DE4202707C1 - Large polyurethane casting prodn. - based on isophorone di:isocyanate and polyether from tri:ol and propylene oxide, by stepwise heating and cooling in mould - Google Patents
Large polyurethane casting prodn. - based on isophorone di:isocyanate and polyether from tri:ol and propylene oxide, by stepwise heating and cooling in mouldInfo
- Publication number
- DE4202707C1 DE4202707C1 DE19924202707 DE4202707A DE4202707C1 DE 4202707 C1 DE4202707 C1 DE 4202707C1 DE 19924202707 DE19924202707 DE 19924202707 DE 4202707 A DE4202707 A DE 4202707A DE 4202707 C1 DE4202707 C1 DE 4202707C1
- Authority
- DE
- Germany
- Prior art keywords
- hours
- propylene oxide
- polyether
- castings
- cooling
- 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 - Fee Related
Links
Classifications
-
- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
- B29C39/38—Heating or cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
- B29C39/40—Compensating volume change, e.g. retraction
-
- 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
-
- 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
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4816—Two or more polyethers of different physical or chemical nature mixtures of two or more polyetherpolyols having at least three hydroxy groups
-
- 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
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
Description
Bekanntlich lassen sich aus Gießharzen auf Polyurethan basis großvolumige Gießkörper, die glasklar sind und weder Blasen noch Spannungsrisse im Innern aufweisen, kaum herstellen.As is well known, cast resins can be made from polyurethane base large-volume castings that are crystal clear and there are no bubbles or stress cracks inside, hardly manufacture.
Aus der DE-OS 33 29 392 sind Konstruktionsmaterialien auf Basis von Polyurethanen bekannt, die erhältlich sind durch Umsetzung von u. a. einem cycloaliphatischen Diiso cyanat, wie Isophorondiisocyanat, mit mindestens einem vorwiegend aus Propylenoxideinheiten aufgebauten Polyether, der auf einem Triol beruht und eine OH-Zahl von 250 bis 600 hat. Die Herstellung der Konstruktions materialien erfolgt nach den in der Polyurethantechnik üblichen Methoden, beispielsweise durch homogene Ver mischung der Komponenten, Einbringen in eine Form und Aushärtung bei erhöhter Temperatur. Jedoch lassen sich diese Materialien nicht zu großvolumigen Formkörpern vergießen. DE-OS 33 29 392 are construction materials based on polyurethanes that are available by implementing u. a. a cycloaliphatic diiso cyanate, such as isophorone diisocyanate, with at least one predominantly composed of propylene oxide units Polyether based on a triol and an OH number from 250 to 600. The construction of the construction materials are made according to those in polyurethane technology usual methods, for example by homogeneous ver mixing the components, placing them in a mold and Curing at an elevated temperature. However, these materials do not form large-volume moldings shed.
Es wurde nun gefunden, daß großvolumige Gußkörper auf Polyurethanbasis hergestellt werden können, wenn bestimmte Polyisocyanate nach einem bestimmten Tempe rungsverfahren verarbeitet werden.It has now been found that large-volume castings can be made on a polyurethane basis, if certain polyisocyanates according to a certain tempe processing procedures.
Gegenstand der Erfindung ist daher ein Verfahren zur Herstellung großvolumiger Gußkörper auf Polyurethanbasis durch Zusammengeben cycloaliphatischer Isocyanate auf Basis von Isophorondiisocyanat und Polyethern auf Basis von einem Triol und Propylenoxid mit einer OH-Zahl von 300 bis 600 bei wenig erhöhter Temperatur und Verguß in Formen und anschließender Härtung. Das Verfahren ist da durch gekennzeichnet, daß das vergossene Gemisch im Temperaturbereich von 50 bis 150°C schrittweise über einen Zeitraum bis 72 Stunden getempert wird, daß je weils nach mindestens 10 Stunden die Temperatur um mindestens 10°C erhöht wird und man den erhaltenen Guß körper über ca. 12 Stunden bei stufenweiser Herabschal tung der Temperatur abkühlt. The invention therefore relates to a method for Production of large-volume castings based on polyurethane by combining cycloaliphatic isocyanates Based on isophorone diisocyanate and polyethers based of a triol and propylene oxide with an OH number of 300 to 600 at slightly elevated temperature and potting in Molding and subsequent hardening. The procedure is there characterized in that the poured mixture in Temperature range from 50 to 150 ° C gradually is annealed for a period of up to 72 hours, that because after at least 10 hours the temperature changes is increased at least 10 ° C and the obtained casting body over approx. 12 hours with gradual descent cooling of the temperature.
