CN1051770A - The aramid fiber of deposit-free finish - Google Patents
The aramid fiber of deposit-free finish Download PDFInfo
- Publication number
- CN1051770A CN1051770A CN90109362A CN90109362A CN1051770A CN 1051770 A CN1051770 A CN 1051770A CN 90109362 A CN90109362 A CN 90109362A CN 90109362 A CN90109362 A CN 90109362A CN 1051770 A CN1051770 A CN 1051770A
- Authority
- CN
- China
- Prior art keywords
- fiber
- acid amides
- fragrant acid
- aramid fiber
- finishing agent
- 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.)
- Pending
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Classifications
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
- D06M13/295—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof containing polyglycol moieties; containing neopentyl moieties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
- Chemical Treatment Of Fibers During Manufacturing Processes (AREA)
Abstract
The present invention is a kind of aramid fiber, adopts the sylvite arrangement of ethoxylated alkyl phosphate, and at this, arrangement back fiber has showed outstanding antistatic property, and has in fact placed restrictions on finishing agent in fiber process deposition mechanically, obtains normal working ability.Selected finishing agent is the sylvite of list/two octanols (2EO) phosphate.
Description
The invention relates to aromatic arginyl amine fiber is put in order, not only increased the fiber surface lubricity and improved the antistatic property of fiber, and can not make fiber lose normal feel.With the fiber of the present invention of regulation finishing agent arrangement, during fiber product processing, on the fibre bundle and on other zone of fiber process operation seldom or do not have a deposition of finishing agent.
Come out from fiber is manufactured, arrangement is applied to the fiber of the overwhelming majority.Put feel or the easing characteristic that is used to change fiber in order with ad hoc fashion; The result who obtains arrangement on the fiber of certain material often is very special.
As an example, the sylvite of alkyl phosphate is used as finishing agent for a long time to reduce polyester and nylon fiber electric charge and gather and to improve its feel.In fact, this class aliphatic phosphate partly is successfully used to the antistatic finish of aromatic arginyl amine fiber, but during fiber process, on other unit that they are deposited on the fibre bundle loathsomely and fiber process is operated.
Fatty acid ester, for example coconut oil, castor oil, polyethyleneglycol/di fatty acid ester are often used as finishing agent improving the lubricity of aromatic arginyl amine fiber, but these compositions can not help to reduce electrostatic charge.
The invention provides a kind of aromatic arginyl amine fiber product, it has the long filament DENIER of 0.75-3 or 5, and has evenly applied the sylvite of ethoxylated alkyl phosphate on fiber, and quantity is the 0.2-1.0% of aramid fiber weight.
The present invention also provides a kind of method for preparing fiber product, this method comprises sets up a liquid arrangement to bathe, body lotion contains the sylvite (in the gross weight of body lotion) of the ethoxylated alkyl phosphate of 1-50%, the aramid fiber that with Denier values is 0.75-5 is bathed contact with aqueous arrangement, dry then aramid fiber makes it evenly to be coated with the sylvite of the ethoxylated alkyl phosphate that applies 0.2-1.0% on fiber.
Fiber of the present invention is an aramid fiber, and it can prepare with any aramid polymeric material.Preferred fragrant acid amides is to fragrant acid amides, be poly-(right-phenylene terephthalate amine) preferably to fragrant acid amides, term " to (right-phenylene terephthalate amine) (PPD-T) refer to equimolar right-homopolymers that phenylenediamine and terephthalyl chloride polymerization obtain, also refer to the right-phenylenediamine that mixes a spot of other aromatic diamine and mix the copolymer that the terephthalyl chloride polymerization of a spot of other aromatic dicarboxylic acid chloride obtains.As a common rule, in preparation PPD-T, other aromatic diamine that uses and the maximum of other aromatic dicarboxylic acid chloride are about right-phenylenediamine or terephthalyl chloride 10% mole, or it is higher slightly, other diamines and the diacid chloride that provide do not have active group, therefore do not influence polymerisation.Fiber can be made into the short silk or the continuous filament yarn of any DENIER.
Fragrant acid amides manufacturing between aromatic arginyl amine fiber equally also can be used, preferred between-the Fang acid amides is poly-(-the different phthalamide of phenylene).Between-the Fang acid amides and-Fang acyl family amine fiber can be that 324 is described as U.S. Pat-3,287.To fragrant acid amides with to aramid fiber can be that 429 is described as United States Patent (USP) 3,869.
Usually, aramid fiber is to get with the spinning solution wet spinning of fragrant amide polymer, after spinning head is extruded, by or do not pass one non-solidify slit after, spinning solution solidifies in a water-based coagulating bath.Washing in many ways and dry after coagulation step, this is having tension force or is not having under the tension force situation and carry out.
