WO2000069551A1 - Multi-component adhesive and gluing device, used with a multi-component adhesive of this type - Google Patents

Multi-component adhesive and gluing device, used with a multi-component adhesive of this type Download PDF

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Publication number
WO2000069551A1
WO2000069551A1 PCT/EP2000/004131 EP0004131W WO0069551A1 WO 2000069551 A1 WO2000069551 A1 WO 2000069551A1 EP 0004131 W EP0004131 W EP 0004131W WO 0069551 A1 WO0069551 A1 WO 0069551A1
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WO
WIPO (PCT)
Prior art keywords
component adhesive
carbon dioxide
liquid
solvent
components
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Application number
PCT/EP2000/004131
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German (de)
French (fr)
Inventor
Oliver Muth
Thomas Hirth
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Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
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Publication of WO2000069551A1 publication Critical patent/WO2000069551A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/008—Processes carried out under supercritical conditions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/34—Applying different liquids or other fluent materials simultaneously
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/0838—Manufacture of polymers in the presence of non-reactive compounds
    • C08G18/0842—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents
    • C08G18/0847—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of solvents for the polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C11/00—Component parts, details or accessories not specifically provided for in groups B05C1/00 - B05C9/00
    • B05C11/10—Storage, supply or control of liquid or other fluent material; Recovery of excess liquid or other fluent material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
    • B05D2401/90—Form of the coating product, e.g. solution, water dispersion, powders or the like at least one component of the composition being in supercritical state or close to supercritical state
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Definitions

  • Multi-component adhesive and device for gluing with such a multi-component adhesive are Multi-component adhesive and device for gluing with such a multi-component adhesive
  • the invention relates to a multicomponent adhesive with at least two reactive mono-, di-, oligo- or polymer components, at least one of which is dissolved in at least one solvent, and a device for gluing with such a multicomponent.
  • Multi-component adhesives are known in particular in the form of two-component adhesives.
  • they consist of reactive mono-, di- or oligomers, and on the other hand, hardeners, which are each stored as separate components and are mixed immediately before use.
  • two-component adhesives consisting of mixtures of polymerizable components and inactive hardeners are known, the hardeners being used immediately before use, e.g. through thermal energy. While the reactive mono-, di- or oligomers are mostly liquid or dissolved in an organic solvent, the hardeners are often in solid form, e.g. particulate.
  • BESXti ⁇ increase and in particular to be able to completely wet large parts to be joined, either one component, both components or - in the case of a multi-component adhesive having more than two components - all components are added to organic components before mixing, or an organic solvent and the respective components are introduced of the adhesive mixed into this.
  • the disadvantage here is that the liquid, often toxic and flammable organic solvents pose an increased environmental and safety risk, on the other hand they delay the curing time of the adhesive, since they evaporate only slowly and the final strength of the adhesive is only achieved after the solvents have completely evaporated .
  • the invention has for its object to provide a multi-component adhesive of the type mentioned, which makes the use of liquid, organic, often toxic and flammable solvents unnecessary and also has shorter curing times with increased adhesiveness. It is also directed to a device for gluing with such a multi-component adhesive.
  • the first part of this object is achieved according to the invention with a multi-component adhesive of the type mentioned at the outset in that the solvent is liquid or supercritical carbon dioxide (C0 2 ).
  • Supercritical C0 2 is used for example for the extraction of solids (SFE, supercritical fluid extraction).
  • SFE supercritical fluid extraction
  • DE 44 06 899 AI describes a method for decontamination of soils that are contaminated with military pollutants, such as explosives. Substances, propellant powders, rocket solid propellants, pyrotechnic charges or liquid propellants are contaminated, the pollutants with supercritical CC> 2 as a solvent, optionally mixed with organic solvents, extracted from the soil and then chemically decomposed.
  • Supercritical CO 2 is also used as a matrix liquid for carrying out chemical reactions, for example for carrying out polymerizations (DE 36 09 829 AI, US 5,663,237).
  • the known methods have so far not been able to give the experts any suggestions for solving the problem on which the invention is based.
  • supercritical carbon dioxide as an inert solvent in a multi-component adhesive makes it possible to completely dispense with conventional liquid solvents, which are often toxic and / or flammable.
  • the critical point of carbon dioxide is around 31 ° C and 73 bar.
  • Supercritical carbon dioxide is chemically inert, toxicologically harmless and can be separated spontaneously by transferring it to the subcritical area in which it is converted into gas.
