EP0079014B1 - Matériau à couches multiples, procédé de fabrication et son utilisation - Google Patents

Matériau à couches multiples, procédé de fabrication et son utilisation Download PDF

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Publication number
EP0079014B1
EP0079014B1 EP82110033A EP82110033A EP0079014B1 EP 0079014 B1 EP0079014 B1 EP 0079014B1 EP 82110033 A EP82110033 A EP 82110033A EP 82110033 A EP82110033 A EP 82110033A EP 0079014 B1 EP0079014 B1 EP 0079014B1
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EP
European Patent Office
Prior art keywords
unsaturated polyester
polyester resin
weight
film
elastically modified
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP82110033A
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German (de)
English (en)
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EP0079014A1 (fr
Inventor
Heinz B. Dr.Rer.Nat. Dipl.-Chem. Kemper
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kunststoff- and Lackfabrik Kemper
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Kunststoff- and Lackfabrik Kemper
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Publication date
Application filed by Kunststoff- and Lackfabrik Kemper filed Critical Kunststoff- and Lackfabrik Kemper
Priority to AT82110033T priority Critical patent/ATE18448T1/de
Publication of EP0079014A1 publication Critical patent/EP0079014A1/fr
Application granted granted Critical
Publication of EP0079014B1 publication Critical patent/EP0079014B1/fr
Expired legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06N3/06—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with polyvinylchloride or its copolymerisation products

