 as they emerge at surface 28, and has a wldth of 0.0056 inch (0.142 mm.). Plate 22 has a thickness of 0.554 inch (14.07 mm.). Capillaries 26 and 30 together with counterbores 20 and 24 constitute a combined orifice for spinning various novel and useful filaments according to the invention, as will be more particularly described hereinafter.
FIGURE 3 is a graph showing how polyester filament shrinkage varies with spinning speed for two illustrative cases of jet stretch. The curve in dotted lines shows tha~ the shrinkage falls from about 65~/o at 3400 ypm (about 3100 mpm) to about 5% at 5000 ypm (about 4500 mpm) when using spinneret capillaries having diameters of 0.063 inch (1.6 mm.) and when sirnultaneously spinning 34 such filaments to be false-twist draw-textured to yield a textured yarn having 150 denier. The solid curve shows that the shrinkage drops off at higher speeds when using spinneret capillaries having diameters of 0.015 inch (0.38 mm.) when similarly simultaneously spinning 34 such filaments to be false-twist draw-textured to yield a textured yarn having 150 denier. Using different capillary diameters produces a family of curves between, to the left, and to the ....
.... .. . ... . . ... . . . .. . ...
C-14-54-0288 ~5~ LS
right of those illustrated. The curves also can be shifted (for a given capillary diameter) by varying the polymer through-put. In other words, the curves can be shifted by varying the jet stretch, which is the ratio of yarn speed just after solidification to average speed of molten polymer in the capillary. It is thus possible to provide a combined orifice for spinning a composite filament of a single polymer wherein one side of the filament has a much higher shrinkage than the other side. This is done by selecting the individual capillaries to give different jet stretches, and also selecting the spinning speed within the range whereln an individual filament quenched from one of the individual streams would have a shrinkage at least ten percentage points higher than that of an individual filament ~uenched from the other o the individual streams. Under the spinning conditions illustrated in E'IGURE
3, at a spinning speed of 5000 yards per minute the individual streams would have shrinkages differing by about 25 percentage points. Combining these molten streams into a side-by-side configuration results in a highly crimped filament in its as-spun form, without the necessity of drawing the yarn to develop the crimp as in the Privott and Chapman patents noted above.
Such combining may be done uslng a spinneret design similar to that disclosed in FIGUR~ 1, or the spinneret may merge the two streams at or just prior to emergence of the streams from surface 28, In any event, the two streams merge substantially coincident with the face of the spinneret according to this aspect of the invention.
Advantageously, the spinneret is so designed that one of the individual streams has a velocity in its capillary between 2.0 and 7 times (preferably between 3.5 and 5.5 times) the velocity of the other of the streams in its capillary.
Further advantages are obtained when the fas~er of the two C-14-54-0288 1 ~ 54 ~ 1~
streams has a smaller cross-sectional area than the slower of the streams, particularly in degree of crimp and spinning stability. Productivity is increased when the spinning speed is selected such that the combined filament has a shrinkage less than 30%, and is maximized when the shrinkage is less than 10/~, .
Further aspects of the inventionJ applicable to melt-spinnable polymers as a class, are achievable by use of spinnerets wherein the streams intersect outside the spinneret.
As a specific example, molten polyester polymer of norm~l textile molecular weight is metered at a temperature of 290C.
through a spinneret having 34 combined orifices as above specifically disclosed. The polymer ~hroughpu~ is adjusted to produce filaments of 4 average denier per filament at a spinning speed of 52~0 yards per minute, the molten streams being conventionally quenched into filaments by transversely directed quenching air.