  • Carbon dioxide has very good solvent properties in a compressed and in particular in a supercritical state, the solvent properties being obtained by varying the parameters
  • Temperature and pressure are controllable. Furthermore, it lowers the viscosity of the reaction components or the mixture of the reaction components and thus enables the bonding of parts to be joined in areas which are difficult to access, for example the bonding of large areas
  • the multi-component adhesive Due to the spontaneous volatilization of carbon dioxide in the subcritical state, for example under normal conditions, the multi-component adhesive has short curing times, which is solely due to the reaction time of the reactive components is determined. In addition, carbon dioxide inhibits the chemical reaction of the components - that is, the polymerization or crosslinking of the reactive components - so that a premix of the components can be stored for a long time. Due to the reaction-inhibiting effect of compressed or supercritical carbon dioxide, the processing times of the multi-component adhesive can be controlled, for example, by varying the concentration of the mixture of the polymer components in the carbon dioxide. Depending on the temperature, pressure and amount of compressed or supercritical carbon dioxide, thin or foam-like adhesive layers can be produced.
  • modifiers can be added to the C0 2 , with small amounts of organic solvents, for example acetone, alcohols or the like, generally being used as modifiers. , be used.
  • the multicomponent adhesive can consist of two or more reactive mono-, di-, oligo- or polymer components.
  • the reactive mono-, di-, oligo- or polymer components are polyadditive prepolymers and hardeners.
  • the prepolymers can, for example, also be epoxides with at least two epoxy groups and the hardeners amines with at least two amino groups.
  • a device for gluing with such a multicomponent adhesive is characterized in that it has at least two containers for holding the reactive mono-, di-, oligo- or polymer components, of which at least one can be pressurized with C0 2 and has a metering device connected to both containers. If premixing of the reactive components with compressed or supercritical carbon dioxide is desired, both containers of the device are designed to be pressurized with CO 2 .
  • a preferred embodiment provides that at least the container which can be pressurized with C0 2 is heated.
  • the pressurized container has an agitator in order to produce a homogeneous solution of the respective component in the compressed or supercritical carbon dioxide.
  • the metering device for example in the form of a nozzle, is also preferably heatable.
  • a preferred embodiment provides that between the containers and the metering device a pressurized, preferably heatable and a stirrer mixing chamber is arranged to vary the parameters pressure, temperature and concentration of the mixture of the components in the compressed or supercritical carbon dioxide, the adhesion properties, adjust the viscosity and the processing time or the possible storage time of the already mixed multi-component adhesive in the mixing chamber without it curing there.
  • a mixture of polyadditive prepolymers in the form of polyols (component 1) and hardeners in the form of di- and triisocyanates (component 2) is in an autoclave with a stirring device with a device for measuring the torque at constant temperature with compressed, liquid or supercritical carbon dioxide acted upon.
  • the reduction in the viscosity of the reaction mixture is evident after a short mixing time in a reduction in the torque of the stirring device.
  • the reaction mixture is applied to the joining surface by a metering device and cured.
  • the device according to the invention is explained in more detail below with reference to the drawing, which shows a schematic representation of an embodiment of a device for gluing with a two-component adhesive.
  • the device shown has two containers la, lb for receiving the reactive mono-, di-, oligo or polymer components, of which the container la is heated and via valves 5, 11 by means of a pump 12, for.
  • B. a diaphragm pump can be pressurized with compressed or liquid or supercritical carbon dioxide.
  • the carbon dioxide is stored in a storage container 13. While the container la z.
  • B. Contains prepolymers in the form of polyols are in the container 2b z.
  • the container 1 a has an agitator 6.
  • the components stored in the containers la, lb are via a valve 8 or via a valve 9 and a z. B. designed as a syringe, piston pump or the like pump 14 in a heatable mixing chamber 4.
  • the mixing chamber 4 the reaction mixture containing polyols, isocyanates and liquid or supercritical carbon dioxide is homogenized by means of an agitator 7.
  • the mixing chamber 4 can be supplied with liquid or supercritical carbon dioxide via the valves 5, 8, 11 by means of the pump 12. Alternatively or additionally, the mixing chamber 4 can in turn have a valve (not shown) for direct application of liquid or supercritical carbon dioxide.
  • a metering device 2 in the form of a heatable nozzle 3 connects to the mixing chamber 4 via a valve 10.
  • the valves 5, 8, 9, 10, 11 are designed in particular as high-pressure valves.
  • the mixing chamber 1b can also be pressurized or heated with carbon dioxide via a valve (not shown) and in this case the premixes stored in the containers 1a, 1b can also be mixed and metered directly in the metering device via valves.

Abstract

The invention relates to a multi-component adhesive, containing at least two reactive monomer, dimer, oligomer or polymer components. At least one of said components is dissolved in at least one solvent, whereby the solvent is liquid or supercritical carbon dioxide (CO2). Liquid, often toxic and flammable organic solvents can be substituted by using compressed, liquid or supercritical CO2. The dispersion properties of the liquid or supercritical CO2 can be controlled by varying the pressure and temperature parameters and the adhesive is thus easier to dose. The invention also relates to a gluing device which is used with a multi-component adhesive of this type.