Definitions

  • the invention relates to a composite material, process for its production and its use.
  • polyester resins are prepared by reacting a mixture of a polyester obtained by polycondensing saturated and unsaturated polycarboxylic acids with polyols and a free isocyanate group-containing prepolymer obtained by addition reaction of a compound containing hydroxyl groups to a polyisocyanate in the presence of styrene and catalysts. In this process, the polyester is condensed such that the acid number is below 20 mg KOH / g.
  • the elastically modified polyester resins obtained can be used as coating compositions for sealing flat roofs, patios and balconies. It has also been shown to be advantageous to use these elastic, modified polyester resins as coating compositions in conjunction with nonwovens made of synthetic fibers for sealing flat roofs, patios and balconies.
  • the elastically modified polyester resins Due to their content of unsaturated dicarboxylic acids, the elastically modified polyester resins belong to the so-called unsaturated polyester resins. These unsaturated polyester resins have a low water vapor diffusion resistance number ⁇ of 5,000 to 6,000. With a layer thickness d of 2 mm, this results in a value of 10-12000, ie a large permeability to water vapor, by multiplying the water vapor diffusion resistance number kt by the layer thickness d. For this reason, it is possible to apply the elastically modified polyester resins fully adhering to a substrate, such as roofs, patios and balconies.
  • polyester resins Another advantage of such polyester resins is that they retain their elasticity at temperatures below 0 ° C and that they remain elastic at temperatures of - 35 ° C.
  • the present invention was therefore based on the object of providing a suitable composite material which adheres to the entire surface of a substrate, has a low water vapor diffusion resistance number with a layer thickness of up to approximately 3 mm and can also be processed at elevated temperatures to form a completely hardened surface layer, thus prevents evaporation of the monomer contained in the unsaturated polyester resin and prevents the entry of atmospheric oxygen.
  • the invention thus relates to a composite material consisting of a film of chlorinated polyethylene elastomers with a content of 36 to 48 percent by weight of chlorine, a random fiber fleece and elastically modified, unsaturated polyester resins on the surface of a substrate.
  • Films made of chlorinated polyethylene elastomers with a chlorine content of 36 to 48 percent by weight, which can be used as sealing sheets, are known per se. They can be applied with or without reinforcement in the form of a woven, knitted or laid fabric in layer thicknesses of 1.2 to 1.5 mm for loose laying or also partial gluing on substrates as a seal.
  • full-surface gluing is not possible because the relatively large impermeability to water vapor leads to the formation of bubbles.
  • the water vapor diffusion resistance number ⁇ of such chlorinated polyethylene elastomers is 50,000. With a layer thickness d of 1.5 mm, this results in a value of 75,000 by multiplying the water vapor diffusion resistance number ⁇ by the layer thickness d.
  • thinner films made of chlorinated polyethylene elastomers which have a thickness of 0.2 to 3 mm, preferably 0.2 to 3 mm, can be used by this measure 1 mm; because previously it was necessary for mechanical reasons to use such films in a layer thickness of at least 1.2 mm.
  • the use of elastically modified, unsaturated polyester resins as an intermediate layer between the film made of chlorinated polyethylene elastomers and the substrate not only achieves full-surface adhesion of the film made of chlorinated polyethylene elastomers to the substrate, but also adjustable water vapor permeability up to water vapor impermeability.
  • the composite materials according to the present invention can also be used at higher temperatures without the need to use skin-forming substances such as paraffins and stearins.
  • the films made of chlorinated polyethylene elastomers also prevent evaporation of the monomers contained in the elastically modified, unsaturated polyester resin, in particular styrene, so that the polyester and the prepolymer can crosslink with the monomers to form the polyester resin.
  • the chlorinated polyethylene elastomer film also prevents the ingress of atmospheric oxygen.
  • the high extensibility and tensile strength of the composite material according to the present invention made of a film made of chlorinated polyethylene elastomers, a random fiber fleece and an elastically modified, unsaturated polyester resin is particularly advantageous.
  • the tensile strength is surprisingly much higher than can be achieved with the known elastically modified, unsaturated polyester resins as seals.
  • the films of chlorinated polyethylene elastomers to be used as the top layer in the composite materials of the present invention with a chlorine content of 36 to 48 percent by weight are known per se.
  • aqueous slurries of high density polyethylenes By chlorinating aqueous slurries of high density polyethylenes, amorphous powders with molecular weights between 10 5 and 10 6 g / mol are obtained. The density is 1.16 to 1.32 g / cm 3 .
  • the commercially available chlorinated polyethylene elastomers are free-flowing powders with grain sizes between 300 and 500 J.Lm and after the addition of 5 to 10% stabilizers, lubricants, chlorine acceptors, UV stabilizers, dyes or pigments and / or vulcanizing agents, on conventional Rubber processing machines processed into foils.
  • Films with a thickness of at least 0.2 mm are used to produce the composite materials according to the present invention.
  • the film thickness in particular in the case of composite materials which are permeable to water vapor, is preferably 0.2 to 1 mm and in the case of composite materials which are impervious to water vapor, preferably 1 to 3 mm.
  • Woven fabrics, knitted fabrics or scrims made of natural, semisynthetic and / or synthetic fibers are suitable for reinforcing the chlorinated polyethylene elastomers, with fibers made of polyester and glass being preferred.
  • the random fiber nonwovens used in the composite materials of the present invention can be formed from staple fibers or continuous threads, which are also needled and / or are thermally and / or connected to one another at individual crossing points of the fibers or threads by an adhesive.
  • the random fiber fleeces have a weight of 80 to 250 g / m 2 .
  • the elastically modified unsaturated polyester resins used for the composite materials according to the present invention are also known per se. Commercially available unsaturated polyester resins are suitable which have been elastically modified by the addition of low-temperature plasticizers. The use of such unsaturated polyester resins mixed with cold-resistant plasticizers is suitable when the substrates on which they contain plasticizers. Unsaturated polyester resins are applied, do not allow or favor plasticizer migration.
  • polyester resins When using the commercially available unsaturated polyester resins, preference is given to an unsaturated polyester based on phthalic acid, adipic acid and neopentyl glycol, the acid number of which is approximately 15 to 19 mg KOH / g. Such polyesters are relatively elastic and also resistant to hydrolysis. These polyesters are dissolved in styrene so that the proportion is 33 to 37 percent by weight of styrene.
  • plasticizers for example based on dialkyl esters of phthalic acid, adipic acid and / or sebacic acid, chlorinated paraffins, vinyl acetate / ethylene copolymers or phosphates such as diphenyl-cresyl phosphate, or mixtures of these plasticizers desired elasticization achieved.
  • An additional improvement in fire behavior can be achieved by adding antimony trioxide, bromine or chlorine additives. which can be added in addition to fillers and dyes and thixotropic agents in customary amounts.
