CA1234703A - Mixture of fibres for the reinforcement of construction materials, specifically for the reinforcement of hydraulic binding agents, a method of reinforcing construction materials, and formed articles of said mixture - Google Patents
Mixture of fibres for the reinforcement of construction materials, specifically for the reinforcement of hydraulic binding agents, a method of reinforcing construction materials, and formed articles of said mixtureInfo
- Publication number
- CA1234703A CA1234703A CA000475492A CA475492A CA1234703A CA 1234703 A CA1234703 A CA 1234703A CA 000475492 A CA000475492 A CA 000475492A CA 475492 A CA475492 A CA 475492A CA 1234703 A CA1234703 A CA 1234703A
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- Prior art keywords
- fibres
- mixture
- pan
- pva
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-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B16/04—Macromolecular compounds
- C04B16/06—Macromolecular compounds fibrous
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
The mixture of PVA- and PAN-fibres comprises at least 10 %
PVA-fibres. The mixture is utilized to produce asbest-less, fibre-reinforced, hydraulically setting material by processing a suspension of hydraulic binding agent, fibres, water and possibly further additives on machines commonly used in the asbestos cement industry. The reinforcing fibres are preferably re-duced mixtures of 50 - 90 % polyacrylnitrile fibres of a high modulus and of a length of at least 2 mm.
The mixture of PVA- and PAN-fibres comprises at least 10 %
PVA-fibres. The mixture is utilized to produce asbest-less, fibre-reinforced, hydraulically setting material by processing a suspension of hydraulic binding agent, fibres, water and possibly further additives on machines commonly used in the asbestos cement industry. The reinforcing fibres are preferably re-duced mixtures of 50 - 90 % polyacrylnitrile fibres of a high modulus and of a length of at least 2 mm.
Description
~2~7~33 A MIXTURE OF FIRES FOR THE REINFORCEMENT OF CONSTRUCTION
MATERIALS, SPECIFICALLY FOR THE REINFORCEMENT OF HYDRAULIC
BINDING AGENTS, A METHOD OF REINFORCING CONSTRUCTION
BACKGROUND OF THE INVENTION
nun a I EVE ,rlcN
The present invention relates to a mixture ox fires for the production of fire reinforced Construction materials, such as e.g. hydraulically setting materials, specifically of a cementitious material having reinforcing fires in form of polyacrylni-trlle fires and polyvinyl alcohol fires. The in-mention relates further to a method of reinforcing sunk con-struction materials by such mixtures of fires which set after the molding thereof.
The polyacrylnitrile fires will be referred to throughout this specification as PAN-fibres and the polyvinyl alcohol fires will be referred to as PVA-fibres.
MATERIALS, SPECIFICALLY FOR THE REINFORCEMENT OF HYDRAULIC
BINDING AGENTS, A METHOD OF REINFORCING CONSTRUCTION
BACKGROUND OF THE INVENTION
nun a I EVE ,rlcN
The present invention relates to a mixture ox fires for the production of fire reinforced Construction materials, such as e.g. hydraulically setting materials, specifically of a cementitious material having reinforcing fires in form of polyacrylni-trlle fires and polyvinyl alcohol fires. The in-mention relates further to a method of reinforcing sunk con-struction materials by such mixtures of fires which set after the molding thereof.
The polyacrylnitrile fires will be referred to throughout this specification as PAN-fibres and the polyvinyl alcohol fires will be referred to as PVA-fibres.
2. DESCRIPTION OF THE PRIOR ART
The leasability of producing shaped articles such as puffins, corrugated plates pipes or garden articles in various forms prom hydrous suspensions comprising e.g. asbestos and cement by means of dehydrating machines, echoic mechanizer by means ox injection methods is generally known. Such articles were able to secure a dominant position among construction material during the past decennials In the course of the recent years it has increasingly become obvious that the most important raw material or the production of these products, namely asbestos, will soon no longer be available for such utilization due to various reasons, such as availability, ~3~7Q~
development of costs as well as due to health considerations.
It is not only the known excellent service properties of asbestos cement which are based on the unique combination of properties inherent in asbestos fires, said properties form additionally the basis of the Hatscheck-dehydrating methods which are known world wide All of the above circumstances have caused in the recent years an intensive research activity having as object the finding of replacement fires which can completely replace the as-bests in the known manufacturing processes of the dodder-tying methods. It has, however, been discovered extremely soon that not one kind of fires would be found which incorporated all positive properties of asbestos.
Following properties characterize asbestos as excellent pro-diction process as well as reinforcement fires:
- large specific surface - excellent dispersive power - outstanding chemical festivity - high concrete retention capability - excellent capability of forming nonwovens - high breaking strength high modulus of elasticity - small elongation at fracture Asbestos displays as process expedient means an excellent dispersive power in an hydraulic cement suspension. Due to its high filtration capability and its affinity to cement asbestos is in to position to retain the binding agent forming in the cement during the dehydrating process step, The high breaking strength combined with the high modulus of elasticity and the small elongation at fracture have a post-live effect on the hydrated final article which can bestow ~23~7Q3 the a~bestos-cement products the known high bending strength.
Because neither natural nor synthetical fires having the combination of properties of asbestos could be found, search efforts for finding possible replacement products lead to the realization that commensurate with the two main functions of asbestos mixtures of fires must be made use of in order to be able to carry out a production utilizing such new fires on existing machines and apparatuses (see e.g. DEEPS
30 02 484 of Amounts). The filtration properties of asbestos can be simulated in the fire mixtures by additions of cell-lose and/or synthetic fib rides. Regarding the reinforcing properties reinforcing fires are made use of. Such fires may be organic or inorganic high modulus flares which are added usually in a cut length of 4-12 millimeters.
There hardly exists a synthetic fire which has not been tested regarding such application as cement reinforcing cement. Most of these fires did, however, not succeed due to a large variety ox reasons, such as insufficient chemical resistivity, bad affinity to cement, unsatisfactory mechanical properties or due to the exceedingly high price. Among the entire available fires only two types of synthetic fires which meet the demands of a cement reinforcing fire were able to prevail. One of these fires has been developed on the basis of polyacrylnitrile and has been marketed for in-stance by the Hoechst Company (Western Germany under the trademark "Nolan 10"~ The other fiber is formed on -the basis of polyvinyl alcohol and is e.g. available from the Queerer C. Japan under the trademark "Kuralon" (DEEPS 28 50 337~. The most important properties of these fires are tabulated in table 1.