Description

Mehrkomponentenkleber und Vorrichtung zum Kleben mit einem solchen MehrkomponentenkleberMulti-component adhesive and device for gluing with such a multi-component adhesive
Die Erfindung betrifft einen Mehrkomponentenkleber mit wenigstens zwei reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten, von denen wenigstens eine in wenig- stens einem Lösungsmittel gelöst ist, und eine Vorrichtung zum Kleben mit einem solchen Mehrkomponenten.The invention relates to a multicomponent adhesive with at least two reactive mono-, di-, oligo- or polymer components, at least one of which is dissolved in at least one solvent, and a device for gluing with such a multicomponent.
Mehrkomponentenkleber sind insbesondere in Form von Zweikomponentenklebern bekannt. Sie bestehen einerseits aus reaktiven Mono-, Di- oder Oligomeren, andererseits aus Härtern, die jeweils als separate Komponenten bevorratet sind und unmittelbar vor der Benutzung gemischt werden. Ferner sind aus Mischungen von polymerisierbaren Komponenten und inaktiven Härtern bestehende Zweikompo- nentenkleber bekannt, wobei die Härter unmittelbar vor der Benutzung, z.B. durch Wärmeenergie, aktiviert werden. Während die reaktiven Mono-, Di- oder Oligomere meist flüssig oder in einem organischen Lösungsmittel gelöst sind, liegen die Härter häufig in fester Form, z.B. partikelförmig vor.Multi-component adhesives are known in particular in the form of two-component adhesives. On the one hand, they consist of reactive mono-, di- or oligomers, and on the other hand, hardeners, which are each stored as separate components and are mixed immediately before use. Furthermore, two-component adhesives consisting of mixtures of polymerizable components and inactive hardeners are known, the hardeners being used immediately before use, e.g. through thermal energy. While the reactive mono-, di- or oligomers are mostly liquid or dissolved in an organic solvent, the hardeners are often in solid form, e.g. particulate.
Um das Adhäsionsvermögen von Mehrkomponentenklebern zuTo increase the adhesive power of multi-component adhesives
BESXtiβ erhöhen und insbesondere großflächige Fügeteile vollständig benetzen zu können, werden entweder einer Komponente, beiden Komponenten bzw. -im Falle eines mehr als zwei Komponenten aufweisenden Mehrkomponentenklebers- allen Komponenten vor dem Vermischen organische Lösungsmittel zugesetzt, oder es werden ein organisches Lösungsmittel vorgelegt und die jeweiligen Komponenten des Klebers in dieses eingemischt. Nachteilig hierbei ist einerseits, daß die flüssigen, häufig toxischen und entflammbaren organischen Lösungsmittel ein erhöhtes Umwelt- und Sicherheitsrisiko darstellen, andererseits verzögern sie die Aushärtezeit des Klebers, da sie sich nur langsam verflüchtigen und die Endfestigkeit des Klebers erst nach vollständiger Verflüchtigung der Lösungsmittel erreicht wird.BESXti β increase and in particular to be able to completely wet large parts to be joined, either one component, both components or - in the case of a multi-component adhesive having more than two components - all components are added to organic components before mixing, or an organic solvent and the respective components are introduced of the adhesive mixed into this. The disadvantage here is that the liquid, often toxic and flammable organic solvents pose an increased environmental and safety risk, on the other hand they delay the curing time of the adhesive, since they evaporate only slowly and the final strength of the adhesive is only achieved after the solvents have completely evaporated .
Der Erfindung liegt die Aufgabe zugrunde, einen Mehrkomponentenkleber der eingangs genannten Art vorzuschlagen, welcher die Verwendung flüssiger, organischer, häufig toxischer und entflammbarer Lösungsmittel entbehrlich macht und darüber hinaus kürzere Aushärtungszeiten bei einem erhöhten Adhäsionsvermögen aufweist. Sie ist ferner auf eine Vorrichtung zum Kleben mit einem solchen Mehrkomponentenkleber gerichtet .The invention has for its object to provide a multi-component adhesive of the type mentioned, which makes the use of liquid, organic, often toxic and flammable solvents unnecessary and also has shorter curing times with increased adhesiveness. It is also directed to a device for gluing with such a multi-component adhesive.
Der erste Teil dieser Aufgabe wird erfindungsgemäß mit einem Mehrkomponentenkleber der eingangs genannten Art dadurch gelöst, daß das Lösungsmittel flüssiges oder überkritisches Kohlendioxid (C02) ist.The first part of this object is achieved according to the invention with a multi-component adhesive of the type mentioned at the outset in that the solvent is liquid or supercritical carbon dioxide (C0 2 ).