Under these spinning conditions a remarkable phenomenon occurs, as illustrated in FIGURE ~. Due to the geometry of the spinneret construction, the polymer flowing through the smaller capillaries 30 has a higher velocity than that flowing through the larger capillaries. The speeds and momenta of the paired streams iSSUillg from each combined ori~ice and the angle at which the streams converge outside the spinneret are such that the slower streams 34 travel in substan-tiallv strai~ht lines a~ter the Doints at which the paired streams first touch and attach, while each of the smaller and faster of the streams 36 forms sinuous loops back and forth between successive points of attachment 38 with its associated larger streams. This action can be readily observed using a stroboscopic light directed onto`the streams immediately below the spinneret face 28. As the molten streams accelerate away _ 9 _ l:~S~ S
C~ 54-0288 rom the spinneret, the slower stream attenuates between the points of attachment 38 and the loops of the faster stream become straightened until the faster stream is brought into continuous contact with the slower stream. The slower stream attenuates more between than at the points of first attachment, so that the resulting combined stream has a cross-section which is larger at the points of first attachment than in the regions between these points. The resulting combined stream is then further attenuated somewhat until it is solidified into a filament 40 by the transverse quench air.
Each solidified filament 40 has non-round cross-sectional areas which vary repetitively along its length, and, a~ter being heated while under low tension, has variable pitch S-twisted and Z~twisted helically coiled sections, the sections being less tigh~ly coiled in regions of large cross-sectional area than in regions of small cross-sectional area. As illustrated qualitatively in FIGURE 6, when using the above spinning conditions, the filament cross-sectional area repetitively varies at a repetition rate of about one per meter, although this can be varied by modifying the spinning conditions and the geometry of the spinnere~ passages.
Due to minor differences between combined orifices, temperature gradations across the spinneret, and other like deviations from exactly the same treatment for each pair of streams, a multiple orifice spinneret will typically provide somewhat different repetition rates among the several resulting streams and ~ilaments. An example of this is qualitatively shown in FIGURE 7, wherein is shown that various orifices produce somewhat different repetition rates as determined by stroboscopic examination of the comhined streams just below the spinneret face. In the resulting multifilament yarn, the filaments have non-round cross-sections which vary by more C `4~54-0288 :~S~Z~
than + lO~o along the length of the filaments, and alternating -S-twisted and Z-twisted helically crimped sections, the variations in cross-sectional areas being out of phase from filament to filament and the helically crimped sections being out of phase from filament to filament.
The multifilament yarn has various applications and end uses. When woven into a fabric, the fabric has a pleasing novelty effect, resembling in some respects a fabric containing yarns spun from staple fibers. Other novelty effects can readily be obtained by minor variations of the spinneret and spinning conditions.
For certain of these effects, it is advantageous that the filaments vary repetitively along their lengths by more than + 25% (preferably more than ~ 30%~ in cross-sectional area. The effects are particularly pronounced when the yarn has a Uster unevenness of at least 2.5% U. The Uster measure-ment is made using the Uster*Evenness Tester, Model C, together with integrator ITG-101 for this instrument. The yarn speed is 182.8 meters per minute (200 ypm), the service selector is set on normal, and the sensitivity selector is set to 12.5%.
The /0 U is read from the integrator after a sample run time of 5 minutes.
Shrinkage is determined by the method disclosed in this paragraph. Generally speaking, a sample yarn's initial length Lo is determined while the yarn is under a tension of 0.1 grams per denier. The yarn is then subjected to a tension of 0.0025 grams per denier and placed in an oven at 120C. for five minutes. The yarn is then removed from the oven, again subjected to a tension of 0.1 grams per denier and its length L2 determined. Shrinkage percentage equals Lo~L2 X 100 Lo * Trademark
Claims (19)
1. A process for producing a variable denier filament, comprising:
a. generating two individual streams of molten polyester of fiber-forming molecular weight, said individual streams traveling at different velo-cities;
b. converging said individual streams side-by-side to form a combined stream;
c. quenching said combined stream to form a combined filament; and d. withdrawing said combined filament from said com-bined stream at a rate of speed in excess of 2500 meters per minute.
a. generating two individual streams of molten polyester of fiber-forming molecular weight, said individual streams traveling at different velo-cities;
b. converging said individual streams side-by-side to form a combined stream;
c. quenching said combined stream to form a combined filament; and d. withdrawing said combined filament from said com-bined stream at a rate of speed in excess of 2500 meters per minute.
2. The process of Claim 1 wherein the withdrawal speed of said combined filament is selected such that an individual filament quenched from one of said individual streams would have a shrinkage at least ten percentage points higher than that of an individual filament quenched from the other of said indi-vidual streams.