  • plasticizer-free, elastically modified, unsaturated polyester resins are particularly advantageous.
  • Such elastically modified, unsaturated polyester resins are prepared by using a mixture of 70 to 80 percent by weight of saturated dicarboxylic acids, such as adipic acid and / or sebacic acid, and 30 to 20 percent by weight of unsaturated dicarboxylic acids, such as maleic acid, fumaric acid, phthalic acid and / or terephthalic acid a glycol with at least 5 carbon atoms, such as neopentyl glycol, is condensed to form a polyester such that the acid number is below 20 mg KOH / g. The polyester obtained is then mixed with styrene.
  • a free hydroxyl-containing polyester for example based on adipic acid, 1,3-butylene glycol and 1,2,4-hexanetriol with a hydroxyl number of 6.5 percent
  • polyether for example adducts of ethylene oxide and / or propylene oxide with polyhydric alcohols, such as 1,2,4-hexanetriol, and
  • Catalysts known per se such as peroxides, for example benzoyl peroxide or cyclohexanone peroxide, accelerators, such as amines, for example dimethylaniline or cobalt naphthenate or octoate, furthermore dyes, pigments, such as titanium dioxide, iron oxide black or chromium oxide green, and further fillers are added to the mixture obtained , such as aluminum hydroxides, and / or thixotropic agents, such as finely divided silica.
  • accelerators such as amines, for example dimethylaniline or cobalt naphthenate or octoate
  • dyes, pigments such as titanium dioxide, iron oxide black or chromium oxide green
  • further fillers are added to the mixture obtained , such as aluminum hydroxides, and / or thixotropic agents, such as finely divided silica.
  • the styrene which is also used serves as a further crosslinking agent in addition to the prepolymer which already serves as a crosslinking agent and has free isocyanate groups. It has proven to be very advantageous if the styrene added is stabilized in order to achieve a storage stability of the substances.
  • the total amount of styrene added is preferably 30 to 50 percent by weight, based on the other resin components.
  • random fiber fleece which serves as a reinforcing insert, and depending on the basis weight of the random fiber fleece, it is up to you to influence the thickness, the elasticity and the tensile strength of the composite material.
  • the lamination according to b) and d) can be carried out in such a way that the random fiber fleece is thermally bonded to the chlorinated polyethylene elastomer film, for example by bringing the two webs together in a calender that is heated to elevated temperatures, for example 150 to 250 ° C. is heated. You can also glue the two sheets together.
  • An 8 to 10 percent solution of chlorinated polyethylene with a Chlorine content of 42 percent by weight in ketones and / or aromatic hydrocarbons has proven to be particularly advantageous. Mixtures of methyl isobutyl ketone and xylene or of cyclohexanone and xylene are particularly preferred as solvents.
  • the curing time of the liquid, elastically modified, unsaturated polyester resin is about 2 to 60 minutes, depending on the catalyst and / or accelerator used.
  • the adhesion of the elastically modified, unsaturated polyester resin is over the entire surface both on the substrate and on the film made of chlorinated polyethylene elastomers.
  • the tensile strength of the coating made of the chlorinated polyethylene elastomer film and the polyester resins applied to the substrate is always higher than the maximum adhesion to the substrate. This has the advantage that when the seal is stretched, for example by so-called working of a building (enlarging joints, cracks and / or cavities), the applied composite film compensates for expansion and does not tear.
  • the expansion compensation can also result from a partial detachment of the composite film from the substrate surface.
  • Another object of the present invention is the use of the composite materials on buildings, components and landfills. These are primarily roofs, especially flat roofs, patios and balconies. Furthermore, the composite materials can also be attached to vertical surfaces, such as walls, a film of chlorinated polyethylene elastomers, which may be reinforced by woven, knitted or scrim, covered with the random fiber fleece and with the liquid, elastically modified, unsaturated polyester resin from the fleece side and the tangled fiber fleece is soaked and then placed on the vertical surface like a wallpaper and the polyester resin is cured. In this way, it is also possible to achieve seals in civil engineering and bridge construction and in landfills, especially chemicals, and pits. The method according to d) has proven to be particularly advantageous for sealing landfills and pits.
  • the composite film is laid out at the application site, then partially, in particular at the edges or at an edge on the top of the film made of chlorinated polyethylene elastomers, provided with the liquid, elastically modified, unsaturated polyester resin, and then another overlapping composite film. with the hardened polyester resin layer placed on the liquid polyester resin layer and allowed to harden the liquid polyester resin.
  • a layer of liquid, elastically modified, unsaturated polyester resin in styrene is applied to a flat roof.
  • a random fiber fleece made of polyester fibers with a basis weight of 150 g / m 2 is placed thereon. This random fiber fleece is then impregnated with a further amount of the liquid, elastically modified, unsaturated polyester resin in styrene.
  • a film of chlorinated polyethylene elastomer with a chlorine content of 35 to 36 percent by weight and a thickness of 0.2 mm is then placed on and the polyester resin is allowed to harden.
  • the liquid, elastically modified, unsaturated polyester resin is obtained which, before being applied to the substrate (flat roof), with 4% by weight of benzoyl peroxide (50%) and 3 percent by weight of dimethyl-p-toluidine (10 percent in styrene) is added.
  • a layer of the polyester resin described in Example 1 is applied to a film of chlorinated polyethylene elastomers in a thickness of 0.2 mm and with a chlorine content of 35 to 36 percent by weight of chlorine.
  • a random fiber fleece made of polyester fibers with a weight per unit area of 150 g / m 2 is placed thereon and impregnated with further liquid polyester resin.
  • the thickness of the polyester resin layer after curing is 2.0 mm.
  • a composite film is obtained.
  • the composite film is designed in suitable dimensions and a 10 percent solution of chlorinated polyethylene with a chlorine content of 42 percent in a mixture of cyclohexanone and xylene is applied to an edge on the top of the chlorinated polyethylene elastomer film.
  • Another laminated film is overlapped on the coated edge in such a way that the polyester resin layer lies on the coated edge. In this way, pits or landfills can be lined.
  • Example 2 The procedure of Example 2 is repeated with the proviso that a film made of chlorinated polyethylene elastomers is used in a thickness of 2 mm. As stated in Example 2, the K - d value of the composite film is determined. It is 112,000.
  • k t - d values over 100,000 are considered water vapor tight.
  • Such a composite is suitable as a seal in civil engineering and bridge construction, with a firmly adhering composite being produced on the structure, as indicated in Example 1.
  • a very high tear resistance is achieved.
  • the elasticity is also so high that cracking is avoided.
  • FIG. 1 a cross section through a composite material according to the present invention is shown in a schematic view.
  • a film 1 made of chlorinated polyethylene elastomers is applied to a substrate 4 by means of a layer 2 of elastically modified, unsaturated polyester resin, in which a random fiber fleece 3 is embedded.
  • Such a composite material is produced after the method execution a).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Laminated Bodies (AREA)
  • Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)