Table 1 Textllemechanical proper-ties of types of fires suitable as reinforcement of cement:
_ _ Type of fire breaking elongation modulus of strength at fracture elasticity cN/dtex % cN/dtex Polyacrylnitril, PAN (e.g. * 690 - 8,5 10 - 16 mint 130 "Nolan 10") Polyvinyl alcohol, PEA 10 - 15 5,5 - 15 min. 175 (ego "Kuralon~') l _ .
The comparison of -the textile-mechanical properties between the PVA-fibres and the PAN-fibres reveals that the PVA-fibres display -the better mechanical properties. If now fire cut-tongs having a length of 6 millimeters of both types are distributes in an hydraulic cement suspension and worked on a filter press to fire cement plates, the measured strength values of such plates reveal that the better properties of the fires can also bestow the final product with better strength properties (table 2).
Table 2 Strength properties of plates of fibre-cement, produced on a filter press, of port land cement and the high modulus fires on the basis of PEA and PAN.
_ .
fires bending energy of density absorption strength fracture of water wit,% N/mm2 kJ/m2 g/ccm fires __ 1,0 12,5 0,203 ~,982 15,0 1,5 14,7 0,457 19920 14,5 ' _ 16,0 0,701 1~851 15~7 fires 1,0 14,8 0,652 1,935 14,6 1,5 16,1 1,208 1,900 15,1 2,0 19,5 1,835 1,863 16,0 . ................................. .. _ .
Jo - * Trade mark ~3~7~3 Textile mechanical properties of the fires used.
_ Breaking Modulus of Elongation Titer strain elasticity at fracture cN/dtex cN/d-tex _ _ dtex PAN 7,5 150 11 to PEA 12 240 _ __ _ _ The energy of fracture incorporates an extremely important material technological property. It gives evidence of the brittleness or impact tensile strength, rest. of a product.
This can have such effect in a practical application that e.g.
when placing of roof covering plates having differing values of an energy of fracture, but identical bending strengths, some plates may break suddenly without prints when sub-jacketed to a loading by a roofer (brittleness), however, in the second case may take the loading up by a larger bending.
The analysis of the results reveals that in comparison with the PAN-fibres the PVA-fibres having the better textile-mechanical properties can not only bestow the fibre-cement plates with a higher bending strength, but that their energy of fracture is larger, too. In these tests, the energy of fracture is defined as the surface area under the strain-elon-gallon curve up to the point where the maximal bending strength is reached, i.e. the plate has ruptured (fig. 1).
By knowledge of the relationship between -the data of the fires and -the product proper-ties ox the fibre-cement plates resulting these from it would be an easy task to produce fire-cement products exposed to high demands regarding bending strength and energy of fracture exclusively by utilizing PEA-fires. However, -the high costs of PVA-fibres counteract this solution. Due -to the high costs of the raw material combined with an extremely intrinsic fire production process, the costs 7~33 of producing PVA-fibres are 50 - 100 % higher than those of PAN-fibres.
Considering additionally that the present prices of asbestos amount to a fraction only of the prices of synthetic fires it is quite obvious that a decisive importance must be given to the price of the fires to allow the production of market table fire cement products at all. Accordingly, it would be a highly desirable object for the fibre-cement industry to provide a fire having the properties of the PVA-fibres desk cried above which, however, is economically acceptable, i.e.
not substantially more expensive than the PAN-fibre.
According to the rules of mixtures for fire reinforced come pound construction materials it should be expected that in Gaze of reducing ire mixtures the strength properties or energy of rupture, rest. resulting in the reinforced material follow linearly and proportionally the mixing ratio (see "Fiber-Reinforced Cement Composites", Technical Report 51.067, The Concrete Society, Terminal House, Grosvenor Gardens, London 1973 and H. Crinkly "Fiber Reinforcement", Akademisk Foreleg, Copenhagen, 1964).
SUMMARY OF TOE INVENTION
Hence, it is an object of the invention to provide a fire no-enforcement mixture in which cheap PAN-fibres are substituted for a large amount of PVA-fibres without suffering a loss of the positive properties in the fibre-cement product.
A further object is to provide a mixture of fires for the production of fibre-reinforced concrete comprising PEA- and PAN-fibres and having as little as possible, at least, how-ever, 10 % PVA-fibres.
I
- pa -Therefore the present invention relates to a mixture of polyacrilnitrile and polyvinyl alcohol fires as reinforcing fires for materials setting after the molding thereof, specifically for hydraulically setting materials, said mixture of fires comprising about 50-90% polyacrilni-trite fires and about SUE polyvinylalcoho e .,~.
~3'~L'7(~'3 DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
I.. _ ..__ . . . ... . .. _ _ _ The mixtures of fires realized by the present invention will be explained now based on following testing examples made in the praxis.
Suitable fires for the production of the decrease-mixtures of PAN- with PVA-fibres are polyacrylnitrile fires having a high modulus, a modulus of elasticity of at least 130 cN/dtex, an elongation at fracture of maximal 16 % and a breaking strength of a-t least 6 cN/dtex~
Suitable polyvinyl alcohol fires are high modulus fires ha-vying following specifications:
Modulus of elasticity ox at least 175 cN/dtex, elongation at fracture of maximal 15 % and a breaking strength of at least 10 cN/dtex.
Both kinds of fires can be used with uniform titers or as mixtures of fires of differing titers. Preferred use is made of fires in the range of 0.5 - 5.0 dtex. The fires can be cut either to exact, uniform lengths or when be ground or mixed in various lengths, Preferred is the application of the PVA-fibres in lengths of 4 - 15 mm and the PAN-fibres in lengths of 2 - 12 mm.
The hollowing examples will disclose that it is specifically advantageous if the PVA-fibres used are larger than the ad-mixed fires by about 1/3.
Possible production methods for structural members or articles, in which the fire mixtures according to the invention are used are e.g. dehydrating method by sitting drum machines or fourdriniers, however also mono-extrusion machines, injection apparatuses or filter-presses.