Die Verwendung von überkritischem C02 als Lösungsund Extraktionsmittel ist bekannt. Überkritisches C02 wird beispielsweise zur Extraktion von Feststoffen (SFE, supercritical fluid extraction) eingesetzt. Die DE 44 06 899 AI beschreibt ein Verfahren zur Dekontamination von Böden, die mit militärischen Schadstoffen, wie Explosiv- Stoffen, Treibladungspulvern, Raketenfesttreibstoffen, pyrotechnischen Sätzen oder flüssigen Treibmitteln, kontaminiert sind, wobei die Schadstoffe mit überkritischem CC>2 als Lösungsmittel gegebenenfalls in Mi- schung mit organischen Lösungsmitteln aus dem Boden extrahiert und anschließend chemisch zersetzt werden. Überkritisches C02 wird weiterhin als Matrixflüssig- keit zur Durchführung chemischer Reaktionen, z.B. zur Durchführung von Polymerisationen (DE 36 09 829 AI, US 5 663 237) verwendet. Die bekannten Verfahren konnten der Fachwelt bislang jedoch keine Anregung zur Lösung des der Erfindung zugrundeliegenden Problems geben.The use of supercritical C0 2 as a solvent and extractant is known. Supercritical C0 2 is used for example for the extraction of solids (SFE, supercritical fluid extraction). DE 44 06 899 AI describes a method for decontamination of soils that are contaminated with military pollutants, such as explosives. Substances, propellant powders, rocket solid propellants, pyrotechnic charges or liquid propellants are contaminated, the pollutants with supercritical CC> 2 as a solvent, optionally mixed with organic solvents, extracted from the soil and then chemically decomposed. Supercritical CO 2 is also used as a matrix liquid for carrying out chemical reactions, for example for carrying out polymerizations (DE 36 09 829 AI, US 5,663,237). However, the known methods have so far not been able to give the experts any suggestions for solving the problem on which the invention is based.
Der Einsatz von überkritischem Kohlendioxid als inertem Lösungsmittel in einem Mehrkomponentenkleber gestattet den völligen Verzicht herkömmlicher flüssiger Lösungsmittel, die häufig toxisch und/oder entflammbar sind. Der kritische Punkt von Kohlendioxid liegt bei etwa 31°C und 73 bar. Überkritisches Kohlendioxid ist chemisch inert, toxikologisch unbedenklich und läßt sich durch Überführen in den unterkritischen Bereich, in dem es in Gasform übergeht, spontan abtrennen. Kohlendioxid weist in komprimiertem und insbesondere in überkritischem Zustand sehr gute Lösungsmitteleigenschaften auf, wobei die Lösemitteleigenschaften durch Variation der ParameterThe use of supercritical carbon dioxide as an inert solvent in a multi-component adhesive makes it possible to completely dispense with conventional liquid solvents, which are often toxic and / or flammable. The critical point of carbon dioxide is around 31 ° C and 73 bar. Supercritical carbon dioxide is chemically inert, toxicologically harmless and can be separated spontaneously by transferring it to the subcritical area in which it is converted into gas. Carbon dioxide has very good solvent properties in a compressed and in particular in a supercritical state, the solvent properties being obtained by varying the parameters
Temperatur und Druck steuerbar sind. Weiterhin erniedrigt es die Viskosität der Reaktionskomponenten bzw. der Mischung der Reaktionskomponenten und ermöglicht somit das Kleben von Fügeteilen in schwer zugänglichen Fügebe- reichen, beispielsweise das Kleben von großflächigeTemperature and pressure are controllable. Furthermore, it lowers the viscosity of the reaction components or the mixture of the reaction components and thus enables the bonding of parts to be joined in areas which are difficult to access, for example the bonding of large areas
Ausnehmungen oder Vorsprünge aufweisenden Fügeteilen im industriellen Bereich. Durch die spontane Verflüchtigung von Kohlendioxid im unterkritischen Zustand, beispielsweise bei Normalbedingungen, weist der Mehrkomponenten- kleber kurze Aushärtungszeiten auf, die ausschließlich durch die Reaktionszeit der reaktionsfähigen Komponenten bestimmt ist . Darüber hinaus inhibiert Kohlendioxid die chemische Reaktion der Komponenten -d.h. die Polymerisation bzw. Vernetzung der reaktionsfähigen Komponenten- so daß eine Vormischung der Komponenten über längere Zeit lagerbar ist . Durch die reaktionsinhibierende Wirkung von komprimiertem bzw. überkritischem Kohlendioxid sind die Verarbeitungszeiten des Mehrkomponentenklebers beispielsweise durch Variation der Konzentration der Mischung der Polymerkomponenten im Kohlendioxid steuerbar . Je nach Temperatur, Druck und Menge an komprimiertem oder überkritischem Kohlendioxid können somit filmartig dünne oder schaumartig dicke Kleberschichten erzeugt werden.Joining parts with recesses or projections in the industrial area. Due to the spontaneous volatilization of carbon dioxide in the subcritical state, for example under normal conditions, the multi-component adhesive has short curing times, which is solely due to the reaction time of the reactive components is determined. In addition, carbon dioxide inhibits the chemical reaction of the components - that is, the polymerization or crosslinking of the reactive components - so that a premix of the components can be stored for a long time. Due to the reaction-inhibiting effect of compressed or supercritical carbon dioxide, the processing times of the multi-component adhesive can be controlled, for example, by varying the concentration of the mixture of the polymer components in the carbon dioxide. Depending on the temperature, pressure and amount of compressed or supercritical carbon dioxide, thin or foam-like adhesive layers can be produced.