3. The process defined in Claim 2, wherein one of said individual streams has a velocity between 2.0 and 7 times as high as the velocity of the other of said individual streams.
4. The process defined in Claim 2, wherein one of said streams has a velocity between 3.5 and 5.5 times as high as the velocity of the other of said individual streams.
5. The process defined in Claim 3, wherein said one of said individual streams has a smaller cross-sectional area than said other of said individual streams.
6. The process defined in Claim 4, wherein said one of said individual streams has a smaller cross-sectional area than said other of said individual streams.
7. The process as defined in Claim 3, wherein said with-drawal is selected such that said combined filament has a shrinkage less than 30%.
8. The process defined in Claim 6, wherein said with-drawal speed is selected such that said combined filament has a shrinkage less than 10%.
9. In a process for producing a filament, the improvement comprising generating first and second streams of molten polyester polymer of fiber-forming molecular weight traveling at different speeds to converge at a point below a spinneret face, the speeds and momenta of said streams and the angle at which said streams converge being selected such that the first of said streams is slower and travels in substantially a straight line after the point at which said streams first touch and attach and the second of said streams is faster and forms sinuous loops back and forth between successive points of attach-ment with said first of said streams, converging said indivi-dual streams side-by-side to form a combined stream, quenching the combined streams to form a filament and withdrawing said filament, wherein said filament is withdrawn at a speed in excess of 2500 meters per minute.
10. A process for producing a self-crimping yarn com-prising a plurality of variable denier filaments, each of said variable denier filaments being produced by the steps comprising:
a. generating first and second streams of molten polymer of fiber forming molecular weight traveling at different speeds to converge at a point below a spinneret face, the speeds of said streams and the angle at which said streams converge being selected such that the first of said streams is slower and travels in substan-tially a straight line after the point at which said streams first touch and attach and the second of said streams is faster and forms sinuous loops back and forth between successive points of attachment with said first of said streams;
b. attenuating said first of said streams whereby said sinuous loops become straightened and said second of said streams is brought into continuous contact with said first of said streams thereby converging said individual streams into a com-bined stream; and c. quenching the resulting combined stream into a filament, and d. withdrawing said filament at a speed in excess of 2500 meters per minute.
a. generating first and second streams of molten polymer of fiber forming molecular weight traveling at different speeds to converge at a point below a spinneret face, the speeds of said streams and the angle at which said streams converge being selected such that the first of said streams is slower and travels in substan-tially a straight line after the point at which said streams first touch and attach and the second of said streams is faster and forms sinuous loops back and forth between successive points of attachment with said first of said streams;
b. attenuating said first of said streams whereby said sinuous loops become straightened and said second of said streams is brought into continuous contact with said first of said streams thereby converging said individual streams into a com-bined stream; and c. quenching the resulting combined stream into a filament, and d. withdrawing said filament at a speed in excess of 2500 meters per minute.
11. The process defined in Claim 10, wherein said first of said streams is larger in cross-section than the second of said streams.
12. A self-crimping yarn comprising a plurality of poly-ester continuous filaments, (a) said filaments having non-round cross-sectional areas which vary substantially regularly along the lengths of said filaments from regions of large cross-sectional area to regions of small cross-sectional area, said variation in cross-sectional area being more than ? 10% about a mean value, b. said regions of large and small cross-sectional area being out of phase from filament to filament to thereby form said self-crimping yarn, c. each of said polyester continuous filaments having been formed by a process comprising the steps;
i. generating two individual streams of molten poly-ester of fiber-forming molecular weight, said individual streams traveling at different veloci-ties;
ii. converging said individual streams side-by-side to form a combined stream;
iii. quenching said combined stream to form a combined filament; and iiii. withdrawing said combined filament from said combined stream at a rate of speed in excess of 2500 meters per minute.
i. generating two individual streams of molten poly-ester of fiber-forming molecular weight, said individual streams traveling at different veloci-ties;
ii. converging said individual streams side-by-side to form a combined stream;
iii. quenching said combined stream to form a combined filament; and iiii. withdrawing said combined filament from said combined stream at a rate of speed in excess of 2500 meters per minute.