~3~7~?3 Mixtures which are suitable for a production on above macho-noes comprise in a hydrous suspension apart of the inventive fire mixtures also a binding agent, such as e.g. cement and possibly additional fibrous materials having filtering pro-parties as well as a variety of filling materials or additives.
Suitable binding agents are hydraulic inorganic binding agents such as cement, gypsum earth alkaline silicates or earthalka-line ailments However, organic binding agents such as e.g.
synthetic resins may be used too. Suitable filling materials or additives are e.g. quartz sand, blast-furnace slag, fly ash, pu~zolane, mica, rock dust. Suitable auxiliary fires operative to retain the binding agents and additives on the screens may be cellulose fires in form of sulfate cellulose, wood shavings, thermomechanical pulp and/or synthetic fib rides on the basis of plastic materials, e.g. polyethylene. The retention capability can be improved additionally by the use of flocculation agents, e.g. on -the basis of polyacrylamides.
Products which can be produced with those mixtures on the de-hydrating machines are e.g. planar plates, corrugates plates or boards, tubes or shaped articles,e.g. garden articles.
The inventive PVA/PAN-fibre mixtures will now be explained based on a number of exemplar applications.
The tests were made on a sifting drum dehydrating machine of the Hatschek design.
The fibre-cement-suspensions were prepared in a separate put-per and comprised a solids content of 80 g/l and continuously pumped from the pulper into the material chamber of a Hatschek-machine.
Shortly before entering into the material chamber, a dosage of 200 Pam of a flocculation agent type polyacrylamide was added to 3 for improving the retention of the cement. On the machine plates of about 6 mm were produced by 2Z full notations of the pattern plate, which plates were pressed between oiled plates during 60 minutes in a staple press at a specific pressing pressure of 250 bar to a thickness of 4,8 mm. Of all variations unpressed specimens were produced and tested, too.
The setting of the fibre-cement plates proceeded in a wetting room of 100 % relative humidity at 20C. After the plates were additionally stored for 3 days submerged in water, the tests were made in a wet or damp, rest. condition.
by xtu s used For the production on filter press:
Port land cement (2800 Elaine) 100 parts fire mixtures 2.0 parts For the production according to the Hatschek method:
Port land cement (2800 Elaine) 100 parts Old waste paper (45 SO) 3.5 parts Polyethylenefibride ~"Pulpex"E~A, Hercules USA) 2.0 parts fire mixtures 2.0 parts Following variants were used as fire mixtures:
PAN 2 1,7 1,3 1~0 0,7 parts PEA 0 0,3 0.7 1,0 I 2,0 parts The textile-mechanical proper-ties of the fires were:
- PAN
Titer 1,5 dtex, breaking strength 7,2 cN/dtex, modulus of elasticity 140 cN/dtex, elongation at fracture 9 %
- PEA
Titer 2 dtex, breaking strength 12,5 cN/dtex, modulus of elasticity 250 oN/dtex, elongation at fracture 6,5 %
*Trade mark , "I., ;. -~3'~7~P3 PAN and PEA fires were used in a variety of combination of 4 and 6 mm cut lengths.
For the tests on the filter press mixtures were prepared in water which consisted only of Port land cement and the PVA/PAN-fires.
The test of the fire cement plates proceeded by aid of a Wolpert testing apparatus having a three-point bearing con-tact on plates of 25 x 25 mm. The bearing contact distance amounted to 167 mm and the test speed to 26 mm/min. The anal louses of the results were made by aid of a computer connected to the testing apparatus.
do Results The results are tabulated in the tables 3 to 7.
7~3 Table 3 Test results ox fire cement plates having variable PVA-PAN-fire rations, produced on a Ha-tschek-machine.
. ___ .
fire mixture bending energy of Density Absorption PAN PEA strength fracture of water 6 mm 6 mm parts parts N/mm2 kJ/m2 g/ccm %
_ press plates _ 2,0 22,4 3,047 1,941 12,3 0~3 1,7 21,1 2,799 1,934 11,4 0,7 1,3 21,8 2,884 1,943 10,9 1,0 1,0 20,7 2,698 1,928 12,0 1,3 0,7 21,3 2,532 1,919 11,9 1,7 0,3 19,0 2,105 1,932 12,4 2,0 - 1791 1,108 1,911 12,1 -- A. . Jo ._ ______ . ._ _ unpressed plates __ - 2,0 14,8 4,272 1,555 20,1 0,3 1,7 14,7 3,820 1,567 19,9 0,7 1,3 14,5 4,133 1,557 19,8 1,0 1,0 13,6 3,740 1,539 21,2 1,3 0,7 13,8 4,010 19500 23,7 1,7 0,3 13~1 3,205 1,532 20,8 2,0 - 12,4 1,902 1,514 21,9 ._ _.___ e_ _, ,_,, Table 4 Test results of fire cement plates having variable PAP
fire rations, produced on a filtering press.
_ .
fire mixture bending energy of density absorption PAN PEA strength rupture of water 6 mm 6 mm parts parts _ _ Kim g/ccm %
_ 2,0 14,2 2,603 1,753 19,9 0,3 1,7 14~4 2,512 1,758 19,8 0,7 1,3 13,9 2,543 1,752 1997 1,0 1,0 13,9 2,527 1,754 19,8 1,3 0,7 1397 2,410 1,732 19,9 1,7 0,3 13,1 1,700 1,748 19,6 2,0 - 12,2 0,9'75 1,731 19,8 . ___ . ... _ . _ ~347~3 Table 5 Test results of fire cement plates having variable - PVA-PAN-fibre rations, produced on a Hatschek-machine.