Arrangement of the present invention is being applied on the aramid fiber during the fiber production, and applies after washing step usually.Certainly, finishing agent is the aqueous solution, is applied on the fiber by the aqueous solution that fiber is passed finishing agent, then dried fibres.Very possible is that aramid fiber is still " never being dried " form with the contacted while fiber of water-based arrangement bath.Fiber still keeps at least the water that brings from spinning process of about 20wt% before applying arrangement.Finishing agent is applied to more finishing agent is drawn in the fibre structure.Advantage of the present invention can be applied on the dry fiber that cross or that never be dried by finishing agent to be familiar with, and it is more effective than the arrangement that is coated on the fiber outer surface to believe that finishing agent is bonded in fiber.But preferred and more actual is that finishing agent is put on dry fiber.
In the yarn preparation, many fibers are owing to rupturing with fiber deflector roll or the contact of other gripping device, and yarn is owing to the formation of electrostatic charge is ruptured sometimes.Arrangement provides lubricant fiber and has eliminated electrostatic charge, has therefore reduced the damage of fiber, has improved the processing characteristics of fiber.In fragrant acid amides yarn production field, need more effective arrangement to improve process velocity significantly; It is very clear and definite needing more effective arrangement in the production of fragrant acid amides short fiber.
By using the RING SPINNING method that but discontinuous staple fibre is produced continuous yarn, this method briefly may further comprise the steps.
(ⅰ) open a position, the staple fibre of " package " machine compacting is formed loose staple fibre, continuous compacting becomes loose formula web and is called " lap in flakes ",
(ⅱ) mix (combing) lap, therefore, discontinuous staple fibre in fact parallelization and make these parallelizations staple fibre become loose continuous band, this is called " carded sliver ".
(ⅲ) carded sliver of row of mixing makes it to become one, and many, even a branch of being called " tensile bars ", independent here staple fibre can stretch by stretching-machine become many parallel relations.
(ⅳ) further stretch one or several tensile bars that combines make it to become a continuous line, and term is called " rove ", is having than under the low-tension rove being twisted by the Speed frames device; With
(ⅴ) stretch and further twisting, slubbing is to produce " yarn " on the RING SPINNING machine.The short suddenly yarn production technology of this multistep is because deposition yarn contact surface, carded webs for example, and draw roll, therefore the spinning roller has caused tangible fibre damage, and sedimental generation has caused fiber further to damage, roll cladding and reduced productivity ratio.
In further operation, for example heat treatment is reeled etc., and fiber is arranged to pass the deflector roll of row to carry out yarn arrays and layout.This further technology also can make fiber deposit on deflector roll equipment, and the problem that this deposit produces is just to have tension force to affact on the fiber because deposit produces when aromatic arginyl amine fiber passes, and produces friction between fiber and deflector roll.The present invention includes a kind of arrangement, its can improve finish solution the improved stability fiber electric charge and during producing short yarn in guide roller surface or producing and on other holder, produce deposition before or after can spinning.
Finishing agent of the present invention comprises a kind of sylvite of ethyoxyl aliphatic phosphate ester, particularly list or dialkyl phosphate.Aliphatic portion is the alkyl of 8-18 carbon in the finishing agent, and two or three chain ethoxy groups are arranged, and the finishing agent molecular structure is as follows:
The monoalkyl dialkyl group
R=C wherein
nH
2n+1(EO)
1-3
EO is the ethoxy group, and n is 8-18
Finishing agent composition of the present invention can react with phosphorus pentoxide by the aliphatic alcohol with 8-18 carbon atom and 2 or 3 oxireme groups, prepares with the potassium hydroxide neutralized product then.The oxireme group has increased the water-soluble of finishing agent, has reduced the generation of deposition.
As previously mentioned, finishing agent of the present invention be dissolved in excessive 50% or more water in, be benchmark with the weight of water.In any case the excessive dissolving of finishing agent material has been placed restrictions on and has been easy to emulsification or dispersion.The application of finishing agent of the present invention under the big portion situation, is bathed into arrangement by fiber is tilted and to be realized that this arrangement bath is prepared by the aqueous solution of finishing agent compound.In the arrangement bath, the concentration of finishing agent is such, and promptly when contact and arrangement bath drying are bathed in the arrangement of all others of consideration, fiber product will have the finishing agent of about 0.2-1.0%, and this is a benchmark with initial aramid fiber weight.For the great majority practice, during bathing, arrangement should comprise the finishing agent compound of 1-50%.