Claims (12)

1. Matériau à couches multiples, constitué d'une feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore, d'une nappe de fibres entremêlées et de résines de polyester insaturées, élastiquement modifiées, sur la surface d'un substrat.
2. Matériau à couches multiples suivant la revendication 1, caractérisé en ce que la feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore a une épaisseur de 0,2 à 3 mm.
3. Matériau à couches multiples suivant l'une des revendications 1 et 2, caractérisé en ce que la feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore a une épaisseur de 0,2 à 1 mm.
4. Matériau à couches multiples suivant au moins l'une des revendications 1 à 3, caractérisé en ce que la feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore est renforcée par une matière tissée, tricotée ou appliquée.
5. Matériau à couches multiples suivant au moins une des revendications 1 à 4, caractérisé en ce que la nappe de fibres entremêlées est constituée de fibres de polyester.
6. Matériau à couches multiples suivant au moins une des revendications 1 à 5, caractérisé en ce que la nappe de fibres entremêlées est aiguilletée.
7. Matériau à couches multiples suivant au moins une des revendications 1 à 6, caractérisé en ce que les fibres de la nappe de fibres entremêlées sont reliées de manière fixe en certains points de croisement.
8. Matériau à couches multiples suivant au moins une des revendications 1 à 7, caractérisé en ce que la nappe de fibres entremêlées présente un poids de 80 à 250 g/m2.
9. Matériau à couches multiples suivant au moins une des revendications 1 à 8, caractérisé en ce que la résine de polyester insaturée, élastiquement modifiée, est préparée par réaction d'un mélange
a) d'un polyester insaturé présentant un indice d'acide inférieur à 20 mg de KOH/g, qui a été obtenu par condensation d'un mélange de 70 à 80 % en poids d'acides dicarboxyliques saturés et de 30 à 20 % en poids d'acides dicarboxyliques insaturés avec un glycol comprenant au moins 5 atomes de carbone, et de styrène, et
b) d'une solution dans du styrène d'un pré- polymère qui présente des groupes isocyanate libres et qui a été obtenu par une réaction d'addition d'un polyisocyanate et d'un polyéther et/ou d'un polyester présentant des groupes hydroxyle libres.
10. Procédé de préparation du matériau à couches multiples suivant les revendications 1 à 9, caractérisé en ce que
a) sur une surface de substrat on applique à l'état fluide une résine de polyester insaturée, élastiquement modifiée, conjointement avec un catalyseur, un accélérateur et/ou d'autres additifs courants, on introduit une nappe de fibres entremêlées sur ou respectivement dans la résine de polyester insaturée, élastiquement modifiée, fluide, on pose dessus une feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore et on laisse durcir la résine de polyester insaturée, élastiquement modifiée, ou
b) on double une feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore par une nappe de fibres entremêlées, on imprègne la feuille doublée, du côté nappe, par une résine de polyester insaturée, élastiquement modifiée, à l'état fluide, conjointement avec un catalyseur, un accélérateur et/ou des additifs courants, on pourvoit éventuellement également la surface de substrat de résines de polyester insaturées, élastiquement modifiées, à l'état fluide, conjointement avec un catalyseur, un accélérateur et/ou d'autres additifs courants, on place la feuille doublée et imprégnée par la résine de polyester insaturée, élastiquement modifiée, fluide, avec le côté nappe sur la surface du substrat pourvue de résine de polyester insaturée, élastiquement modifiée et on laisse durcir la résine de polyester insaturée, élastiquement modifiée, ou
c) on combine les modes opératoires a) et b) de telle sorte qu'une feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore, qui est doublée par une nappe de fibres entremêlées, est posée, après l'imprégnation de la nappe de fibres entremêlées, sur une surface de substrat pourvue d'une couche de résine de polyester insaturée, élastiquement modifiée, renforcée par une nappe de fibres entremêlées, et ensuite la résine de polyester insaturée, élastiquement modifiée, est durcie, la somme des poids par unité de surface des deux nappes de fibres entremêlées étant de 80 à 250 g/m2, ou
d) on double une feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore, comme indiqué sous b), d'une nappe de fibres entremêlées et on l'imprègne avec une résine de polyester insaturée, élastiquement modifiée, fluide, et on laisse durcir la résine de polyester insaturée, élastiquement modifiée, on entrepose éventuellement la feuille à couches multiples obtenue et ensuite, d'une manière décalée dans le temps, on l'applique sur une surface de substrat au moins partiellement pourvue de résine de polyester insaturée, élastiquement modifiée, à l'état fluide, la couche de résine de polyester insaturée, élastiquement modifiée, fluide, présentant éventuellement un renforcement sous la forme d'une nappe de fibres entremêlées, et on laisse durcir la résine de polyester insaturée, élastiquement modifiée.
11. Utilisation des matériaux à couches multiples suivant les revendications 1 à 9 comme revêtements de surface de constructions, d'éléments préfabriqués et dans le cas de décharges pour déchets.
12. Feuille à couches multiples constituée d'une feuille en élastomères de polyéthylène chlorés présentant une teneur de 36 à 48 % en poids de chlore, d'une nappe de fibres entremêlées et de résines de polyester insaturées, élastiquement modifiées.
EP82110033A 1981-11-02 1982-10-29 Matériau à couches multiples, procédé de fabrication et son utilisation Expired EP0079014B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82110033T ATE18448T1 (de) 1981-11-02 1982-10-29 Verbundmaterial, verfahren zu seiner herstellung und seine verwendung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19813143414 DE3143414A1 (de) 1981-11-02 1981-11-02 Verbundmaterial, verfahren zu seiner herstellung und seine verwendung
DE3143414 1981-11-02