__ _ _ fire mixture bending energy of density absorption PUN PEA strength rupture of water6 mm 4 mm parts parts N/mm2 Kim g/ccm %
, _ _ _ _ . __ pressed plates _ 2,0 24,2 3,075 1,93512,6 0,3 1,7 23,1 2,418 199421176 0,7 1,3 20,4 1,990 1,91912,0 1,0 1,0 19,2 2,001 1,92011,6 193 0,7 18S9 1,820 1,92311,2 1~7 0,3 17,5 1,221 1,91711,8 2,0 - 17,1 1,108 1,91112,0 _ unpressed plates - 2,0 15,0 4,519 1,55022,6 0,3 1,7 14,7 4,059 1,54122,4 0,7 1,3 14,2 3,465 1,52821,9 1,0 1,0 13,4 2,968 1,53620,4 1,3 0,7 13,1 2~436 1,53220,4 197 0,3 12,7 2,150 1~52121,3 2,0 - 12,4 2,100 1,51421,9 . _ _ . _ SKYE
Table 6 Test results of fire cement plates having variable PVA-PAN fire rations, produced on a filtering press ire mixture bending energy of density absorption PAN PEA strength rupture of water 6mm 4 mm parts parts N/mm2 kJ/m2 g/ccm __ _ __ _ 2~0 14,8 2,429 1,807 18,7 0,3 1,7 15,3 2,510 1,823 17,7 0,7 1~3 14,0 2,010 1,779 18,6 1,0 1,0 13.5 1,619 1,785 18,2 1,3 0,7 12,9 1,327 1,761 18,8 1,7 0,3 1295 0,902 1,750 18,7 2,0 12,4 0,945 1,747 18,9 __ 7~3 Table 7 Fibre-cement plates produced in accordance with the invention and having materials PVA-PAN-ratios, produced on a Hatschek-machine.
.
fire mixture bending energy of density absorption PAN PEA strength rupture of water 4 mm 6 mm parts parts N/mm2 Kim g/ccm %
_ Do Do .
_ 2,0 22,6 3 9 331 1,938 12,2 0,3 1,7 22,8 3,115 1,933 12,1 0,7 1,3 22,1 ~101 1,941 11,0 1,0 1~0 22,0 2,987 1,9~1 11,5 1,3 0,7 21,3 2,605 1,929 12,3 1,7 I 18,2 1,980 1,937 12,0 2,0 - 15,3 0,972 1,941 11,1 unpressed plates _ 2,0 15,1 4,657 1,548 22,3 0,3 1,7 15,2 4,450 1,551 22,0 0,7 1,3 14,8 4,522 1,550 21,9 1,0 1,0 14~8 4,186 1,542 22,6 1,3 0,7 14,1 3,475 1,553 21,9 1,7 0,3 12,9 2,497 1,561 20,7 2,0 - 11,7 1,303 1,568 19,9 Textile-mechanical properties of the fires used in table 7.
Titer 3,0 dtex, breaking strength 7,3 cN/dtex modulus of elasticity 152 cN/dtex elongation at rupture 9,8 %
Titer 2,0 dtex, breaking strength 12,5 cN/dtex modulus of elasticity 250 cN/dtex elongation at rupture 6,5 I.
While there are shown and described a number of embodiments of the present invention, it shall be clearly understood that such are for sake of illustration only and not to be inter-preyed in a limiting sense
The leasability of producing shaped articles such as puffins, corrugated plates pipes or garden articles in various forms prom hydrous suspensions comprising e.g. asbestos and cement by means of dehydrating machines, echoic mechanizer by means ox injection methods is generally known. Such articles were able to secure a dominant position among construction material during the past decennials In the course of the recent years it has increasingly become obvious that the most important raw material or the production of these products, namely asbestos, will soon no longer be available for such utilization due to various reasons, such as availability, ~3~7Q~
development of costs as well as due to health considerations.
It is not only the known excellent service properties of asbestos cement which are based on the unique combination of properties inherent in asbestos fires, said properties form additionally the basis of the Hatscheck-dehydrating methods which are known world wide All of the above circumstances have caused in the recent years an intensive research activity having as object the finding of replacement fires which can completely replace the as-bests in the known manufacturing processes of the dodder-tying methods. It has, however, been discovered extremely soon that not one kind of fires would be found which incorporated all positive properties of asbestos.
Following properties characterize asbestos as excellent pro-diction process as well as reinforcement fires:
- large specific surface - excellent dispersive power - outstanding chemical festivity - high concrete retention capability - excellent capability of forming nonwovens - high breaking strength high modulus of elasticity - small elongation at fracture Asbestos displays as process expedient means an excellent dispersive power in an hydraulic cement suspension. Due to its high filtration capability and its affinity to cement asbestos is in to position to retain the binding agent forming in the cement during the dehydrating process step, The high breaking strength combined with the high modulus of elasticity and the small elongation at fracture have a post-live effect on the hydrated final article which can bestow ~23~7Q3 the a~bestos-cement products the known high bending strength.
Because neither natural nor synthetical fires having the combination of properties of asbestos could be found, search efforts for finding possible replacement products lead to the realization that commensurate with the two main functions of asbestos mixtures of fires must be made use of in order to be able to carry out a production utilizing such new fires on existing machines and apparatuses (see e.g. DEEPS
30 02 484 of Amounts). The filtration properties of asbestos can be simulated in the fire mixtures by additions of cell-lose and/or synthetic fib rides. Regarding the reinforcing properties reinforcing fires are made use of. Such fires may be organic or inorganic high modulus flares which are added usually in a cut length of 4-12 millimeters.
There hardly exists a synthetic fire which has not been tested regarding such application as cement reinforcing cement. Most of these fires did, however, not succeed due to a large variety ox reasons, such as insufficient chemical resistivity, bad affinity to cement, unsatisfactory mechanical properties or due to the exceedingly high price. Among the entire available fires only two types of synthetic fires which meet the demands of a cement reinforcing fire were able to prevail. One of these fires has been developed on the basis of polyacrylnitrile and has been marketed for in-stance by the Hoechst Company (Western Germany under the trademark "Nolan 10"~ The other fiber is formed on -the basis of polyvinyl alcohol and is e.g. available from the Queerer C. Japan under the trademark "Kuralon" (DEEPS 28 50 337~. The most important properties of these fires are tabulated in table 1.
Table 1 Textllemechanical proper-ties of types of fires suitable as reinforcement of cement:
_ _ Type of fire breaking elongation modulus of strength at fracture elasticity cN/dtex % cN/dtex Polyacrylnitril, PAN (e.g. * 690 - 8,5 10 - 16 mint 130 "Nolan 10") Polyvinyl alcohol, PEA 10 - 15 5,5 - 15 min. 175 (ego "Kuralon~') l _ .