Zur Erhöhung des Lösevermögens können dem C02 soge- nannte Modifier zugesetzt sein, wobei als Modifier in der Regel geringe Mengen organischer Lösungsmittel, z.B. Ace- ton, Alkohole od. dgl . , verwendet werden.To increase the dissolving power, so-called modifiers can be added to the C0 2 , with small amounts of organic solvents, for example acetone, alcohols or the like, generally being used as modifiers. , be used.
Der Mehrkomponentenkleber kann, wie gesagt, aus zwei oder mehr reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten bestehen.As mentioned, the multicomponent adhesive can consist of two or more reactive mono-, di-, oligo- or polymer components.
In bevorzugter Ausführung ist vorgesehen, daß die reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten polyaddierende Prepolymere und Härter sind. Die Prepolymere können z.B. Di-, Tri- oder Polyole, wie Polyether- , Polyesterpolyole od. dgl., und die Härter Isocyanate mit wenigstens zwei Isocyanatgruppen (-N=C=0) sein. Die Prepolymere können beispielsweise auch Epoxide mit wenig- stens zwei Epoxidgruppen und die Härter Amine mit wenigstens zwei Aminogruppen sein.In a preferred embodiment it is provided that the reactive mono-, di-, oligo- or polymer components are polyadditive prepolymers and hardeners. The prepolymers can e.g. Di-, tri- or polyols, such as polyether, polyester polyols or the like, and the hardeners are isocyanates with at least two isocyanate groups (-N = C = 0). The prepolymers can, for example, also be epoxides with at least two epoxy groups and the hardeners amines with at least two amino groups.
Eine Vorrichtung zum Kleben mit einem solchen Mehrkomponentenkleber ist dadurch gekennzeichnet, daß sie wenig- stens zwei Behälter zur Aufnahme der reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten, von denen wenigstens einer mit C02 unter Druck beaufschlagbar ist, und eine mit beiden Behältern in Verbindung stehende Dosiereinrichtung aufweist. Ist ein Vormischen der reaktiven Komponenten mit komprimiertem bzw. überkritischem Kohlendioxid erwünscht, so sind beide Behälter der Vorrichtung mit C02 unter Druck beaufschlagbar ausgebildet .A device for gluing with such a multicomponent adhesive is characterized in that it has at least two containers for holding the reactive mono-, di-, oligo- or polymer components, of which at least one can be pressurized with C0 2 and has a metering device connected to both containers. If premixing of the reactive components with compressed or supercritical carbon dioxide is desired, both containers of the device are designed to be pressurized with CO 2 .
Um das Kohlendioxid in einen überkritischen Zustand zu überführen, ist in bevorzugter Ausführung vorgesehen, daß zumindest der mit C02 unter Druck beaufschlagbare Behälter beheizbar ist.In order to convert the carbon dioxide into a supercritical state, a preferred embodiment provides that at least the container which can be pressurized with C0 2 is heated.
In weiterhin bevorzugter Ausführung weist der mit Druck beaufschlagte Behälter ein Rührwerk auf, um eine homogene Lösung der jeweiligen Komponente im komprimierten bzw. überkritischen Kohlendioxid herzustellen.In a further preferred embodiment, the pressurized container has an agitator in order to produce a homogeneous solution of the respective component in the compressed or supercritical carbon dioxide.
Aus den genannten Gründen ist auch die beispielsweise als Düse ausgebildete Dosiereinrichtung vorzugsweise beheizbar.For the reasons mentioned, the metering device, for example in the form of a nozzle, is also preferably heatable.