13. The yarn defined in Claim 12, wherein said variation in cross-sectional area is at least ? 30% about said mean value.
14. The yarn defined in Claim 12 wherein each of said filaments has a shrinkage of less than 30%.
15. The yarn defined in Claim 14 wherein each of said filaments has a shrinkage of less than 10%.
16. A self-crimping yarn comprising a plurality of poly-ester continuous filaments, (a) said filaments having non-round cross-sectional areas which vary substantially regularly along the lengths of said filaments from regions of large cross-sectional area to regions of small cross-sectional area, said variation in cross-sectional area being more than ? 10% about a mean value, (b) said regions of large and small cross-sectional area being out of phase from filament to filament to thereby form said self-crimping yarn, (c) each of said filaments having been formed by a process comprising the steps, i. generating a pair of streams of molten polymer of fiber-forming molecular weight traveling at different speeds to converge below a spinneret face, the speeds of said streams and the angle at which said streams converge being selected such that the first of said streams is slower and travels in substantially a straight line after the point at which said streams first touch and attach and the second of said streams is faster and forms sinuous loops back and forth between successive points of attachment with said first of said streams, said first of said streams being larger in cross-section than the second of said streams;
ii. attenuating said first of said streams whereby said sinuous loops become straightened and said second of said streams is brought into continu-ous contact with said first of said streams thereby converging said individual streams into a combined stream;
iii. quenching the resulting combined stream into a filament, and iiii. withdrawing said filament at a speed in excess of 2500 meters per minute.
ii. attenuating said first of said streams whereby said sinuous loops become straightened and said second of said streams is brought into continu-ous contact with said first of said streams thereby converging said individual streams into a combined stream;
iii. quenching the resulting combined stream into a filament, and iiii. withdrawing said filament at a speed in excess of 2500 meters per minute.
17. The yarn defined in Claim 16, wherein said variation in cross-sectional area is at least ? 30% about said mean value.
18. The yarn defined in Claim 16 wherein each of said filaments has a shrinkage of less than 30%.
19. The yarn defined in Claim 18 wherein each of said filaments has a shrinkage of less than 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA376,665A CA1123562A (en) | 1977-08-17 | 1981-04-30 | Self crimping yarn and process |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US82549577A | 1977-08-17 | 1977-08-17 | |
| US825,495 | 1977-08-17 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1154215A true CA1154215A (en) | 1983-09-27 |
Family
ID=25244144
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000309498A Expired CA1154215A (en) | 1977-08-17 | 1978-08-16 | Self crimping yarn and process |
Country Status (7)
| Country | Link |
|---|---|
| JP (1) | JPS5442415A (en) |
| CA (1) | CA1154215A (en) |
| DE (2) | DE2835706A1 (en) |
| FR (3) | FR2421964A1 (en) |
| GB (1) | GB2003423B (en) |
| IT (1) | IT1098072B (en) |
| SE (1) | SE7902135L (en) |
Families Citing this family (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4489543A (en) * | 1977-08-17 | 1984-12-25 | Celanese Corporation | Self-crimping yarn |
| US4772347A (en) * | 1980-05-09 | 1988-09-20 | Minnesota Mining And Manufacturing Company | Process for making filamentary structure |