The comparison of -the textile-mechanical properties between the PVA-fibres and the PAN-fibres reveals that the PVA-fibres display -the better mechanical properties. If now fire cut-tongs having a length of 6 millimeters of both types are distributes in an hydraulic cement suspension and worked on a filter press to fire cement plates, the measured strength values of such plates reveal that the better properties of the fires can also bestow the final product with better strength properties (table 2).
Table 2 Strength properties of plates of fibre-cement, produced on a filter press, of port land cement and the high modulus fires on the basis of PEA and PAN.
_ .
fires bending energy of density absorption strength fracture of water wit,% N/mm2 kJ/m2 g/ccm fires __ 1,0 12,5 0,203 ~,982 15,0 1,5 14,7 0,457 19920 14,5 ' _ 16,0 0,701 1~851 15~7 fires 1,0 14,8 0,652 1,935 14,6 1,5 16,1 1,208 1,900 15,1 2,0 19,5 1,835 1,863 16,0 . ................................. .. _ .
Jo - * Trade mark ~3~7~3 Textile mechanical properties of the fires used.
_ Breaking Modulus of Elongation Titer strain elasticity at fracture cN/dtex cN/d-tex _ _ dtex PAN 7,5 150 11 to PEA 12 240 _ __ _ _ The energy of fracture incorporates an extremely important material technological property. It gives evidence of the brittleness or impact tensile strength, rest. of a product.
This can have such effect in a practical application that e.g.
when placing of roof covering plates having differing values of an energy of fracture, but identical bending strengths, some plates may break suddenly without prints when sub-jacketed to a loading by a roofer (brittleness), however, in the second case may take the loading up by a larger bending.
The analysis of the results reveals that in comparison with the PAN-fibres the PVA-fibres having the better textile-mechanical properties can not only bestow the fibre-cement plates with a higher bending strength, but that their energy of fracture is larger, too. In these tests, the energy of fracture is defined as the surface area under the strain-elon-gallon curve up to the point where the maximal bending strength is reached, i.e. the plate has ruptured (fig. 1).
By knowledge of the relationship between -the data of the fires and -the product proper-ties ox the fibre-cement plates resulting these from it would be an easy task to produce fire-cement products exposed to high demands regarding bending strength and energy of fracture exclusively by utilizing PEA-fires. However, -the high costs of PVA-fibres counteract this solution. Due -to the high costs of the raw material combined with an extremely intrinsic fire production process, the costs 7~33 of producing PVA-fibres are 50 - 100 % higher than those of PAN-fibres.
Considering additionally that the present prices of asbestos amount to a fraction only of the prices of synthetic fires it is quite obvious that a decisive importance must be given to the price of the fires to allow the production of market table fire cement products at all. Accordingly, it would be a highly desirable object for the fibre-cement industry to provide a fire having the properties of the PVA-fibres desk cried above which, however, is economically acceptable, i.e.
not substantially more expensive than the PAN-fibre.
According to the rules of mixtures for fire reinforced come pound construction materials it should be expected that in Gaze of reducing ire mixtures the strength properties or energy of rupture, rest. resulting in the reinforced material follow linearly and proportionally the mixing ratio (see "Fiber-Reinforced Cement Composites", Technical Report 51.067, The Concrete Society, Terminal House, Grosvenor Gardens, London 1973 and H. Crinkly "Fiber Reinforcement", Akademisk Foreleg, Copenhagen, 1964).
SUMMARY OF TOE INVENTION
Hence, it is an object of the invention to provide a fire no-enforcement mixture in which cheap PAN-fibres are substituted for a large amount of PVA-fibres without suffering a loss of the positive properties in the fibre-cement product.
A further object is to provide a mixture of fires for the production of fibre-reinforced concrete comprising PEA- and PAN-fibres and having as little as possible, at least, how-ever, 10 % PVA-fibres.
I
- pa -Therefore the present invention relates to a mixture of polyacrilnitrile and polyvinyl alcohol fires as reinforcing fires for materials setting after the molding thereof, specifically for hydraulically setting materials, said mixture of fires comprising about 50-90% polyacrilni-trite fires and about SUE polyvinylalcoho e .,~.
~3'~L'7(~'3 DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
I.. _ ..__ . . . ... . .. _ _ _ The mixtures of fires realized by the present invention will be explained now based on following testing examples made in the praxis.
Suitable fires for the production of the decrease-mixtures of PAN- with PVA-fibres are polyacrylnitrile fires having a high modulus, a modulus of elasticity of at least 130 cN/dtex, an elongation at fracture of maximal 16 % and a breaking strength of a-t least 6 cN/dtex~
Suitable polyvinyl alcohol fires are high modulus fires ha-vying following specifications:
Modulus of elasticity ox at least 175 cN/dtex, elongation at fracture of maximal 15 % and a breaking strength of at least 10 cN/dtex.
Both kinds of fires can be used with uniform titers or as mixtures of fires of differing titers. Preferred use is made of fires in the range of 0.5 - 5.0 dtex. The fires can be cut either to exact, uniform lengths or when be ground or mixed in various lengths, Preferred is the application of the PVA-fibres in lengths of 4 - 15 mm and the PAN-fibres in lengths of 2 - 12 mm.
The hollowing examples will disclose that it is specifically advantageous if the PVA-fibres used are larger than the ad-mixed fires by about 1/3.
Possible production methods for structural members or articles, in which the fire mixtures according to the invention are used are e.g. dehydrating method by sitting drum machines or fourdriniers, however also mono-extrusion machines, injection apparatuses or filter-presses.
~3~7~?3 Mixtures which are suitable for a production on above macho-noes comprise in a hydrous suspension apart of the inventive fire mixtures also a binding agent, such as e.g. cement and possibly additional fibrous materials having filtering pro-parties as well as a variety of filling materials or additives.
Suitable binding agents are hydraulic inorganic binding agents such as cement, gypsum earth alkaline silicates or earthalka-line ailments However, organic binding agents such as e.g.
synthetic resins may be used too. Suitable filling materials or additives are e.g. quartz sand, blast-furnace slag, fly ash, pu~zolane, mica, rock dust. Suitable auxiliary fires operative to retain the binding agents and additives on the screens may be cellulose fires in form of sulfate cellulose, wood shavings, thermomechanical pulp and/or synthetic fib rides on the basis of plastic materials, e.g. polyethylene. The retention capability can be improved additionally by the use of flocculation agents, e.g. on -the basis of polyacrylamides.
