CA2017836A1 - Cotton/polyester fiber blends and batts - Google Patents
Cotton/polyester fiber blends and battsInfo
- Publication number
- CA2017836A1 CA2017836A1 CA002017836A CA2017836A CA2017836A1 CA 2017836 A1 CA2017836 A1 CA 2017836A1 CA 002017836 A CA002017836 A CA 002017836A CA 2017836 A CA2017836 A CA 2017836A CA 2017836 A1 CA2017836 A1 CA 2017836A1
- Authority
- CA
- Canada
- Prior art keywords
- batt
- cotton
- fibers
- copolyester
- blend
- 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.)
- Abandoned
Links
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/04—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres
- D04H1/08—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres and hardened by felting; Felts or felted products
- D04H1/10—Felts made from mixtures of fibres
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Abstract
Cotton/Polyester fiber blends and batts Abstract of the Disclosure A blend, a batt, and a process for making the batt from the blend is disclosed. The blend and batt are made from a uniform combination of cotton and copolyester binder fibers wherein the binder fibers have a melting temperature of 230 to 340°F.
Description
~Sl:~'7~
-- 1 ~
Tltle Cotton/Polyester Piber blends and batt~
~ack~round of the Invention Field of the Invention Thi6 invention relats~ to blends of cotton and polyester copolymer binder fibers ~nd to batts made from such blends. The batt~ are made by ~ean~ of O thermal bonding proces6~ and they ~re durable enough to wlth~tand the stresseæ o repeatod washing6. The bl~nd~ aro o a high bulk and a low density.
Description of the Prior Art U.S. 4,685,914, i~6Ued AU9UBt 11, 1987 (Personal Pr~duct~) teache~ the manufacture of an ~bsorbent pad by heat fusing a combinat$on of absorbent fiber6 ~nd binder flb~r~. Ab60rbent ~iber~ can be wood pulp, rayon, cellulose acetate, fl~x, hemp, ~ute, ramie, cotton, ~nd the like. ~inder iber~ are polye6ter. One pad, u~ing a blend o~ polye~ter ~taple and polyeeter binder ~iber~ and a blend of acrylic fiber~ and polye~ter binder ~iber6, 16 about 20-25~ binder fiber6 and 1~ bonded at about 315F.
European Patent publication 227,~14 ~eem~ to teach consolidation of cotton 6wabbing by 6uper~1cially fu~ing thermoplastic $iber~ uniformly di6tributed throughout the cotton. The temper~tur~ for the fu~ing appear6 to be about 250F.
Japan~e Publications, J60029182A (Toray) ~nd J60040239A (Kanegafuchi), available in ab~tract form, teach manufacturin~ a blend of fibers; and fusing the blend by thermal means. The fibers can be selected from a li~t o~ relatively high melting materials including polyester, polypropylene, polyacrylic, cotton, wool, hemp, ~2~3~ ~
rayon, and the like; and a list of binder fiber~ including - copolyester, polyolefin, and the like.
U.S. 4,769,022, i6sued September 6, 1988 (3M) teaches the preparatlon o~ a pad made by he~ting a blend of 50/50, wt. cotton and polyester for 20 eecond~ at 285~F.
Polyerter Staple for Thermally Bonded Nonwovens, by W. ~. Kwok, et al., Nonwoven6 Indu6try, ~une, 1988, teache~ that particular polyester binder fiber products can be u~ed to make thermally bondable bl~nds of fibers.
Cotton is not mentioned a6 a cand$date fiber for the blendæ.
Summary o the Inv~nt~on The pre~ent invention provides a thermofusible blend of ~iber~ including a unifor~ mixture o~ 75 ~5 weight percent cotton and 15-25 weight percent ethylene terephthalate/i~ophthalate copolye~ter compri~ing 60-80 mole percent terephthalate and 20-40 mole percent i60phthalate ~nd having a melting point of about 230 to 340 F.
The invention includes a proces~ for fu~ing the aforementioned blend by ~ubjecting the blend to heat at a temperature of about 230 to 390 F for ~ duration of from 20 to lOQ seconds under no compre~ive pre6~ure. The~
invent~on, also, include~ ~ batt which re~ults from the aforementionsd proce~, ha~ a den~ity of 0.014 to 0.038 grams per cubic centi~eter, and i6 capable of with~tanding repe~ted washing ~tre~e~.
Detailed De~cription of the Invention Thi~ invention is directed toward the u~e of cotton fib~r~ in a blend of other fibers including copolye~ter binder fibers. De pite the fa~t that the blend contains cotton fibers which are not thermofu~ible, 3~ it al~o include~ thermo~usible binder fibers and can, therefore, be heated and melted to create bonds between adjacent fiber6. The invention represent~ a meanB or ~ 3~
utllizing cotton ~taple to make lmprc)ved batts of high quality, low den~ity, and excellent clurability.
Cotton 6taple can be obtained from any commercial source and it can be ~coured or not ~nd bleaehed or raw. For the purpo~e~ of this invention, cotton can also mean wood pulp and regenerated cellulo~e such ~ rayon.
The oopolye~ter preEerred for u~e in the practice of thi~ invention i~ a copolye~ter ~ade from a 1~ mole-for-mole condensation of ethylene glycol and a combination of terephthalic ~nd 160phthalic aeld6. For 6uch a copolye6ter h~ving ~ terephthal~te/~ophth~late mole ratio of 70/30, it ha~ ~ melting point o~ about 28BF
and a ~tick point of about 1~4DF. ~iber~ made from thi6 copolyester 6erve a~ thermal binder fiber~ and mu~t exhibit melting points below the temperature at which cotton i8 discolored and must, al60, exhib~t a melt adhe6ion to cotton ~t~ple.