Because finishing agent of the present invention is water miscible, and can use with aqueous solution form, so it is just effective especially, solution application allows finishing agent to apply equably, and does not have too much or very few zone.But water-soluble is not unique quality index of the aramid fiber well handled.When having determined that the arrangement of water-soluble finishing agent puts on the aramid fiber for several times, the aramid fiber product of producing has level and smooth finish coating and good electrostatic property; When crossing the yarn contact surface, those arrangements on aramid fiber have stayed the deposit that generates continuously, the example of the water-soluble finishing agent of excess deposition thing that these stay on contact surface is a potassium alkyl phosphate, and at this, alkyl has 4-12 carbon atom; The sylvite of ethyoxyl alkyl amine sulfuric ester is tallow amine diethyl sulfide acid esters, comprises 2-20 ethylene oxide group at this ox ester; The alkyl phosphate of diethyl amine salt, here alkyl is the mixture of 8,10,12 carbon atoms; The sylvite of alkyl phosphoric acid ethyl acid esters is 8 carbon atoms at this alkyl.
Have to be noted that in the present invention the finishing agent that uses combines the monomer of top listed material, and become the finishing agent of premium properties, although other material of poor performance is made up of similar sometimes.
In fact, the aromatic arginyl amine fiber that the present invention is based on has the specific sorted material-sylvite of ethyoxyl aliphatic phosphate to show the combination of quality, and it has showed the combination of unique fiber and arrangement.
Test method
Be dissolved in finishing agent on the sample yarn by methyl alcohol and be determined at finishing agent (FOY) on the yarn.Evaporation methyl alcohol claims remaining weight to dry, claims clean yarn sample heavy, calculates the finishing agent percentage on clean yarn:
FOY%=(remaining arrangement dosage)/(clean yarn is heavy) * 100
Use electron microscope to measure the arrangement uniformity, check fiber quality.In a large amount of arrangement things, the stain of interruption is represented the arrangement uniformity of " bad "." medium " arrangement uniformity is represented with the measurement microscope arrangement continuous basically, but is inhomogeneous coating.It is to apply continuously and evenly that the arrangement uniformity of " good " refers to the measurement microscope arrangement.Outstanding arrangement uniformity can not be used microscopic examination.
The finishing agent deposition is to measure the finishing agent material to be deposited in amount on test thread frame or the creel, promptly under the specified conditions, and the amount of being piled up by the known quantity fiber.
In order to test, yarn was with 100yard/ minute speed.1.5g/d tension force, 180 ° of cornerites, were removed and are deposited in the finishing agent that deposits on the roller, and weigh after two minutes by two 14 roller tension force saddles two minutes, calculated the gross weight of passing the deflector roll yarn.The finishing agent of deposition is heavily represented with the yarn of deposition (milligram)/pass deflector roll:
Deposition (mg/kg)=(deposit is heavy)/(yarn is heavy) * 10
6
Embodiment
In this example, prepare fiber of the present invention, and utilize finishing agent of the present invention relatively with the contrast fiber.
It is 1.5 that dry PPD-T copolymer fibre continuous filament yarn has the long filament Denier values, and it is imported in the arrangement bath, and it is the finishing agent of 15wt% that this bath has concentration; After arrangement one was soaped, long filament was imported into a curler with crimp filament, and removes unnecessary finisher solution, when needs obtain required arrangement yarn, add other finishing agent then to the long filament that has curled, long filament cuts into staple fibre, length is 1 1/2-2 inches, and staple fibre is packaged then.Use RING SPINNING staple fibre continuous spinning.
To staple fibre test finish content, arrangement uniformity and finishing agent deposition.