Products which can be produced with those mixtures on the de-hydrating machines are e.g. planar plates, corrugates plates or boards, tubes or shaped articles,e.g. garden articles.
The inventive PVA/PAN-fibre mixtures will now be explained based on a number of exemplar applications.
The tests were made on a sifting drum dehydrating machine of the Hatschek design.
The fibre-cement-suspensions were prepared in a separate put-per and comprised a solids content of 80 g/l and continuously pumped from the pulper into the material chamber of a Hatschek-machine.
Shortly before entering into the material chamber, a dosage of 200 Pam of a flocculation agent type polyacrylamide was added to 3 for improving the retention of the cement. On the machine plates of about 6 mm were produced by 2Z full notations of the pattern plate, which plates were pressed between oiled plates during 60 minutes in a staple press at a specific pressing pressure of 250 bar to a thickness of 4,8 mm. Of all variations unpressed specimens were produced and tested, too.
The setting of the fibre-cement plates proceeded in a wetting room of 100 % relative humidity at 20C. After the plates were additionally stored for 3 days submerged in water, the tests were made in a wet or damp, rest. condition.
by xtu s used For the production on filter press:
Port land cement (2800 Elaine) 100 parts fire mixtures 2.0 parts For the production according to the Hatschek method:
Port land cement (2800 Elaine) 100 parts Old waste paper (45 SO) 3.5 parts Polyethylenefibride ~"Pulpex"E~A, Hercules USA) 2.0 parts fire mixtures 2.0 parts Following variants were used as fire mixtures:
PAN 2 1,7 1,3 1~0 0,7 parts PEA 0 0,3 0.7 1,0 I 2,0 parts The textile-mechanical proper-ties of the fires were:
- PAN
Titer 1,5 dtex, breaking strength 7,2 cN/dtex, modulus of elasticity 140 cN/dtex, elongation at fracture 9 %
- PEA
Titer 2 dtex, breaking strength 12,5 cN/dtex, modulus of elasticity 250 oN/dtex, elongation at fracture 6,5 %
*Trade mark , "I., ;. -~3'~7~P3 PAN and PEA fires were used in a variety of combination of 4 and 6 mm cut lengths.
For the tests on the filter press mixtures were prepared in water which consisted only of Port land cement and the PVA/PAN-fires.
The test of the fire cement plates proceeded by aid of a Wolpert testing apparatus having a three-point bearing con-tact on plates of 25 x 25 mm. The bearing contact distance amounted to 167 mm and the test speed to 26 mm/min. The anal louses of the results were made by aid of a computer connected to the testing apparatus.
do Results The results are tabulated in the tables 3 to 7.
7~3 Table 3 Test results ox fire cement plates having variable PVA-PAN-fire rations, produced on a Ha-tschek-machine.
. ___ .
fire mixture bending energy of Density Absorption PAN PEA strength fracture of water 6 mm 6 mm parts parts N/mm2 kJ/m2 g/ccm %
_ press plates _ 2,0 22,4 3,047 1,941 12,3 0~3 1,7 21,1 2,799 1,934 11,4 0,7 1,3 21,8 2,884 1,943 10,9 1,0 1,0 20,7 2,698 1,928 12,0 1,3 0,7 21,3 2,532 1,919 11,9 1,7 0,3 19,0 2,105 1,932 12,4 2,0 - 1791 1,108 1,911 12,1 -- A. . Jo ._ ______ . ._ _ unpressed plates __ - 2,0 14,8 4,272 1,555 20,1 0,3 1,7 14,7 3,820 1,567 19,9 0,7 1,3 14,5 4,133 1,557 19,8 1,0 1,0 13,6 3,740 1,539 21,2 1,3 0,7 13,8 4,010 19500 23,7 1,7 0,3 13~1 3,205 1,532 20,8 2,0 - 12,4 1,902 1,514 21,9 ._ _.___ e_ _, ,_,, Table 4 Test results of fire cement plates having variable PAP
fire rations, produced on a filtering press.
_ .
fire mixture bending energy of density absorption PAN PEA strength rupture of water 6 mm 6 mm parts parts _ _ Kim g/ccm %
_ 2,0 14,2 2,603 1,753 19,9 0,3 1,7 14~4 2,512 1,758 19,8 0,7 1,3 13,9 2,543 1,752 1997 1,0 1,0 13,9 2,527 1,754 19,8 1,3 0,7 1397 2,410 1,732 19,9 1,7 0,3 13,1 1,700 1,748 19,6 2,0 - 12,2 0,9'75 1,731 19,8 . ___ . ... _ . _ ~347~3 Table 5 Test results of fire cement plates having variable - PVA-PAN-fibre rations, produced on a Hatschek-machine.
__ _ _ fire mixture bending energy of density absorption PUN PEA strength rupture of water6 mm 4 mm parts parts N/mm2 Kim g/ccm %
, _ _ _ _ . __ pressed plates _ 2,0 24,2 3,075 1,93512,6 0,3 1,7 23,1 2,418 199421176 0,7 1,3 20,4 1,990 1,91912,0 1,0 1,0 19,2 2,001 1,92011,6 193 0,7 18S9 1,820 1,92311,2 1~7 0,3 17,5 1,221 1,91711,8 2,0 - 17,1 1,108 1,91112,0 _ unpressed plates - 2,0 15,0 4,519 1,55022,6 0,3 1,7 14,7 4,059 1,54122,4 0,7 1,3 14,2 3,465 1,52821,9 1,0 1,0 13,4 2,968 1,53620,4 1,3 0,7 13,1 2~436 1,53220,4 197 0,3 12,7 2,150 1~52121,3 2,0 - 12,4 2,100 1,51421,9 . _ _ . _ SKYE
Table 6 Test results of fire cement plates having variable PVA-PAN fire rations, produced on a filtering press ire mixture bending energy of density absorption PAN PEA strength rupture of water 6mm 4 mm parts parts N/mm2 kJ/m2 g/ccm __ _ __ _ 2~0 14,8 2,429 1,807 18,7 0,3 1,7 15,3 2,510 1,823 17,7 0,7 1~3 14,0 2,010 1,779 18,6 1,0 1,0 13.5 1,619 1,785 18,2 1,3 0,7 12,9 1,327 1,761 18,8 1,7 0,3 1295 0,902 1,750 18,7 2,0 12,4 0,945 1,747 18,9 __ 7~3 Table 7 Fibre-cement plates produced in accordance with the invention and having materials PVA-PAN-ratios, produced on a Hatschek-machine.