Fibers used in this invention are u6ed in a blend form and the flber~ 1n the blend must be cho~en to interact appropriately at the time that the blend i6 tran6formed into a durable batt. One of the lmportant elements of interaction reæide~ in the relative ~ize OF
the cotton fibers and the binder fiber~. The cotton fiber~ 6hould have a denier of 1.0 tD 1.8 and preferably ~bout 1.6; and it has been found that length6 of rom 0.8 to 1.5 inche6 are preferred. The binder fiber6 ~hould have a denisr about the same a~ the cotton taple~ but, if they mu~t be ~omewhat different, they ~hould be Pro~ 0.75 to 2~7 time~ the denier of the cotton. The length of the binder fiber6 can range from 0.5 to 3 inche~; but it i~
preferred that the binder fibers be from 0.75 to 2.0 time~
the length of the cotton ~taple in any given blend.
The cotton fiber~ and the copolyester fiber~ can be combined by any commercial blending equipment. Of cour e, the combination of fiber~ can be accompli6hed by any other effective means provided, only, that the blend is a uniform mixture of the different fiber~.
It should be pointed out that the blend~ of thi~
invention are not limited to cotton ~nd copolyester fiberfi, alone. If it i6 desired or required for any reason, other fibers can be added to the blend and the other fibers can perform an ac:tive function or can merely be present as a filler material. The other ibees can be hollow or 601id and inorganic or organic, whethsr natural or 6ynthetic. Additive material6 other than fiber~ ~n, al80, be ~dded to the blend~ as fillers, colorants, 6cents, antimicrobial agents, bulking agents, flame retardant6, ~ntistats, ~nd the like. In the c~se of additive materials, it has been found that ~hey 6hould, 15 generally, be u6ed in an amount of from 0.1 to 20 weight percent, based on the total weight of the blend. In the case of additive ~iberz which perform an active function in the blends,~the amount of fiber~ ~hould b8 cho~en to accomplish the desired purpose.
Th~ blends of this invention include 15 to 25 weight percent copolye~ter binder fibers based on th~
total amount of fiber in the blend~0 It ha~ been determined that blend6 ~ade from le6s than 15 percent o copolye~ter binder fibers cannot be bonded for adequate durability at any condition6; ~nd that blends ~ade from more than 25 percent o ~opolyest~r binder fiber~ re~ult in bonded batt~ which exhibit poor wash durablllty.
Blend~ h~ving 15 to 25 percent copolyester binder fiber~
yield batt of very good a~d durable qualitie8. Afi has been disclosed in the art, binder material need only be present as a surface component of the binder iber, for example as a sheath component of a sheath/core blcomponent fiber. The remainder or core of the fiber may be of 35 higher melting point, ~nd thus would remain in fiber form as a bridging structure after the lower melting material has fu~ed and performed its binding ~unction. Such ~r~~ ?,~
bicomponent binder fibers have been di~closed, for example, ln U.S. Patents No. 3,5ag,956 and 4,0S8,036. It will be under~tood that, for best results when u~ing bieomponent fibers, ~ome corresponding adjustment of proportion6 may be advi6abl~ to optimize re6ult6 in rel~tion to those preferr~d when monocompon@nt binder fiber6 are blended with cotton.
Blends c8n be ~ade into batt~ of this ~nvention as a single layer of the bleild or it can ~e built up of 6ev~ral layers. Typically, l:he batt will be ormed from ~everal layers of a eard-formed or garnett-formed web of the blend, by cro6slapping ttl2 web on a movlng apron to the batt thickneæs de~lred such a8 dl~ClOBed i~l U.S.
Patent No. 3,29~,704. One~ formed, the batt iB ~ub~ected to heat at a temperature equal to or greater than the ~tick temperature of the binder fiber~ 6uch that the binder fiber6 will be 60ftened and will adhere to the~selve~ and to the cotton fiber6 in the batt. The heat can be provided by means of open ovens, through-air drum6 or ovens, infrared heaters, radiation heaters, and the liks. The heat should not exceed the temperature at which cotton beg~ns to discolor, that i&, about 390F, and pre erably 60mewhat 188æ. The temperature o the heat ~hould be ~s low as pos~ible; and, for that rea~on, it i~
important that a copolye6ter is u6ed ~ith a low melting point. In practical operation, bondins te~perature~ of 360 to 380~F are high. Duration of the heating ~hould be adeguate ~or the binder ~iber to 60ften and adhere --usually from 20 to 100 seconds or, perhaps, 61ightly longer. ~e~use it i6 the intention to make batt~ hav~ng as low a den~ity as possible, the he~ting is, generally, eonducted with no pre6sure on the batt~. However, the batts can be heated under &ome degree of compressive 6trength to a~hieve whatever batt density is desired for nny p~rtl~ular purpo6e.
~he batt~ of this lnventiorl are u~eful or fiberfill, in~ulation, padding, re~ilient cu6hioning, and the like. The batts are generally made to hav~ a den6$ty of 0.018 to 0.03a gram6 per cubic c~ntimeter. The~e batts exhibit excellent washability and have high 6trength as indicated by large values of adju~ted total work-to-break.
Washability is a measure of t:he dur~bility of batt~ of thi~ invention through autom~tic wash~ng and drying cycles. It ha~ been found that batts with too little blnder fiber di~integrate during laundering because of inadequate fiber-to-fiber ~dhe~ion and that b~tt6 with too much binder fiber are boardy and are broken apart during laundering becau~e o being t:oo ~tiff and brlttle. Batts of this invent~on exhiblt an ~ppearance a~ter l~under~ng which i~ ruperior to batt6 made using the ~me kinds of ~ateri~l~ under the ~ame ~ondition6 but with l~s6 than 15 or more than 25 weight percent copolye6ter binder fiber6.
Test methods used to determine the~e qualities are ~et out below.
Te~t Methods .
Denier - ~he denier of a filament i6 c~lculated fro~ it5 ~undamental resonant frequency~ determlned by vibrating a 2 to 4 cm length of filament under tenaion with changing frequ~ncy. ~ASTM Dl577-66), part 25, 196~)~
Density ~ Th~ density of a batt ~ determined by weighing a batt of known volume.
Stick Temperature - Fiber ~tick temperature i~
mea~ured a~ described by Beaman and Cramer, J. Polymer Science 21, page 228 ~1956). A flat bra66 block i~ heated electrically to rai~e the block temperature at a hlow rate. The ~iber sample i~ su~pended under slight ten~ion between gl~ss rods over and near the ~urface of the block.