| EP0041820B1 (en) * | 1980-06-06 | 1984-07-04 | Celanese Corporation | Process for production of self-crimping polyester yarn |
| US4562029A (en) * | 1980-06-06 | 1985-12-31 | Celanese Corporation | Self-crimping polyester yarn |
| US4720314A (en) * | 1980-06-06 | 1988-01-19 | Celanese Corporation | Process for producing self-crimping polyester yarn |
| US4376743A (en) * | 1981-06-12 | 1983-03-15 | Fiber Industries, Inc. | Melt spinning process |
| EP0078869B2 (en) * | 1981-11-09 | 1988-09-28 | Minnesota Mining And Manufacturing Company | Filamentary structure |
| US4411852A (en) * | 1982-02-18 | 1983-10-25 | Fiber Industries, Inc. | Spinning process with a desensitized spinneret design |
| EP0088744A3 (en) * | 1982-03-08 | 1986-02-12 | Monsanto Company | Easily splittable conjugate filament |
| US4600644A (en) * | 1982-06-10 | 1986-07-15 | Monsanto Company | Polyester yarn, self-texturing in fabric form |
| JPS594557A (en) * | 1982-06-30 | 1984-01-11 | Kanzaki Paper Mfg Co Ltd | Paper tension adjusting method immediately before reel |
| JPS5915510A (en) * | 1982-07-20 | 1984-01-26 | Teijin Ltd | Production of latently crimped yarn |
| US4522773A (en) * | 1983-02-24 | 1985-06-11 | Celanese Corporation | Process for producing self-crimping polyester yarn |
| GB2136025B (en) * | 1983-03-01 | 1986-06-11 | Monsanto Co | Crimped polyester tow and staple |
| EP0122250A3 (en) * | 1983-04-11 | 1986-02-05 | Monsanto Company | Easily splittable self-texturing conjugate yarn |
| EP0122906A3 (en) * | 1983-04-11 | 1986-02-05 | Monsanto Company | Deep dyeing helically crimped conjugate yarn process |
| JPS6018333A (en) * | 1983-07-11 | 1985-01-30 | Nichiei Sangyo Kk | Manufacture of spiral body made of synthetic resin |
| US4619803A (en) * | 1984-07-23 | 1986-10-28 | Monsanto Company | Self-texturing nylon yarn spinning process |
| JPS61226466A (en) * | 1985-03-30 | 1986-10-08 | Mitsubishi Metal Corp | Wind up method for very fine yarn |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3387327A (en) * | 1966-06-09 | 1968-06-11 | Monsanto Co | Filament spinning apparatus |
| US3497585A (en) * | 1966-06-09 | 1970-02-24 | Monsanto Co | Self-crimping filament process |
| DE2263302A1 (en) * | 1971-12-29 | 1973-07-12 | Asahi Chemical Ind | POLYESTER FILAMENT YARN WITH MULTICOLOR EFFECT AND THE METHOD OF MANUFACTURING IT |
| JPS5199109A (en) * | 1975-02-25 | 1976-09-01 | Kuraray Co | ETSUKUSUJIKEIIKEIDANMENSENI OYOBI SONOSEIZOHO |
-
1978
- 1978-08-16 IT IT26786/78A patent/IT1098072B/en active
- 1978-08-16 DE DE19782835706 patent/DE2835706A1/en active Granted
- 1978-08-16 FR FR7823900A patent/FR2421964A1/en active Granted
- 1978-08-16 DE DE2858687A patent/DE2858687C2/de not_active Expired
- 1978-08-16 GB GB7833531A patent/GB2003423B/en not_active Expired
- 1978-08-16 CA CA000309498A patent/CA1154215A/en not_active Expired
- 1978-08-16 JP JP10045278A patent/JPS5442415A/en active Granted
-
1979
- 1979-03-09 SE SE7902135A patent/SE7902135L/en unknown
- 1979-05-02 FR FR7911058A patent/FR2423567A1/en active Granted
- 1979-05-02 FR FR7911057A patent/FR2422742A1/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| FR2422742B1 (en) | 1982-02-05 |
| FR2422742A1 (en) | 1979-11-09 |
| FR2423567A1 (en) | 1979-11-16 |
| FR2423567B1 (en) | 1982-02-05 |
| DE2858687C2 (en) | 1988-11-24 |
| IT1098072B (en) | 1985-08-31 |
| FR2421964A1 (en) | 1979-11-02 |
| SE7902135L (en) | 1980-09-09 |
| DE2835706C2 (en) | 1988-04-21 |
| GB2003423B (en) | 1982-07-14 |
| DE2835706A1 (en) | 1979-02-22 |
| IT7826786A0 (en) | 1978-08-16 |
| JPS6158566B2 (en) | 1986-12-12 |
| JPS5442415A (en) | 1979-04-04 |
| GB2003423A (en) | 1979-03-14 |
| FR2421964B1 (en) | 1982-02-05 |
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