.
fire mixture bending energy of density absorption PAN PEA strength rupture of water 4 mm 6 mm parts parts N/mm2 Kim g/ccm %
_ Do Do .
_ 2,0 22,6 3 9 331 1,938 12,2 0,3 1,7 22,8 3,115 1,933 12,1 0,7 1,3 22,1 ~101 1,941 11,0 1,0 1~0 22,0 2,987 1,9~1 11,5 1,3 0,7 21,3 2,605 1,929 12,3 1,7 I 18,2 1,980 1,937 12,0 2,0 - 15,3 0,972 1,941 11,1 unpressed plates _ 2,0 15,1 4,657 1,548 22,3 0,3 1,7 15,2 4,450 1,551 22,0 0,7 1,3 14,8 4,522 1,550 21,9 1,0 1,0 14~8 4,186 1,542 22,6 1,3 0,7 14,1 3,475 1,553 21,9 1,7 0,3 12,9 2,497 1,561 20,7 2,0 - 11,7 1,303 1,568 19,9 Textile-mechanical properties of the fires used in table 7.
Titer 3,0 dtex, breaking strength 7,3 cN/dtex modulus of elasticity 152 cN/dtex elongation at rupture 9,8 %
Titer 2,0 dtex, breaking strength 12,5 cN/dtex modulus of elasticity 250 cN/dtex elongation at rupture 6,5 I.
While there are shown and described a number of embodiments of the present invention, it shall be clearly understood that such are for sake of illustration only and not to be inter-preyed in a limiting sense
Claims (14)
1. A mixture of polyacrilnitrile and polyvinylalcohol fibres as reinforcing fibres for materials setting after the molding thereof, specifically for hydraulically setting ma-terials , said mixture of fibres comprising about 50-90 %
polyacrilnitride fibres and about 50-10 % polyvinylalcohol fibres.
polyacrilnitride fibres and about 50-10 % polyvinylalcohol fibres.
2. The mixture of claim 1,in which the PAN-fibres com-prise a modulus of elasticity of at least about 130 cN/dtex, a maximal elongation at rupture of about 16 % and a strength of at least about 6 cN/dtex.
3. The mixture of claim 1, in which the PVA-fibres com-prise a modulus of elasticity of at least about 175 cN/dtex, a maximal elongation at rupture of about 15 % and a strength of at least about 10 cN/dtex.
4. The mixture of claim 1, in which the used PVA- and PAN-fibres comprise titers in the range of about 0,5-10 dtex.
5. The mixture of claim 1, in which the length of the PAN-fibres is in the range of about 2 to 12 mm.
6. The mixture of claim 1, in which the length of the PVA-fibres is in the range of about 4 to 15 mm.
7. The mixture of claim 1, in which the preferred ratio of the cut length of the PVA- and PAN-fibres, respectively, amounts to about 4:3 to 3:2.
8. The mixture of claim 1, in which the reinforcing fibre mixture contains additives selected from the group cellulose fibres and/or synthetical pulp as process aids.
9. The mixture of claim 8, in which the reinforced fibre mixture contains additives selected from the group quartz sand, amorphous silicic acid, blast furnace slags, fly ashes, puzzolane, limestone and mica.
10. A method of reinforcing hydraulically setting mate-rials, in which a mixture of polyacrilnitrile and polyvinyl-alcohol fibres present in a ratio of about 50-90 % PAN-fibres and about 50-10 % PVA-fibres are added to such hydraulically setting materials selected from the group cement, gypsum, earth alkaline silinates, earth alkaline silicates, earth alkaline-aluminates.
11. The method of claim 10, in which a diluted, hydrous suspension is produced from said materials, which hydrous sus-pension is moulded into a desired shape and set thereafter for the production of fibre reinforces shaped articles, such as e.g. plates, corrugated plates and tubes.
12. A shaped article, e.g. plate, corrugated plate or tube, produced by utilization of a mixture of polyacril-nitrile and polyvinylalcohol fibres as reinforcing fibres for materials hydraulically setting after the molding thereof, said mixture comprising about 50-90 % polyacrilnitride fibres and about 50-10 % polyvinylalcohol fibres.
13. The shaped article of claim 12, in which said re-inforcing fibres are present in a ratio of about 1-5 %, of the reinforced mass.