Eine bevorzugte Ausführungsform sieht vor, daß zwischen den Behältern und der Dosiereinrichtung eine mit Druck beaufschlagte, vorzugsweise beheizbare und ein Rührwerk aufweisende Mischkammer angeordnet ist, um durch Variation der Parameter Druck, Temperatur und Konzentration der Mischung der Komponenten im komprimierten oder überkritischen Kohlendioxid die Adhäsionseigenschaften, die Viskosität und die Verarbeitungszeit bzw. die mögliche Bevorratungszeit des bereits gemischten Mehrkomponenten- klebers in der Mischkammer, ohne daß dieser dort aushärtet, einzustellen.A preferred embodiment provides that between the containers and the metering device a pressurized, preferably heatable and a stirrer mixing chamber is arranged to vary the parameters pressure, temperature and concentration of the mixture of the components in the compressed or supercritical carbon dioxide, the adhesion properties, adjust the viscosity and the processing time or the possible storage time of the already mixed multi-component adhesive in the mixing chamber without it curing there.
Nachstehend ist die Erfindung anhand eines Ausführungs- beispiels beschrieben. AusführungsbeispielThe invention is described below using an exemplary embodiment. Embodiment
Eine Mischung von polyaddierenden Prepolymeren in Form von Polyolen (Komponente 1) und Härtern in Form von Di- und Triisocyanaten (Komponente 2) wird in einem Autoklaven mit einer Rühreinrichtung mit einer Einrichtung zur Messung des Drehmoments bei konstanter Temperatur mit komprimiertem, flüssigen oder überkritischem Kohlendioxid beaufschlagt. Die Verringerung der Viskosität der Reaktionsmischung zeigt sich nach kurzer Mischzeit in einer Verringerung des Drehmomentes der Rühreinrichtung. Die Reaktionsmischung wird über eine Dosiereinrichtung auf die Fügefläche benetzend aufgebracht und ausgehärtet . Gelchromatographische Analysen an solchermaßen gebildeten Polyurethanen zeigen, daß diese einen geringeren Polymerisationsgrad als die ohne den Zusatz von Kohlendioxid, aber unter ansonsten identischen Bedingungen aus den gleichen Ausgangskomponenten (Polyole und Di- bzw. Tri- isocyanate) erzeugten Polymere aufweisen. Flüssiges bzw. überkritisches Kohlendioxid inhibiert folglich die Bildungsreaktion des Polyurethans bzw. die Polymerisation oder Vernetzung der reaktionsfähigen Komponenten.A mixture of polyadditive prepolymers in the form of polyols (component 1) and hardeners in the form of di- and triisocyanates (component 2) is in an autoclave with a stirring device with a device for measuring the torque at constant temperature with compressed, liquid or supercritical carbon dioxide acted upon. The reduction in the viscosity of the reaction mixture is evident after a short mixing time in a reduction in the torque of the stirring device. The reaction mixture is applied to the joining surface by a metering device and cured. Gel chromatography analyzes on polyurethanes formed in this way show that these have a lower degree of polymerization than the polymers produced without the addition of carbon dioxide, but under otherwise identical conditions from the same starting components (polyols and di- or tri-isocyanates). Liquid or supercritical carbon dioxide consequently inhibits the formation reaction of the polyurethane or the polymerization or crosslinking of the reactive components.
Nachstehend ist die erfindungsgemäße Vorrichtung anhand der Zeichnung näher erläutert, die eine Ausführungsform einer Vorrichtung zum Kleben mit einem Zweikomponentenkleber in schematischer Darstellung zeigt .The device according to the invention is explained in more detail below with reference to the drawing, which shows a schematic representation of an embodiment of a device for gluing with a two-component adhesive.
Die dargestellte Vorrichtung weist zwei Behälter la, lb zur Aufnahme der reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten auf, von denen der Behälter la beheizbar und über Ventile 5, 11 mittels einer Pumpe 12, z. B. einer Membranpumpe, mit komprimiertem bzw. flüssigem oder überkritischem Kohlendioxid druckbeaufschlagbar ist. Das Kohlendioxid ist in einem Vorratsbehälter 13 bevorratet . Während der Behälter la z . B . Prepolymere in Form von Polyolen enthält, sind im Behälter 2b z. B. Härter in Form von Di- oder Triisocyanaten socyaraten bevorratet. Zur Herstellung einer homogenen Vormischung weist der Behälter la ein Rührwerk 6 auf .The device shown has two containers la, lb for receiving the reactive mono-, di-, oligo or polymer components, of which the container la is heated and via valves 5, 11 by means of a pump 12, for. B. a diaphragm pump, can be pressurized with compressed or liquid or supercritical carbon dioxide. The carbon dioxide is stored in a storage container 13. While the container la z. B. Contains prepolymers in the form of polyols are in the container 2b z. B. hardener in the form of di- or triisocyanate stocks. In order to produce a homogeneous premix, the container 1 a has an agitator 6.