3~ At ~ntervals, the fiber is pressed against the block for 5 ~econds with a 200 gram bras~ weight which has been in continuous contact with the heated blockO The fiber stick Z~3~.7~33~
temperature is the temperature of th~s block when the f iber 6ticks to it for at least 2 seconds after removing the weight.
Work-to-Break The strength of the batt6 of this invention i6 measured by determ:ining the Adju6ted Tot~l Work to ~reak. The Ad~u6ted Total Work to Break i~
determined in accordance with ASTM D885 - 85 as follow~:
Sample~ of the batt to be te6ted are cut 1 inch wide and 7 inches long. Ten of those ~ample~ are cut with the length in the machine direction ~nd ten ~re cut with the length in the tran~ver~e direction. The ~ample6 are condit~oned for 2 hour~ at about 75F ~nd 55% relative hum~dity.
Each of the ~amples i8 mounted in the jaws of a ten~ile testing machine with a 5 inch gage length; and the samples are pulled with the re~ult~ recorded on a ~tre~s-~train curve gen~rated by the testlng machine.
The Work-to-~reak is ~alculated using the equation -Work-to-Break, in.-lb~. ~ A x F x E
wherein A ~ area under the lo~d-elongation curve, in.2, F ~ load æcale factor, in., of chart, and E - elongation ~eale actor, in., o~ &pecimen elongation per inch o~ chart.
Work to-Break i6 the average value of ten 6ample~. Work-to-~reak i~ determined for the mach~ne direction and for the transver6e direction. Total Work-to-Break i~ the su~ o~ the machin~ direction ~ork-to-Break and the transverse direction Work-to-Break.
To calculate the Adjusted Total Work-to-Break, the Total Work-to-Break is divided by the basi~ weight of the batt in ounces per yard2. ~or purpo~es of thi~
invention, acceptable batts exhibit an ~djusted Total Work-to-~reak of gre~ter than 2 inch-pound~ per oz/yd2.
~ppearance after Launderin~ - A quality of major - 8 -~ 7~
importance for the batts of thi~ invention i6 the durability of the batt6 to laundering ~tres~es. The te~t for such durability i~ the AATCC Te~t Method 135-19B7 (AATCC stand for American A~ociation of Textil~ Ch~mi~t~
and Colori~ts). In the conduct of thi6 te~t, 3 test batts 8 x B inches are u~ed for each batt to b~ tested. The laundering i~ conducted in automatic washing ~nd dr~ing machine~ in accordance with the ~ATCC procedure wherein the normal or cotton ~etting6; are u~d for the wa~h~r, cotton ~ettings are uGed for the dryer, ~nd a 4.0 pound load i& u6ed. To compl~te the test, a totzl of five cycle6 of wa hing and drying are u6ed.
The 6amples are juclged by their ~ppear~nce on a scale of 1 to 4, with 1 being worst -- having fibers lumping together and exhibiting nonunlformity -- and 4 being b~st -- havin~ excellent appearance with un~formity similar to the unwa~hed original 6ample. A b~tt appear~nce of 2.5 is considered acceptable for purp~es of this invention.
De6cription of the Preferred ~mbodiments Example 1. Preparation of the ~l~nd~ - In th1~
example, blend~ of fiber6 were made in accordance with the present inv~ntion.
Cotton staple wa~ u~ed ~hlch was ~coured and bleached and which had a denier of about 1.6 and an average length of about 1.1 inch (~ range of ~.8 to 1.5 inche~).
Copolyester binder iber6 were used which had ethylene and a 70/30 mole ratio of terephthalate and isophthalate groups, a ~tick point of 194F, and a melting point of 288F. The binder fibers had a denier of about 3 and an aver~e length of about l.S inches.
Cotton fiber~ and copolye~ter fibers were combined and blended in a commerci~l opener-blender 6uch that the blend was uniform and such that there were varying.concentrations of binder fibers in each of 6everal - B -g Z~ 7~J~
run 6 .
The 6everal run~ are identified in the Table6 which follow the Example~.
~ xample 2. Prep~ration of the ~att6 - In thl~
example, blend~ from Example 1 were thermally bonded to yield batt6 of the pre6ent invention.
Blend6 from Example 1 were carded on a 40 inch roller top carding machine to yield a ~ontinuous web which was ~ro~slapped to a continuou6 batt having a ba~is weight of 3 to 8 ounce6 per 6quare yiard.
The batt~ were pl~cled on ~ conveyer and pa66ed through a through-air oven of 2 meter~ l~ngth at variou~
6peeds and variou~ temperatur~es. The temperatures and rate~ for the thermal bonding were 230 to 420~F and 1.3 to 5 meters/minute.
The batt~ were te6ted ~or the ~dju~ted Total Work-to-Break and the Batt Appearance. ~esults o the te~ts ~re 6et out in Table I below.
_ g _ '7~}~$
TAsLE I
BOND BASIS
Run BOND RAT~ WT. ADJWSTED TOTAL WOR~ BATTING
No. TEMP(F)(m~min)(oz/yd~ cross ~ mach. - total APP~AR
Binder 10~
1 300 1.29 4.5 0.624 ~.710 1.334 2 310 1.~9 4.2 1.016 0.875 1.892 3 320 1.29 4.2' 1.062 0.gl4 1.977 2.3 4 330 1.29 ~.~. 1.211 ~.15~ 2.3~9 340 1.29 4.~. 1.371 1.163 2.S34 ~ 350 1.29 4.3 1.057 1.0~3 ~.139 2.2 7 360 1.29 3.~ 1.227 ~.~27 2.653 R 370 1.29 ~.0 1.459 1.760 3.218 9 370 ~.~6 4.1 1.171 1.070 2.24~
370 ~.00 5.~ 0.5~ 0.515 l.Q20 1~ 380 1.29 4.~ 09 1.553 3.061 2.3 12 390 1.29 4.1 1.988 1.38B 3.376 13 400^ 1.294.0 1.470 1.639 3.~10 14 410^ 1.2g4.~ 1.494 1.~24 3.317 2.3 420' 1.294.6 1.730 1.~53 3.583 16 420~ 2.264.~ 1.5~ 1.567 3.156 ~.~
17 420' 3.104.0 1.743 l.g46 3.68B 2.5 18 420^ 5.004.6 0. aos o . ~os 1 . 618 2.7 Blnder 20~
19 2~0 1.29 3.9 1O2qg 1.454 2.703 2n 2g0 1.29 ~.0 1.0~5 0.~63 2.04~ 2.