Die erfindungsgemäß hergestellten Gußkörper sind völlig amorph und durchsichtig. Es können erfindungsgemäß Guß körper bis zu mehreren hundert Kilogramm Gewicht herge stellt werden.The cast bodies produced according to the invention are complete amorphous and transparent. According to the invention, castings can be made bodies weighing up to several hundred kilograms be put.
Die Polyether des OH-Zahl-Bereichs 300 bis 600 werden hergestellt, indem man an Trimethylolpropan Propylen oxid polyaddiert.The polyethers in the OH number range from 300 to 600 are made by using propylene on trimethylolpropane oxide polyadd.
Die Temperung der Gußkörper erfolgt bei Temperaturen von 50 bis 150°C über einen Zeitraum bis 72 Stunden, wobei die Temperatur jeweils nach mindestens 10 Stunden und mindestens 10°C erhöht wird.The castings are tempered at temperatures of 50 to 150 ° C over a period of up to 72 hours, wherein the temperature after at least 10 hours and is increased by at least 10 ° C.
Aus der DE-OS 23 38 185, Beispiel 1, ist bereits be kannt, PUR-Gußkörper durch Vermischen von Isophorondi isocyanat mit einem Polyether auf Basis von Trimethylol propan und Propylenoxid und Aushärtung des Gemischs in einer 120°C heißen Form herzustellen. Generell beschreibt diese DE-OS (Seite 7), daß die Herstellung von PUR-Guß körpern nach der üblichen Verarbeitungsweise für Gieß harze erfolgen kann und erläutert dann weiter, daß man im einfachsten Fall die Isocyanat-Komponente auf Tempe raturen von 20 bis 130°C erhitzt und unter Rühren das Polyolgemisch hinzugibt. Die so erhaltene Mischung wird in eine Form aus Kunststoff oder Metall gegossen, in der die Härtung bei Temperaturen von 23 bis 30°C nach Zugabe von Katalysatoren (Kalthärtung) oder bei 30 bis 80°C (Wärmehärtung) oder bei 80 bis 180°C (Heißhärtung) während einer Zeit zwischen einigen Minuten bis zu mehreren Stunden erfolgen kann.From DE-OS 23 38 185, Example 1, is already knows, PUR cast body by mixing Isophorondi isocyanate with a polyether based on trimethylol propane and propylene oxide and curing the mixture in a mold at 120 ° C. Generally describes this DE-OS (page 7) that the production of PUR casting bodies according to the usual way of processing for casting Resins can take place and then further explains that one in the simplest case, the isocyanate component on tempe heated from 20 to 130 ° C and with stirring Add polyol mixture. The mixture thus obtained is poured into a plastic or metal mold in which curing at temperatures from 23 to 30 ° C after addition of catalysts (cold hardening) or at 30 to 80 ° C (Heat curing) or at 80 to 180 ° C (heat curing) for a period of between a few minutes up to can take several hours.
Diesem bekannten Stand der Technik ist indessen das er fingungswesentliche Merkmal, daß jeweils nach mindestens 10 Stunden die Temperatur um mindestens 10°C erhöht wird, nicht zu entnehmen. Es hat sich aber gezeigt, daß gerade ein solches langsames Aufheizen zur Aushärtung von großvolumigen Gußkörpern auf Polyurethanbasis not wendig ist, um völlig amorphe und durchsichtige Produkte zu erhalten.This known prior art, however, is that essential feature of the training, that after each at least The temperature is increased by at least 10 ° C for 10 hours will not be removed. However, it has been shown that just such a slow heating up for curing of large-volume castings based on polyurethane not is nimble to completely amorphous and transparent products to obtain.
Die erfindungsgemäß hergestellen Gußkörper können im Bereich der Architektur und Technik z. B. als Säulen element (Zylinder, Quader), als Möbelstück oder im optisch-technischen Bereich verwendet werden. The castings produced according to the invention can be in Area of architecture and technology z. B. as columns element (cylinder, cuboid), as a piece of furniture or in optical-technical area can be used.