14. The shaped article of claim 13 in which said rein-forcing fibres are present in a ratio of 1.5 to 2.5% of the reinforced mass.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH1017/84-0 | 1984-03-01 | ||
| CH1017/84A CH660357A5 (en) | 1984-03-01 | 1984-03-01 | MIXING CONTAINING FIBER FIBERS FOR THE REINFORCEMENT OF MATERIALS. |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1234703A true CA1234703A (en) | 1988-04-05 |
Family
ID=4200502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000475492A Expired CA1234703A (en) | 1984-03-01 | 1985-02-28 | Mixture of fibres for the reinforcement of construction materials, specifically for the reinforcement of hydraulic binding agents, a method of reinforcing construction materials, and formed articles of said mixture |
Country Status (19)
| Country | Link |
|---|---|
| EP (1) | EP0155520B1 (en) |
| JP (1) | JPS60204649A (en) |
| BR (1) | BR8500897A (en) |
| CA (1) | CA1234703A (en) |
| CH (1) | CH660357A5 (en) |
| DE (1) | DE3562221D1 (en) |
| DK (1) | DK160484C (en) |
| ES (1) | ES8606813A1 (en) |
| FI (1) | FI850772L (en) |
| GR (1) | GR850498B (en) |
| IE (1) | IE56925B1 (en) |
| IL (1) | IL74339A (en) |
| MA (1) | MA20360A1 (en) |
| NO (1) | NO850819L (en) |
| OA (1) | OA07959A (en) |
| PH (1) | PH23179A (en) |
| PT (1) | PT80039B (en) |
| TR (1) | TR23396A (en) |
| ZA (1) | ZA851524B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6269599B1 (en) | 1995-12-05 | 2001-08-07 | Josef Scherer | Construction component or construction with a composite structure, associated composite construction element, and method of production |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6296354A (en) * | 1985-10-21 | 1987-05-02 | 株式会社クラレ | Hydraulic inorganic papered product and manufacture |
| JPH07102995B2 (en) * | 1985-10-25 | 1995-11-08 | 住友化学工業株式会社 | Fiber-reinforced curable material and manufacturing method thereof |
| ATE78457T1 (en) * | 1988-10-13 | 1992-08-15 | Polyfibre Sa | FIBER-REINFORCED HYDRAULICALLY BONDED BUILDING MATERIAL AND PROCESS FOR ITS PRODUCTION. |
| DE4133895C2 (en) * | 1991-10-10 | 1994-03-24 | Maerkische Faser Ag | Multi-component system made of natural polymers and PAN moldings with asbestos-specific properties for use in hydraulic binders |
| JP3181375B2 (en) * | 1992-05-30 | 2001-07-03 | 株式会社豊夢 | Bonding tool, method for bonding structural members using the same, and bonding structure between structural members |
| FR2797868B1 (en) * | 1999-08-25 | 2002-02-01 | Schappe Sa | REINFORCING WIRE FOR CONCRETE AND CEMENT MORTARS |
| BR0107280A (en) * | 2001-09-17 | 2004-03-23 | Rhodia Poliamida Ltda | Microfibers for reinforcement of inorganic matrices, such as cement, mortar. plaster and concrete, polyamide-based microfibres for inorganic matrix reinforcement, process for obtaining polyamide-based microfibres for inorganic matrix reinforcement and fiber-cement products |
| FR2918390A1 (en) | 2007-07-05 | 2009-01-09 | Schappe Sa Sa | HYBRID WIRE FOR REINFORCING PLATES |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2128935A1 (en) * | 1970-06-12 | 1971-12-16 | Halliburton Co., Duncan, OkIa. (V.StA.) | High-strength cement bodies contng alkali-resistant fibre reinforcement |
| CH633503A5 (en) * | 1977-11-21 | 1982-12-15 | Inventa Ag | FIBER REINFORCED CEMENT-LIKE MATERIAL. |
| PT72082B (en) * | 1979-12-18 | 1981-10-13 | Amrotex Ag | PRODUCED BY HYDRAULIC BINDER AND / OR PLASTIC PRODUCT |
| AT370064B (en) * | 1980-04-21 | 1983-02-25 | Eternit Werke Hatschek L | BUILDING MATERIAL MIXING OF FIBER REINFORCED, PARTICULARLY CEMENTED PRODUCTS |
| JPS58185474A (en) * | 1982-04-22 | 1983-10-29 | 株式会社クラレ | Fiber reinforced hydraulic moldings |
| JPS60161362A (en) * | 1984-02-01 | 1985-08-23 | 株式会社クラレ | Fiber reinforced hydraulic inorganic paper product and manufacture |
-
1984
- 1984-03-01 CH CH1017/84A patent/CH660357A5/en not_active IP Right Cessation
-
1985
- 1985-02-13 IL IL74339A patent/IL74339A/en unknown
- 1985-02-20 EP EP85101830A patent/EP0155520B1/en not_active Expired
- 1985-02-20 DE DE8585101830T patent/DE3562221D1/en not_active Expired
- 1985-02-25 MA MA20584A patent/MA20360A1/en unknown
- 1985-02-25 PH PH31906A patent/PH23179A/en unknown
- 1985-02-26 FI FI850772A patent/FI850772L/en not_active Application Discontinuation
- 1985-02-27 TR TR8626/85A patent/TR23396A/en unknown
- 1985-02-27 GR GR850498A patent/GR850498B/el unknown
- 1985-02-28 CA CA000475492A patent/CA1234703A/en not_active Expired
- 1985-02-28 DK DK094585A patent/DK160484C/en not_active Application Discontinuation
- 1985-02-28 IE IE494/85A patent/IE56925B1/en not_active IP Right Cessation
- 1985-02-28 BR BR8500897A patent/BR8500897A/en unknown
- 1985-02-28 ZA ZA851524A patent/ZA851524B/en unknown
- 1985-02-28 NO NO850819A patent/NO850819L/en unknown
- 1985-03-01 ES ES540845A patent/ES8606813A1/en not_active Expired
- 1985-03-01 PT PT80039A patent/PT80039B/en unknown
- 1985-03-01 OA OA58533A patent/OA07959A/en unknown
- 1985-03-01 JP JP60039001A patent/JPS60204649A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6269599B1 (en) | 1995-12-05 | 2001-08-07 | Josef Scherer | Construction component or construction with a composite structure, associated composite construction element, and method of production |
Also Published As
| Publication number | Publication date |
|---|---|
| BR8500897A (en) | 1985-10-22 |
| PT80039A (en) | 1985-04-01 |
| DK94585D0 (en) | 1985-02-28 |
| CH660357A5 (en) | 1987-04-15 |
| GR850498B (en) | 1985-04-03 |
| JPS60204649A (en) | 1985-10-16 |
| IL74339A (en) | 1988-10-31 |
| ES540845A0 (en) | 1986-05-16 |
| ES8606813A1 (en) | 1986-05-16 |
| EP0155520B1 (en) | 1988-04-20 |
| EP0155520A1 (en) | 1985-09-25 |
| NO850819L (en) | 1985-09-02 |
| MA20360A1 (en) | 1985-10-01 |
| IE56925B1 (en) | 1992-01-29 |
| FI850772L (en) | 1985-09-02 |
| PT80039B (en) | 1986-11-20 |
| DK94585A (en) | 1985-09-02 |
| DE3562221D1 (en) | 1988-05-26 |
| IL74339A0 (en) | 1985-05-31 |
| ZA851524B (en) | 1985-10-30 |
| FI850772A0 (en) | 1985-02-26 |
| OA07959A (en) | 1987-01-31 |
| IE850494L (en) | 1985-09-01 |
| PH23179A (en) | 1989-05-19 |
| TR23396A (en) | 1989-12-29 |
| DK160484B (en) | 1991-03-18 |
| DK160484C (en) | 1991-08-26 |
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