21 300 1.29 4.8 1.~35 1.160 2.~95 22 310 1.29 4.4 1.611 1.507 3.11~
23 320 1.2g 5.2 1.281 1.27B 2.559 3.5 24 330 1.29 5.0 1.7~5 ~.~31 3.176 3~0 1.29 4.7 1.736 1.890 3.6~6 26 350 1.2g 4.5 1.8~3 2.30~ 4.197 2.
27 360 1.29 4.0 2.3~ 2.266 4.~19 ~8 370 1.29 4,7 2. aD6 2.471 4.67B
29 380 1.29 ~.~ 2.408 2.3~3 4.7~1 3.5 390 1.29 ~.2 2.~ 2.466 5,273 31 400- 1.13 ~ .353 2.146 4.~99 32 410~ 1.29~.1 3.281 2.935 ~.216 3.5 33 ~0^ 1.29 4.5 3.0~3 3.19~ 6.25S
34 420~ 2.264.9 2.372 2.485 4.B57 3.0 420- 3.1~ S.2 2.~32 1.9~4 3.9g6 2.8 36 420^ 5.004.4 1.709 l.~lq 3.30~ 3.2 ~A~LE I ( cont ' d ) BOND ~AS I S
Run ~OND ~ATE WT. ADJUSTED TOTAL WOR~ ~ATTING
No. TEMP(F)~m/mln)(oz/yd2 ) cross ~ mach. ~ total APPEA~
Binder 30~
37 230 1.29 7.6 0.892 0.772 1.665 1.3 38 ~37 1.29 5.1 0.992 0.9~5 1.~3~
39 240 1.29 4.6 1.037 1.085 2.122 240 1.~9 7.3 1.145 1.015 2.1~1 ~1 250 1.29 4.3 1.04~ l.OOS 2.~49 42 260 1.29 4.2 0.769 1.277 2.047 3.2 43 270 1.~9 4.3 1.219 1.294 2.51 44 280 1.29 3.8 1.646 1.~0~ 3.2~
~5 290 1.29 3.9 1.333 1.517 2.~49 2.0 46 300 1.29 5.5 1.40B 1.481 ~.859 47 310 1.29 5.3 1.~36 1.461 3.097 48 320 1.29 5.5 1.372 0.~49 2.221 2.3 49 330 1.29 5.6 1.4B1 0.886 2.368 340 1.29 5.5 1.706 1.154 2.860 51 350 1.29 5.3 2.031 1.601 3.632 2.3 5~ 360 1.29 5.1 1.963 1.5~4 3.527 53 370 1.29 5.4 2.650 2.392 4.742 54 380 1.29 5.2 ~.294 2.410 4.70~ 3 390 1.29 4.7 3.215 2.810 6.025 56 400' 1.29 4.9 2.910 2.B88 5.797 57 410~ 1.29 4.9 6.620 5.012 11.632 58 420- 1.29 5.2 2.879 2.957 5.~36 2.~
59 420~ ~.26 ~.4 2.29~ 1.65~ 3.954 3.2 420~ 5.00 5.2 1.616 1.477 3.093 2.8 ~Indicate~ that the temperature i~ too high--the cotton discolors durinq processing.
-- 1 ~
Tltle Cotton/Polyester Piber blends and batt~
~ack~round of the Invention Field of the Invention Thi6 invention relats~ to blends of cotton and polyester copolymer binder fibers ~nd to batts made from such blends. The batt~ are made by ~ean~ of O thermal bonding proces6~ and they ~re durable enough to wlth~tand the stresseæ o repeatod washing6. The bl~nd~ aro o a high bulk and a low density.
Description of the Prior Art U.S. 4,685,914, i~6Ued AU9UBt 11, 1987 (Personal Pr~duct~) teache~ the manufacture of an ~bsorbent pad by heat fusing a combinat$on of absorbent fiber6 ~nd binder flb~r~. Ab60rbent ~iber~ can be wood pulp, rayon, cellulose acetate, fl~x, hemp, ~ute, ramie, cotton, ~nd the like. ~inder iber~ are polye6ter. One pad, u~ing a blend o~ polye~ter ~taple and polyeeter binder ~iber~ and a blend of acrylic fiber~ and polye~ter binder ~iber6, 16 about 20-25~ binder fiber6 and 1~ bonded at about 315F.
European Patent publication 227,~14 ~eem~ to teach consolidation of cotton 6wabbing by 6uper~1cially fu~ing thermoplastic $iber~ uniformly di6tributed throughout the cotton. The temper~tur~ for the fu~ing appear6 to be about 250F.
Japan~e Publications, J60029182A (Toray) ~nd J60040239A (Kanegafuchi), available in ab~tract form, teach manufacturin~ a blend of fibers; and fusing the blend by thermal means. The fibers can be selected from a li~t o~ relatively high melting materials including polyester, polypropylene, polyacrylic, cotton, wool, hemp, ~2~3~ ~
rayon, and the like; and a list of binder fiber~ including - copolyester, polyolefin, and the like.
U.S. 4,769,022, i6sued September 6, 1988 (3M) teaches the preparatlon o~ a pad made by he~ting a blend of 50/50, wt. cotton and polyester for 20 eecond~ at 285~F.
Polyerter Staple for Thermally Bonded Nonwovens, by W. ~. Kwok, et al., Nonwoven6 Indu6try, ~une, 1988, teache~ that particular polyester binder fiber products can be u~ed to make thermally bondable bl~nds of fibers.
Cotton is not mentioned a6 a cand$date fiber for the blendæ.