Die in den Behältern la, lb bevorrateten Komponenten sind über ein Ventil 8 bzw. über ein Ventil 9 und eine z. B. als Spritzen-, Kolbenpumpe oder dergleichen ausgebildete Pumpe 14 in eine beheizbare Mischkammer 4 überführbar. In der Mischkammer 4 wird die Polyole, Isocyanate und flüssiges oder überkritisches Kohlendioxid enthaltende Reaktionsmischung mittels eines Rührwerks 7 homogenisiert. Die Mischkammer 4 ist über die Ventile 5 , 8 , 11 mittels der Pumpe 12 mit flüssigem oder überkritischem Kohlendioxid beaufschlagbar. Alternativ oder zusätzlich kann die Mischkammer 4 ihrerseits ein (nicht dargestelltes) Ventil zur direkten Beaufschlagung mit flüssigem oder überkritischem Kohlendioxid aufweisen.The components stored in the containers la, lb are via a valve 8 or via a valve 9 and a z. B. designed as a syringe, piston pump or the like pump 14 in a heatable mixing chamber 4. In the mixing chamber 4, the reaction mixture containing polyols, isocyanates and liquid or supercritical carbon dioxide is homogenized by means of an agitator 7. The mixing chamber 4 can be supplied with liquid or supercritical carbon dioxide via the valves 5, 8, 11 by means of the pump 12. Alternatively or additionally, the mixing chamber 4 can in turn have a valve (not shown) for direct application of liquid or supercritical carbon dioxide.
An die Mischkammer 4 schließt über ein Ventil 10 eine Dosiereinrichtung 2 in Form einer beheizbaren Düse 3 an. Die Ventile 5, 8, 9, 10, 11 sind insbesondere als Hochdruckventile ausgebildet.A metering device 2 in the form of a heatable nozzle 3 connects to the mixing chamber 4 via a valve 10. The valves 5, 8, 9, 10, 11 are designed in particular as high-pressure valves.
Durch Variation der Parameter Druck, Temperatur und Konzentration von flüssigem oder überkritischem Kohlendioxid im Behälter la bzw. in der Mischkammer 4 können filmartig dünne oder schaumartig dicke Kleberschichten erzeugt werden. Alternativ kann auch die Mischkammer lb über ein (nicht dargestelltes) Ventil mit Kohlendioxid druckbeaufschlagbar bzw. beheizbar sein und in diesem Fall die in den Behältern la, lb bevorrateten Vormischungen über Ventile auch unmittelbar in der Dosiereinrich- tung miteinander gemischt und dosiert werden. By varying the parameters of pressure, temperature and concentration of liquid or supercritical carbon dioxide in the container 1 a or in the mixing chamber 4, film-like thin or foam-like adhesive layers can be produced. Alternatively, the mixing chamber 1b can also be pressurized or heated with carbon dioxide via a valve (not shown) and in this case the premixes stored in the containers 1a, 1b can also be mixed and metered directly in the metering device via valves.

Claims

Patentansprüche claims
1. Mehrkomponentenkleber mit wenigstens zwei reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten, von denen wenigstens eine in wenigstens einem Lö- sungsmittel gelöst ist, dadurch gekennzeichnet, daß das Lösungsmittel flüssiges oder überkritisches Kohlendioxid (C0 ) ist.1. Multi-component adhesive with at least two reactive mono-, di-, oligo- or polymer components, at least one of which is dissolved in at least one solvent, characterized in that the solvent is liquid or supercritical carbon dioxide (C0).
2. Mehrkomponentenkleber nach Anspruch 1 , dadurch gekennzeichnet, daß dem C02 Modifier zur Erhöhung seines Lösevermögens zugesetzt sind.2. Multi-component adhesive according to claim 1, characterized in that the C0 2 modifiers are added to increase its solvent power.
3. Mehrkomponentenkleber nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß er ein Zweikomponentenkle- ber ist .3. Multi-component adhesive according to claim 1 or 2, characterized in that it is a two-component adhesive.
4. Mehrkomponentenkleber nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten poly- addierende Prepolymere und Härter sind.4. Multi-component adhesive according to one of claims 1 to 3, characterized in that the reactive mono-, di-, oligo- or polymer components are poly-additive prepolymers and hardeners.
5. Mehrkomponentenkleber nach Anspruch 4 , dadurch gekennzeichnet, daß die Prepolymere Di-, Tri- oder Polyole und die Härter Isocyanate mit wenigstens zwei Isocyanatgruppen (-N=C=0) sind.5. Multi-component adhesive according to claim 4, characterized in that the prepolymers di-, tri- or polyols and the hardener isocyanates with at least two isocyanate groups (-N = C = 0).