In test the finishing agent of Shi Yonging and from the experiment obtain the results are shown in the following table:
The table of finishing agent
Test number (TN)
1 C
10H
21(2EO) PO
4Acid esters, sylvite
2 C
10H
21(EO) PO
4Acid esters, sylvite
3 C
12H
25(2EO) PO
4Acid esters, sylvite
4 C
8-10(1.5EO) PO
4Acid esters, sylvite
A [C
12H
25]
1-2PO
4Acid esters, sylvite
B C
4H
9PO
4Acid esters, sylvite
C C
6H
13PO
4Acid esters, sylvite
D C
8H
17PO
4Acid esters, sylvite
E C
8H
17, C
10H
21, C
12H
25PO
4The acid esters mixture, K salt,
F tallow amine (2EO) diethyl sulfide acid esters, K salt
G tallow amine (5EO) diethyl sulfide acid esters, K salt
H tallow amine (10EO) diethyl sulfide acid esters, K salt
I tallow amine (20EO) diethyl sulfide acid esters, K salt
J C
8H
17, C
10H
21, C
12H
25PO
4Acid esters, DEA
*Salt
K C
8H
17C
2H
5PO
3(phosphate) acid esters, K salt
* DEA=monoethanolamine
Table
Number of times is put uniformity finishing agent deposition in order on yarn
1 0.39 excellent 0
2 0.47 excellent 0
3 0.20 excellent 0
4 0.45 excellent 0
A 0.30 difference is heavy
*
B 0.50 is excellent heavy
C 0.50 is excellent heavy
D 0.50 is excellent heavy
E 0.50 is excellent heavy
F 0.99 excellent 19.3
G 1.01 excellent 31.0
H 1.04 excellent 37.0
I 0.88 excellent 37.7
J 0.50 is excellent heavy
K 0.50 is excellent heavy
* " weight " deposition means the deposition degree measured greater than 10mg/kg.
Claims (18)
1, a kind of long filament DENIER is 0.75-5 aramid fiber and the aromatic arginyl amine fiber that evenly is coated with the ethoxylated alkyl phosphate sylvite of the heavy 0.2-1.0% of fragrant acid amides on fiber.
3, as aramid fiber, wherein R=C as described in the claim 2
10H
21(EO)
2
4, fiber as claimed in claim 1, wherein fragrant acid amides is to fragrant acid amides.
5, fiber as claimed in claim 4 is poly-(right-phenylene terephthalate amine) to fragrant acid amides wherein.
6, fiber as claimed in claim 1, wherein fragrant acid amides be between fragrant acid amides.
7, fiber as claimed in claim 6, fragrant acid amides is poly-(-the different phthalamide of phenylene) in the middle of it.
8, a kind of long filament DENIER is the staple fibre of aromatics fiber of the ethoxylated alkyl phosphate sylvite of 0.75-5 aramid fiber and the 0.2-1.0% that evenly is coated with fragrant acid amides weight on fiber.
10, staple fibre as claimed in claim 9, wherein R=C
10H
21(EO)
2
11, staple fibre as claimed in claim 8, wherein fragrant acid amides is to fragrant acid amides.
12, as the staple fibre of claim 11, be poly-(right-phenylene terephthalate amine) wherein to fragrant acid amides.
13, the method for preparing the aramid fiber product comprises the following steps:
A) setting up one, what 1-50% was arranged is the water-bath of sylvite of the ethoxylated alkyl phosphate of benchmark with the water yield
B) aramid fiber with the 0.75-5 DENIER contacts with water-bath; With
C, dry aramid fiber, even coating one deck 0.2-1.0% phosphate on fiber is as the criterion with the weight of fragrant acid amides.
14, as the method for claim 13, wherein aramid fiber is that " never being dried " is in fiber, in the beginning contact procedure time.The water yield is greater than 20wt%.
15, as the method for claim 13, wherein phosphate has at least a structure that can select from following array structure:
R=C wherein
nH
2n+1(Eo)
1-3
Eo is an ethylene oxide group, n=8-18.
16, as the method for claim 15, R=C wherein
10H
21(EO)
2
17, as the method for claim 13, wherein fragrant acid amides is to fragrant acid amides.