Summary o the Inv~nt~on The pre~ent invention provides a thermofusible blend of ~iber~ including a unifor~ mixture o~ 75 ~5 weight percent cotton and 15-25 weight percent ethylene terephthalate/i~ophthalate copolye~ter compri~ing 60-80 mole percent terephthalate and 20-40 mole percent i60phthalate ~nd having a melting point of about 230 to 340 F.
The invention includes a proces~ for fu~ing the aforementioned blend by ~ubjecting the blend to heat at a temperature of about 230 to 390 F for ~ duration of from 20 to lOQ seconds under no compre~ive pre6~ure. The~
invent~on, also, include~ ~ batt which re~ults from the aforementionsd proce~, ha~ a den~ity of 0.014 to 0.038 grams per cubic centi~eter, and i6 capable of with~tanding repe~ted washing ~tre~e~.
Detailed De~cription of the Invention Thi~ invention is directed toward the u~e of cotton fib~r~ in a blend of other fibers including copolye~ter binder fibers. De pite the fa~t that the blend contains cotton fibers which are not thermofu~ible, 3~ it al~o include~ thermo~usible binder fibers and can, therefore, be heated and melted to create bonds between adjacent fiber6. The invention represent~ a meanB or ~ 3~
utllizing cotton ~taple to make lmprc)ved batts of high quality, low den~ity, and excellent clurability.
Cotton 6taple can be obtained from any commercial source and it can be ~coured or not ~nd bleaehed or raw. For the purpo~e~ of this invention, cotton can also mean wood pulp and regenerated cellulo~e such ~ rayon.
The oopolye~ter preEerred for u~e in the practice of thi~ invention i~ a copolye~ter ~ade from a 1~ mole-for-mole condensation of ethylene glycol and a combination of terephthalic ~nd 160phthalic aeld6. For 6uch a copolye6ter h~ving ~ terephthal~te/~ophth~late mole ratio of 70/30, it ha~ ~ melting point o~ about 28BF
and a ~tick point of about 1~4DF. ~iber~ made from thi6 copolyester 6erve a~ thermal binder fiber~ and mu~t exhibit melting points below the temperature at which cotton i8 discolored and must, al60, exhib~t a melt adhe6ion to cotton ~t~ple.
Fibers used in this invention are u6ed in a blend form and the flber~ 1n the blend must be cho~en to interact appropriately at the time that the blend i6 tran6formed into a durable batt. One of the lmportant elements of interaction reæide~ in the relative ~ize OF
the cotton fibers and the binder fiber~. The cotton fiber~ 6hould have a denier of 1.0 tD 1.8 and preferably ~bout 1.6; and it has been found that length6 of rom 0.8 to 1.5 inche6 are preferred. The binder fiber6 ~hould have a denisr about the same a~ the cotton taple~ but, if they mu~t be ~omewhat different, they ~hould be Pro~ 0.75 to 2~7 time~ the denier of the cotton. The length of the binder fiber6 can range from 0.5 to 3 inche~; but it i~
preferred that the binder fibers be from 0.75 to 2.0 time~
the length of the cotton ~taple in any given blend.
The cotton fiber~ and the copolyester fiber~ can be combined by any commercial blending equipment. Of cour e, the combination of fiber~ can be accompli6hed by any other effective means provided, only, that the blend is a uniform mixture of the different fiber~.
It should be pointed out that the blend~ of thi~
invention are not limited to cotton ~nd copolyester fiberfi, alone. If it i6 desired or required for any reason, other fibers can be added to the blend and the other fibers can perform an ac:tive function or can merely be present as a filler material. The other ibees can be hollow or 601id and inorganic or organic, whethsr natural or 6ynthetic. Additive material6 other than fiber~ ~n, al80, be ~dded to the blend~ as fillers, colorants, 6cents, antimicrobial agents, bulking agents, flame retardant6, ~ntistats, ~nd the like. In the c~se of additive materials, it has been found that ~hey 6hould, 15 generally, be u6ed in an amount of from 0.1 to 20 weight percent, based on the total weight of the blend. In the case of additive ~iberz which perform an active function in the blends,~the amount of fiber~ ~hould b8 cho~en to accomplish the desired purpose.
Th~ blends of this invention include 15 to 25 weight percent copolye~ter binder fibers based on th~
total amount of fiber in the blend~0 It ha~ been determined that blend6 ~ade from le6s than 15 percent o copolye~ter binder fibers cannot be bonded for adequate durability at any condition6; ~nd that blends ~ade from more than 25 percent o ~opolyest~r binder fiber~ re~ult in bonded batt~ which exhibit poor wash durablllty.
Blend~ h~ving 15 to 25 percent copolyester binder fiber~
yield batt of very good a~d durable qualitie8. Afi has been disclosed in the art, binder material need only be present as a surface component of the binder iber, for example as a sheath component of a sheath/core blcomponent fiber. The remainder or core of the fiber may be of 35 higher melting point, ~nd thus would remain in fiber form as a bridging structure after the lower melting material has fu~ed and performed its binding ~unction. Such ~r~~ ?,~
bicomponent binder fibers have been di~closed, for example, ln U.S. Patents No. 3,5ag,956 and 4,0S8,036. It will be under~tood that, for best results when u~ing bieomponent fibers, ~ome corresponding adjustment of proportion6 may be advi6abl~ to optimize re6ult6 in rel~tion to those preferr~d when monocompon@nt binder fiber6 are blended with cotton.
Blends c8n be ~ade into batt~ of this ~nvention as a single layer of the bleild or it can ~e built up of 6ev~ral layers. Typically, l:he batt will be ormed from ~everal layers of a eard-formed or garnett-formed web of the blend, by cro6slapping ttl2 web on a movlng apron to the batt thickneæs de~lred such a8 dl~ClOBed i~l U.S.