Das Gießen großformatiger, glasklarer, blasenfreier Ob jekte aus Polyurethan (ohne Füllstoff):The casting of large-format, crystal-clear, bubble-free ob objects made of polyurethane (without filler):
Aus den Komponenten, die zu den anwendungstechnischen Versuchsprodukten zählen, konnten sehr großformatige glasklare Formkörper gegossen werden, die über eine hohe Stabilität verfügen.From the components to the application technology Trial products could count very large format crystal-clear moldings are poured over a high Have stability.
Die verarbeiteten Materialien sind:
modifiziertes cycloaliphatisches Isocyanat auf der Basis
Isophorondiisocyanat (ca. 27% NCO)
(®Baymidur-Versuchsprodukt KU 3-5001-1)
Polyether aus Propylenoxid und Trimethylolpropan
(OHZ: 380) (®Baygal K 55)
(OHZ: 550) (®Baygal K 30)The processed materials are:
modified cycloaliphatic isocyanate based
Isophorone diisocyanate (approx. 27% NCO)
(®Baymidur trial product KU 3-5001-1)
Propylene oxide and trimethylol propane polyether
(OHZ: 380) (®Baygal K 55)
(OHZ: 550) (®Baygal K 30)
Das cycloaliphatische Isocyanat wurde aufbereitet, bis es völlig blasenfrei war.The cycloaliphatic isocyanate was processed until it was completely free of bubbles.
Die beiden Polyetherpolyole wurden ca. 12 Stunden bei ca. 80°C getempert und anschließend ebenfalls aufbe reitet. The two polyether polyols were at about 12 hours annealed at approx. 80 ° C and then also heated up rode.
Die für 110-120 kg Gesamtmaterial notwendigen ein zelnen Komponenten wurden zusammengefügt, wobei auf Ka talysatoren verzichtet wurde und aufbereitet, bis eine homogene Vergußmasse entstand.The necessary for 110-120 kg total material individual components were put together, with Ka was replaced and processed until one homogeneous potting compound was created.
Ein Verarbeiten mit Moltopren® Blaupaste BU erschien geeignet, transparente intensiv blaue Formkörper zu vergießen.Processing with Moltopren® Blaupaste BU appeared suitable, transparent intense blue molded body too shed.
Eine Verarbeitungszeit von ca. 5 Stunden ließ ein vor sichtiges, blasenfreies Vergießen des Materials zu.A processing time of about 5 hours allowed visible, bubble-free pouring of the material.
Umriß- und spannungsfreie Körper zu erhalten, wurde ein vorsichtiges, stufenweises Tempern notwendig, beginnend bei Raumtemperatur.Getting a body that is free of contours and tension became a careful, gradual annealing necessary, starting at room temperature.
Nach dem Entformen erhielt man einen sehr stabilen Gußkörper, wel cher mechanischer Beanspruchung hervorragend standhielt. Die nach dem Schleifen (trocken oder naß) angewendete Methode, welche sich für weniger harte Polyurethan-Sys teme besonders gut eignet, ist das Kaltgas-Poliersystem, wobei ein kalter gasförmiger Stickstoff kontinuierlich während des Poliervorganges die Oberfläche des zu schleifenden Objektes kühlt.After removal from the mold, a very stable cast body was obtained withstand mechanical stress excellently. The one applied after grinding (dry or wet) Method which is suitable for less hard polyurethane systems the cold gas polishing system, taking a cold gaseous nitrogen continuously during the polishing process the surface of the grinding object cools.
Es hinterläßt hochglänzende Objektflächen, die mit her kömmlichen Poliermitteln nicht zu erzielen sind. It leaves high-gloss object surfaces that come with conventional polishing agents cannot be achieved.
Verarbeitungsweise für ca. 130 kg.Processing method for approx. 130 kg.
- 1. Aufbereitung des cycloaliphatischen Isocyanats im Vakuum, ca. 1 Stunde pro 30 kg, bis zur völligen Blasenfreiheit. 1. Preparation of the cycloaliphatic isocyanate in Vacuum, about 1 hour per 30 kg, until complete No bubbles.
- 2. Nach einer ca. 12stündigen Trockenzeit - bei ca. 80°C - der beiden Polyole, wird ebenfalls ein Eva kuieren bis zur geringen Blasenbildung durchge führt.2. After a drying time of approx. 12 hours - at approx. 80 ° C - of the two polyols, also becomes an Eva cut until there is little blistering leads.