18, as the method for claim 17, be poly-(right-phenylene terephthalate amine) wherein to fragrant acid amides.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US42201389A | 1989-10-16 | 1989-10-16 | |
US422,013 | 1989-10-16 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN1051770A true CN1051770A (en) | 1991-05-29 |
Family
ID=23673030
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN90109362A Pending CN1051770A (en) | 1989-10-16 | 1990-10-16 | The aramid fiber of deposit-free finish |
Country Status (10)
Country | Link |
---|---|
EP (1) | EP0423703A3 (en) |
JP (1) | JPH03185180A (en) |
KR (1) | KR910008184A (en) |
CN (1) | CN1051770A (en) |
AU (1) | AU629993B2 (en) |
BR (1) | BR9005205A (en) |
CA (1) | CA2027661A1 (en) |
IE (1) | IE903679A1 (en) |
NO (1) | NO904449L (en) |
PT (1) | PT95604A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104271820A (en) * | 2012-05-09 | 2015-01-07 | 帝人芳纶有限公司 | Textile reinforcement comprising continuous aramid yarn |
CN105189854A (en) * | 2013-03-15 | 2015-12-23 | 帝人芳纶有限公司 | Method for high speed stranding of aramid yarns |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4402193C1 (en) * | 1994-01-26 | 1995-06-01 | Hoechst Ag | Aramid fibres for textile prodn. |
DE4410708C1 (en) * | 1994-03-28 | 1995-07-13 | Hoechst Ag | Aramid fibre with good mechanical, antistatic and processing properties |
EP1435407A1 (en) * | 2003-01-02 | 2004-07-07 | Teijin Twaron B.V. | Aramid filament yarn provided with a conductive finish |
CA2583211A1 (en) | 2004-11-01 | 2006-05-11 | Teijin Techno Products Limited | Para-type aromatic polyamide short fibers |
US7976943B2 (en) | 2007-10-09 | 2011-07-12 | E. I. Du Pont De Nemours And Company | High linear density, high modulus, high tenacity yarns and methods for making the yarns |
KR101310136B1 (en) * | 2008-04-30 | 2013-09-23 | 코오롱인더스트리 주식회사 | Aramid multi-filament and method of manufacturing |
US20130157054A1 (en) | 2011-12-20 | 2013-06-20 | E.I. Du Pont De Nemours And Company | High linear density, high modulus, high tenacity yarns and methods for making the yarns |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3926816A (en) * | 1970-05-22 | 1975-12-16 | Goulston Co George A | Textile fiber lubricants |
JPS531342B2 (en) * | 1972-05-08 | 1978-01-18 | ||
US4126564A (en) * | 1977-12-12 | 1978-11-21 | Allied Chemical Corporation | Spin finish for polyamide carpet yarn |
US4256589A (en) * | 1978-02-16 | 1981-03-17 | Eastman Kodak Company | Fiber treating compositions comprising (a) blend of random copoly(oxyethylene-oxypropylene)butanols (b) alkali metal sulfur compound and (c) alkali metal organic phosphate compound |
US4191656A (en) * | 1978-10-05 | 1980-03-04 | Allied Chemical Corporation | Non-yellowing biocide for control of bacteria in spin finish emulsions used on nylon yarn |
CA1150008A (en) * | 1978-11-06 | 1983-07-19 | Peter A. Taylor | Finishes for polypropylene textile materials, process and product thereof |
US4452709A (en) * | 1981-10-09 | 1984-06-05 | Lester Laboratories, Inc. | Antistatic composition |
JPS58156079A (en) * | 1982-03-09 | 1983-09-16 | 帝人株式会社 | Treatment of aromatic polyamide synthetic fiber |
US4624793A (en) * | 1984-06-20 | 1986-11-25 | National Distillers And Chemical Corporation | Fiber finishes |
-
1990
- 1990-10-15 IE IE367990A patent/IE903679A1/en unknown
- 1990-10-15 NO NO90904449A patent/NO904449L/en unknown
- 1990-10-15 CA CA002027661A patent/CA2027661A1/en not_active Abandoned
- 1990-10-16 AU AU64656/90A patent/AU629993B2/en not_active Withdrawn - After Issue
- 1990-10-16 EP EP19900119787 patent/EP0423703A3/en not_active Withdrawn
- 1990-10-16 PT PT95604A patent/PT95604A/en not_active Application Discontinuation
- 1990-10-16 CN CN90109362A patent/CN1051770A/en active Pending
- 1990-10-16 KR KR1019900016422A patent/KR910008184A/en not_active Application Discontinuation
- 1990-10-16 JP JP2275473A patent/JPH03185180A/en active Pending
- 1990-10-16 BR BR909005205A patent/BR9005205A/en unknown
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104271820A (en) * | 2012-05-09 | 2015-01-07 | 帝人芳纶有限公司 | Textile reinforcement comprising continuous aramid yarn |
CN104271820B (en) * | 2012-05-09 | 2016-06-01 | 帝人芳纶有限公司 | Comprise the textile reinforcement of continuous aramid yarn |
CN105189854A (en) * | 2013-03-15 | 2015-12-23 | 帝人芳纶有限公司 | Method for high speed stranding of aramid yarns |
Also Published As
Publication number | Publication date |
---|---|
NO904449L (en) | 1991-04-17 |
IE903679A1 (en) | 1991-04-24 |
EP0423703A3 (en) | 1991-08-28 |
AU6465690A (en) | 1991-04-18 |
CA2027661A1 (en) | 1991-04-17 |
BR9005205A (en) | 1991-09-17 |
PT95604A (en) | 1991-09-30 |
NO904449D0 (en) | 1990-10-15 |
KR910008184A (en) | 1991-05-30 |
EP0423703A2 (en) | 1991-04-24 |
AU629993B2 (en) | 1992-10-15 |
JPH03185180A (en) | 1991-08-13 |
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