Patent No. 3,29~,704. One~ formed, the batt iB ~ub~ected to heat at a temperature equal to or greater than the ~tick temperature of the binder fiber~ 6uch that the binder fiber6 will be 60ftened and will adhere to the~selve~ and to the cotton fiber6 in the batt. The heat can be provided by means of open ovens, through-air drum6 or ovens, infrared heaters, radiation heaters, and the liks. The heat should not exceed the temperature at which cotton beg~ns to discolor, that i&, about 390F, and pre erably 60mewhat 188æ. The temperature o the heat ~hould be ~s low as pos~ible; and, for that rea~on, it i~
important that a copolye6ter is u6ed ~ith a low melting point. In practical operation, bondins te~perature~ of 360 to 380~F are high. Duration of the heating ~hould be adeguate ~or the binder ~iber to 60ften and adhere --usually from 20 to 100 seconds or, perhaps, 61ightly longer. ~e~use it i6 the intention to make batt~ hav~ng as low a den~ity as possible, the he~ting is, generally, eonducted with no pre6sure on the batt~. However, the batts can be heated under &ome degree of compressive 6trength to a~hieve whatever batt density is desired for nny p~rtl~ular purpo6e.
~he batt~ of this lnventiorl are u~eful or fiberfill, in~ulation, padding, re~ilient cu6hioning, and the like. The batts are generally made to hav~ a den6$ty of 0.018 to 0.03a gram6 per cubic c~ntimeter. The~e batts exhibit excellent washability and have high 6trength as indicated by large values of adju~ted total work-to-break.
Washability is a measure of t:he dur~bility of batt~ of thi~ invention through autom~tic wash~ng and drying cycles. It ha~ been found that batts with too little blnder fiber di~integrate during laundering because of inadequate fiber-to-fiber ~dhe~ion and that b~tt6 with too much binder fiber are boardy and are broken apart during laundering becau~e o being t:oo ~tiff and brlttle. Batts of this invent~on exhiblt an ~ppearance a~ter l~under~ng which i~ ruperior to batt6 made using the ~me kinds of ~ateri~l~ under the ~ame ~ondition6 but with l~s6 than 15 or more than 25 weight percent copolye6ter binder fiber6.
Test methods used to determine the~e qualities are ~et out below.
Te~t Methods .
Denier - ~he denier of a filament i6 c~lculated fro~ it5 ~undamental resonant frequency~ determlned by vibrating a 2 to 4 cm length of filament under tenaion with changing frequ~ncy. ~ASTM Dl577-66), part 25, 196~)~
Density ~ Th~ density of a batt ~ determined by weighing a batt of known volume.
Stick Temperature - Fiber ~tick temperature i~
mea~ured a~ described by Beaman and Cramer, J. Polymer Science 21, page 228 ~1956). A flat bra66 block i~ heated electrically to rai~e the block temperature at a hlow rate. The ~iber sample i~ su~pended under slight ten~ion between gl~ss rods over and near the ~urface of the block.
3~ At ~ntervals, the fiber is pressed against the block for 5 ~econds with a 200 gram bras~ weight which has been in continuous contact with the heated blockO The fiber stick Z~3~.7~33~
temperature is the temperature of th~s block when the f iber 6ticks to it for at least 2 seconds after removing the weight.
Work-to-Break The strength of the batt6 of this invention i6 measured by determ:ining the Adju6ted Tot~l Work to ~reak. The Ad~u6ted Total Work to Break i~
determined in accordance with ASTM D885 - 85 as follow~:
Sample~ of the batt to be te6ted are cut 1 inch wide and 7 inches long. Ten of those ~ample~ are cut with the length in the machine direction ~nd ten ~re cut with the length in the tran~ver~e direction. The ~ample6 are condit~oned for 2 hour~ at about 75F ~nd 55% relative hum~dity.
Each of the ~amples i8 mounted in the jaws of a ten~ile testing machine with a 5 inch gage length; and the samples are pulled with the re~ult~ recorded on a ~tre~s-~train curve gen~rated by the testlng machine.
The Work-to-~reak is ~alculated using the equation -Work-to-Break, in.-lb~. ~ A x F x E
wherein A ~ area under the lo~d-elongation curve, in.2, F ~ load æcale factor, in., of chart, and E - elongation ~eale actor, in., o~ &pecimen elongation per inch o~ chart.
Work to-Break i6 the average value of ten 6ample~. Work-to-~reak i~ determined for the mach~ne direction and for the transver6e direction. Total Work-to-Break i~ the su~ o~ the machin~ direction ~ork-to-Break and the transverse direction Work-to-Break.
To calculate the Adjusted Total Work-to-Break, the Total Work-to-Break is divided by the basi~ weight of the batt in ounces per yard2. ~or purpo~es of thi~
invention, acceptable batts exhibit an ~djusted Total Work-to-~reak of gre~ter than 2 inch-pound~ per oz/yd2.
~ppearance after Launderin~ - A quality of major - 8 -~ 7~
importance for the batts of thi~ invention i6 the durability of the batt6 to laundering ~tres~es. The te~t for such durability i~ the AATCC Te~t Method 135-19B7 (AATCC stand for American A~ociation of Textil~ Ch~mi~t~
and Colori~ts). In the conduct of thi6 te~t, 3 test batts 8 x B inches are u~ed for each batt to b~ tested. The laundering i~ conducted in automatic washing ~nd dr~ing machine~ in accordance with the ~ATCC procedure wherein the normal or cotton ~etting6; are u~d for the wa~h~r, cotton ~ettings are uGed for the dryer, ~nd a 4.0 pound load i& u6ed. To compl~te the test, a totzl of five cycle6 of wa hing and drying are u6ed.
The 6amples are juclged by their ~ppear~nce on a scale of 1 to 4, with 1 being worst -- having fibers lumping together and exhibiting nonunlformity -- and 4 being b~st -- havin~ excellent appearance with un~formity similar to the unwa~hed original 6ample. A b~tt appear~nce of 2.5 is considered acceptable for purp~es of this invention.
De6cription of the Preferred ~mbodiments Example 1. Preparation of the ~l~nd~ - In th1~
example, blend~ of fiber6 were made in accordance with the present inv~ntion.
Cotton staple wa~ u~ed ~hlch was ~coured and bleached and which had a denier of about 1.6 and an average length of about 1.1 inch (~ range of ~.8 to 1.5 inche~).
Copolyester binder iber6 were used which had ethylene and a 70/30 mole ratio of terephthalate and isophthalate groups, a ~tick point of 194F, and a melting point of 288F. The binder fibers had a denier of about 3 and an aver~e length of about l.S inches.