6. Mehrkomponentenkleber nach Anspruch 4 , dadurch gekennzeichnet, daß die Prepolymere Epoxide mit wenigstens zwei Epoxidgruppen und die Härter Amine mit wenigstens zwei Aminogruppen sind. 6. Multi-component adhesive according to claim 4, characterized in that the prepolymers are epoxies with at least two epoxy groups and the hardeners are amines with at least two amino groups.
. Vorrichtung zum Kleben mit einem Mehrkomponentenkleber gemäß einem der Ansprüche 1 bis 6 , dadurch gekennzeichnet, daß sie wenigstens zwei Behälter (la, lb) zur Aufnahme der reaktionsfähigen Mono-, Di-, Oligo- oder Polymerkomponenten, von denen wenigstens einer (la) mit C02 unter Druck beaufschlagbar ist, und eine mit beiden Behältern (la, lb) in Verbindung stehende Dosiereinrichtung (2) aufweist ., Device for gluing with a multicomponent adhesive according to one of Claims 1 to 6, characterized in that it has at least two containers (la, lb) for holding the reactive mono-, di-, oligo- or polymer components, at least one of which (la) with C0 2 can be acted upon under pressure and has a metering device (2) which is connected to both containers (la, lb).
8. Vorrichtung nach Anspruch 7, dadurch gekennzeichnet, daß zumindest der mit C02 beaufschlagbare Behälter (la) beheizbar ist.8. The device according to claim 7, characterized in that at least the container can be acted upon with C0 2 (la) is heated.
9. Vorrichtung nach Anspruch 7 oder 8, dadurch gekennzeichnet, daß zumindest der mit C02 beaufschlagbare Behälter (la) ein Rührwerk (6) aufweist.9. Apparatus according to claim 7 or 8, characterized in that at least the container (la) to which C0 2 can be applied has an agitator (6).
10. Vorrichtung nach einem der Ansprüche 7 bis 9, dadurch gekennzeichnet, daß die Dosiereinrichtung (2) beheizbar ist .10. Device according to one of claims 7 to 9, characterized in that the metering device (2) is heatable.
11. Vorrichtung nach einem der Ansprüche 7 bis 10, dadurch gekennzeichnet, daß die Dosiereinrichtung (2) eine Düse (3) ist.11. Device according to one of claims 7 to 10, characterized in that the metering device (2) is a nozzle (3).
12. Vorrichtung nach einem der Ansprüche 7 bis 11, dadurch gekennzeichnet, daß zwischen den Behältern (la, lb) und der Dosiereinrichtung (2) eine mit Druck beaufschlagbare Mischkammer (4) angeordnet ist.12. Device according to one of claims 7 to 11, characterized in that between the containers (la, lb) and the metering device (2) is arranged a pressurizable mixing chamber (4).
13. Vorrichtung nach Anspruch 12 , dadurch gekennzeich- net, daß die Mischkammer (4) beheizbar ist. 13. The apparatus according to claim 12, characterized in that the mixing chamber (4) is heatable.
4. Vorrichtung nach Anspruch 12 oder 13, dadurch gekennzeichnet, daß die Mischkammer (4) ein Rührwerk auf eist . 4. Apparatus according to claim 12 or 13, characterized in that the mixing chamber (4) has an agitator.
PCT/EP2000/004131 1999-05-12 2000-05-09 Multi-component adhesive and gluing device, used with a multi-component adhesive of this type WO2000069551A1 (en)

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DE19922018.2 1999-05-12
DE19922018A DE19922018A1 (en) 1999-05-12 1999-05-12 Multi-component adhesive and device for gluing with such a multi-component adhesive

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5407132A (en) * 1993-10-20 1995-04-18 Nordson Corporation Method and apparatus for spraying viscous adhesives
EP0758662A2 (en) * 1995-08-15 1997-02-19 Rockwell International Corporation Curable epoxy compositions containing aziridine
WO1997023525A1 (en) * 1995-12-22 1997-07-03 Minnesota Mining And Manufacturing Company Process for making (thio)urethanes under superatmospheric conditions

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5106650A (en) * 1988-07-14 1992-04-21 Union Carbide Chemicals & Plastics Technology Corporation Electrostatic liquid spray application of coating with supercritical fluids as diluents and spraying from an orifice

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5407132A (en) * 1993-10-20 1995-04-18 Nordson Corporation Method and apparatus for spraying viscous adhesives
EP0758662A2 (en) * 1995-08-15 1997-02-19 Rockwell International Corporation Curable epoxy compositions containing aziridine
WO1997023525A1 (en) * 1995-12-22 1997-07-03 Minnesota Mining And Manufacturing Company Process for making (thio)urethanes under superatmospheric conditions

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