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EP0079014A1 EP0079014A1 (fr) 1983-05-18
EP0079014B1 true EP0079014B1 (fr) 1986-03-05

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AT (1) ATE18448T1 (fr)
DE (2) DE3143414A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4437498A1 (de) 1994-10-20 1996-04-25 Basf Ag Emissionsarmes Beschichtungssystem
JPH1022244A (ja) * 1996-06-29 1998-01-23 Komatsu Electron Metals Co Ltd 半導体ウェハの洗浄用バスケット

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3302362A (en) * 1963-12-10 1967-02-07 Keith M Lang Method for forming roof structure
GB1059469A (en) * 1964-07-17 1967-02-22 Ruberoid Co Ltd Waterproof material
GB1251494A (fr) * 1967-11-16 1971-10-27
GB1271233A (en) * 1968-04-17 1972-04-19 Permanite Ltd Thermoplastic sheet material
DE2213939A1 (de) * 1972-03-22 1973-09-27 Erich Ehmann Dachbedeckung fuer warmflachdaecher
FR2336527A1 (fr) * 1975-12-23 1977-07-22 Gall Jean Yves K Dispositif de revetement etanche, notamment pour terrasses, et son procede de fabrication

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DE3143414A1 (de) 1983-05-11
DE3269683D1 (en) 1986-04-10
ATE18448T1 (de) 1986-03-15
EP0079014A1 (fr) 1983-05-18

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