Cotton fiber~ and copolye~ter fibers were combined and blended in a commerci~l opener-blender 6uch that the blend was uniform and such that there were varying.concentrations of binder fibers in each of 6everal - B -g Z~ 7~J~
run 6 .
The 6everal run~ are identified in the Table6 which follow the Example~.
~ xample 2. Prep~ration of the ~att6 - In thl~
example, blend~ from Example 1 were thermally bonded to yield batt6 of the pre6ent invention.
Blend6 from Example 1 were carded on a 40 inch roller top carding machine to yield a ~ontinuous web which was ~ro~slapped to a continuou6 batt having a ba~is weight of 3 to 8 ounce6 per 6quare yiard.
The batt~ were pl~cled on ~ conveyer and pa66ed through a through-air oven of 2 meter~ l~ngth at variou~
6peeds and variou~ temperatur~es. The temperatures and rate~ for the thermal bonding were 230 to 420~F and 1.3 to 5 meters/minute.
The batt~ were te6ted ~or the ~dju~ted Total Work-to-Break and the Batt Appearance. ~esults o the te~ts ~re 6et out in Table I below.
_ g _ '7~}~$
TAsLE I
BOND BASIS
Run BOND RAT~ WT. ADJWSTED TOTAL WOR~ BATTING
No. TEMP(F)(m~min)(oz/yd~ cross ~ mach. - total APP~AR
Binder 10~
1 300 1.29 4.5 0.624 ~.710 1.334 2 310 1.~9 4.2 1.016 0.875 1.892 3 320 1.29 4.2' 1.062 0.gl4 1.977 2.3 4 330 1.29 ~.~. 1.211 ~.15~ 2.3~9 340 1.29 4.~. 1.371 1.163 2.S34 ~ 350 1.29 4.3 1.057 1.0~3 ~.139 2.2 7 360 1.29 3.~ 1.227 ~.~27 2.653 R 370 1.29 ~.0 1.459 1.760 3.218 9 370 ~.~6 4.1 1.171 1.070 2.24~
370 ~.00 5.~ 0.5~ 0.515 l.Q20 1~ 380 1.29 4.~ 09 1.553 3.061 2.3 12 390 1.29 4.1 1.988 1.38B 3.376 13 400^ 1.294.0 1.470 1.639 3.~10 14 410^ 1.2g4.~ 1.494 1.~24 3.317 2.3 420' 1.294.6 1.730 1.~53 3.583 16 420~ 2.264.~ 1.5~ 1.567 3.156 ~.~
17 420' 3.104.0 1.743 l.g46 3.68B 2.5 18 420^ 5.004.6 0. aos o . ~os 1 . 618 2.7 Blnder 20~
19 2~0 1.29 3.9 1O2qg 1.454 2.703 2n 2g0 1.29 ~.0 1.0~5 0.~63 2.04~ 2.
21 300 1.29 4.8 1.~35 1.160 2.~95 22 310 1.29 4.4 1.611 1.507 3.11~
23 320 1.2g 5.2 1.281 1.27B 2.559 3.5 24 330 1.29 5.0 1.7~5 ~.~31 3.176 3~0 1.29 4.7 1.736 1.890 3.6~6 26 350 1.2g 4.5 1.8~3 2.30~ 4.197 2.
27 360 1.29 4.0 2.3~ 2.266 4.~19 ~8 370 1.29 4,7 2. aD6 2.471 4.67B
29 380 1.29 ~.~ 2.408 2.3~3 4.7~1 3.5 390 1.29 ~.2 2.~ 2.466 5,273 31 400- 1.13 ~ .353 2.146 4.~99 32 410~ 1.29~.1 3.281 2.935 ~.216 3.5 33 ~0^ 1.29 4.5 3.0~3 3.19~ 6.25S
34 420~ 2.264.9 2.372 2.485 4.B57 3.0 420- 3.1~ S.2 2.~32 1.9~4 3.9g6 2.8 36 420^ 5.004.4 1.709 l.~lq 3.30~ 3.2 ~A~LE I ( cont ' d ) BOND ~AS I S
Run ~OND ~ATE WT. ADJUSTED TOTAL WOR~ ~ATTING
No. TEMP(F)~m/mln)(oz/yd2 ) cross ~ mach. ~ total APPEA~
Binder 30~
37 230 1.29 7.6 0.892 0.772 1.665 1.3 38 ~37 1.29 5.1 0.992 0.9~5 1.~3~
39 240 1.29 4.6 1.037 1.085 2.122 240 1.~9 7.3 1.145 1.015 2.1~1 ~1 250 1.29 4.3 1.04~ l.OOS 2.~49 42 260 1.29 4.2 0.769 1.277 2.047 3.2 43 270 1.~9 4.3 1.219 1.294 2.51 44 280 1.29 3.8 1.646 1.~0~ 3.2~
~5 290 1.29 3.9 1.333 1.517 2.~49 2.0 46 300 1.29 5.5 1.40B 1.481 ~.859 47 310 1.29 5.3 1.~36 1.461 3.097 48 320 1.29 5.5 1.372 0.~49 2.221 2.3 49 330 1.29 5.6 1.4B1 0.886 2.368 340 1.29 5.5 1.706 1.154 2.860 51 350 1.29 5.3 2.031 1.601 3.632 2.3 5~ 360 1.29 5.1 1.963 1.5~4 3.527 53 370 1.29 5.4 2.650 2.392 4.742 54 380 1.29 5.2 ~.294 2.410 4.70~ 3 390 1.29 4.7 3.215 2.810 6.025 56 400' 1.29 4.9 2.910 2.B88 5.797 57 410~ 1.29 4.9 6.620 5.012 11.632 58 420- 1.29 5.2 2.879 2.957 5.~36 2.~
59 420~ ~.26 ~.4 2.29~ 1.65~ 3.954 3.2 420~ 5.00 5.2 1.616 1.477 3.093 2.8 ~Indicate~ that the temperature i~ too high--the cotton discolors durinq processing.
Claims (10)
1. A thermofusible blend of fibers including a uniform mixture of from 75 to 85 weight percent cotton and 15 to 25 weight percent copolyester binder fibers having a melting point of from 230 to 340°F.
2. The blend of Claim 1 wherein the cotton fibers are from 1 to 1.6 denier and 0.8 to 1.5 inches in length and the binder fibers are 0.75 to 2.7 times the denier of the cotton and 0.75 to 2.0 times the length of the cotton and are of an ethylene terephthalate/isophthalate copolyester with a mole ratio of terephthalate to isophthalate from 80/20 to 60/40.
3. The blend of Claim 2 wherein the copolyester has a mole ratio of terephthalate to isophthalate of 70/30.
4. A process for making a durable batt from a blend of fibers wherein a uniform mixture of from 75 to 85 weight percent cotton and 15 to 25 weight percent copolyester binder fibers having a melting point of from 230 to 340°F comprising the steps of forming the blend into a batt and heating the batt at a temperature of 230 to 390°F for 20 to 100 seconds to effect softening of the binder fibers and bonding of the fibers at points of intersection.
5. The process of Claim 4 wherein the binder fiber in an ethylene terephthalate/isophthalate copolyester with a mole ratio of terephthalate to isophthalate from 80/20 to 60/40.
6. The process of Claim 5 wherein the copolyester has a mole ratio of terephthalate to isophthalate of 70/30.
7. A batt of a uniform mixture of from 75 to 85 weight percent cotton and 15 to 25 weight percent copolyester binder fibers having a melting point of from 230 to 340°F wherein the binder fibers are bonded randomly at points of intersection with other fibers in the batt and wherein the adjusted total work-to-break is greater than 2.0 pound-inches per oz/yd2 and the density is less than 0.038 grams per cubic centimeter.
8. The batt of Claim 7 wherein the binder fiber is an ethylene terephthalate/isophthalate copolyester with a mole ratio of terephthalate to isophthalate of 80/20 to 60/40.
9. The batt of Claim 8 wherein the copolyester has a mole ration of terephthalate to isophthalate of 70/30.
10. The batt of Claim 7 wherein the batt exhibits an appearance after laundering which is superior to batts made using the same kinds of materials under the same conditions but with less than 15 or more than 25 weight percent copolyester binder fibers.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US36141889A | 1989-06-05 | 1989-06-05 | |
| US361,418 | 1989-06-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2017836A1 true CA2017836A1 (en) | 1990-12-05 |
Family
ID=23421968
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002017836A Abandoned CA2017836A1 (en) | 1989-06-05 | 1990-05-30 | Cotton/polyester fiber blends and batts |
Country Status (8)
| Country | Link |
|---|---|
| EP (1) | EP0401738A3 (en) |
| JP (1) | JPH0369649A (en) |
| KR (1) | KR910001129A (en) |
| CN (1) | CN1083026C (en) |
| AR (1) | AR243246A1 (en) |
| AU (1) | AU639866B2 (en) |
| BR (1) | BR9002640A (en) |
| CA (1) | CA2017836A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2048938A1 (en) * | 1991-07-10 | 1993-01-11 | Paul M. Muncrief | Method for making insulation by sequentially utilizing apparatus for opening fibers |
| JP2842100B2 (en) * | 1992-11-04 | 1998-12-24 | トヨタ自動車株式会社 | Manufacturing method of cushioning material |
| CN1081249C (en) * | 1997-10-05 | 2002-03-20 | 泰安市第一山毛纺织有限公司 | Treating method for ironed fabrics |
| JP7220020B2 (en) | 2017-01-06 | 2023-02-09 | モリリン株式会社 | Mixed cotton batting |
| CN107326530A (en) * | 2017-06-15 | 2017-11-07 | 东华大学 | A kind of preparation method of increasing material manufacturing cotton fiber fabric |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1903289A1 (en) * | 1969-01-23 | 1970-07-30 | Talpay Dr Bela M | Non woven fabrics consisting of polyamide - or polyester or their mixtures with cotton |
| EP0044126B1 (en) * | 1980-07-10 | 1984-07-04 | Imperial Chemical Industries Plc | Coverstock fabrics |
| US4685914A (en) * | 1983-09-23 | 1987-08-11 | Personal Products Company | Disposable urinary pad |
| DE3541830A1 (en) * | 1985-11-27 | 1987-06-04 | Hartmann Paul Ag | Cotton swabs and process for their manufacture |
| CN1029414C (en) * | 1986-01-30 | 1995-08-02 | 张俊生 | Elasticized cotton wading by jet melt cohesion and processing |
| US4769022A (en) * | 1986-05-02 | 1988-09-06 | Minnesota Mining And Manufacturing Company | Cleansing pad |
| US4879168A (en) * | 1987-10-28 | 1989-11-07 | The Dow Chemical Company | Flame retarding and fire blocking fiber blends |
-
1990
- 1990-05-30 CA CA002017836A patent/CA2017836A1/en not_active Abandoned
- 1990-06-04 BR BR909002640A patent/BR9002640A/en unknown
- 1990-06-04 KR KR1019900008189A patent/KR910001129A/en not_active Application Discontinuation
- 1990-06-05 AU AU56271/90A patent/AU639866B2/en not_active Ceased
- 1990-06-05 EP EP19900110599 patent/EP0401738A3/en not_active Ceased
- 1990-06-05 JP JP2145556A patent/JPH0369649A/en active Pending
- 1990-06-05 CN CN90104558A patent/CN1083026C/en not_active Expired - Fee Related
- 1990-06-05 AR AR90317025A patent/AR243246A1/en active
Also Published As
| Publication number | Publication date |
|---|---|
| CN1048420A (en) | 1991-01-09 |
| BR9002640A (en) | 1991-08-20 |
| AR243246A1 (en) | 1993-07-30 |
| CN1083026C (en) | 2002-04-17 |
| JPH0369649A (en) | 1991-03-26 |
| EP0401738A2 (en) | 1990-12-12 |
| EP0401738A3 (en) | 1991-04-03 |
| KR910001129A (en) | 1991-01-30 |
| AU639866B2 (en) | 1993-08-05 |
| AU5627190A (en) | 1990-12-06 |
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