Anschließend werden beide Ausgangskomponenten, wobei die Polyetherpolyole abgekühlt zu verarbeiten sind, mitein ander nach den für den Ansatz großformatiger Teile ent sprechenden Gewichten gemischt;Then both starting components, the Processed cooled polyether polyols different after the for the approach of large format parts speaking weights mixed;
71,5 kg cycloaliphatische Isocyanat
49,5 kg Polyether (OHZ = 380)
30,0 kg Polyether (OHZ = 550).71.5 kg of cycloaliphatic isocyanate
49.5 kg polyether (OHZ = 380)
30.0 kg polyether (OHZ = 550).
5×ca. 30 kg Material mußte bis zur vollkommenen Homo genität in der Vakuumanlage aufbereitet werden. Der Vor gang dauerte jeweils 90 Minuten. Der einzelne Ansatz hatte anschließend eine Topfzeit von ungefähr 5 Stunden, wobei das Material zusammen vergossen wurde.5 × approx. 30 kg of material had to be completely gay be processed in the vacuum system. The before each took 90 minutes. The single approach then had a pot life of about 5 hours, the material was shed together.
In der verschlossenen, auf ca. 40°C vorgeheizten Form reagierte der Ansatz bei einer Ofentemperatur von 30°C ca. 24 Stunden bis zu einer noch eindrückbaren, gummi artigen Formmasse, auf dem inzwischen geschrumpften Material (ca. 1,5% des Gesamtansatzes).In the closed form, preheated to approx. 40 ° C the mixture reacted at an oven temperature of 30 ° C approx. 24 hours to a rubber that can still be pushed in like Molding compound on the now shrunk material (approx. 1.5% of the total approach).
Während der Aushärtungszeit bei Temperaturen, die wenig oberhalb der Raumtemperatur liegen, erreicht der Ansatz eine wesentliche Erhöhung der Eigentemperatur.During the curing period at temperatures that are little the approach reaches a significant increase in self temperature.
Messungen an den Formwandungen ergaben 35 bis 40°C.Measurements on the mold walls showed 35 to 40 ° C.
Nach 24 Stunden erhöht man die Ofentemperatur auf 60°C, nach weiteren 24 Stunden auf 70°C.After 24 hours, the oven temperature is increased to 60 ° C, after another 24 hours at 70 ° C.
Dieses vorsichtige, etwas langfristige Tempern verhin dert bei großvolumigen ungefüllten Gußkörpern Material spannung beziehungsweise Rißbildungen.This careful, somewhat long-term annealing prevents changes with large-volume unfilled castings material tension or cracking.
Ein vorsichtiges Abkühlen über ca. 12 Stunden bei stu fenweiser Herabschaltung der Temperatur ist dabei eben falls notwendig.A careful cooling over approx. 12 hours at stu Lowering the temperature by level is even if required.
Der Gußkörper ist gut entformbar und eine Überarbeitung der Oberfläche ist kaum erforderlich.The cast body is easy to demold and one It is hardly necessary to rework the surface.
Der bei der genannten Rezeptur weniger spröde Ansatz ließ sich mit einem für PUR-Lacke (Autoindustrie) ange wandten Kaltgaspolierverfahren hervorragend hochglänzend polieren.The less brittle approach with the recipe mentioned got started with one for PUR paints (auto industry) applied cold gas polishing processes with excellent high gloss polishing.
Der fertige Gußkörper ließ vielerlei Beanspruchung mecha nischer beziehungsweise handwerklicher Art zu.The finished cast body left a lot of stress on mecha African or handicraft type.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19924202707 DE4202707C1 (en) | 1992-01-31 | 1992-01-31 | Large polyurethane casting prodn. - based on isophorone di:isocyanate and polyether from tri:ol and propylene oxide, by stepwise heating and cooling in mould |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19924202707 DE4202707C1 (en) | 1992-01-31 | 1992-01-31 | Large polyurethane casting prodn. - based on isophorone di:isocyanate and polyether from tri:ol and propylene oxide, by stepwise heating and cooling in mould |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE4202707C1 true DE4202707C1 (en) | 1993-06-24 |
Family
ID=6450648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19924202707 Expired - Fee Related DE4202707C1 (en) | 1992-01-31 | 1992-01-31 | Large polyurethane casting prodn. - based on isophorone di:isocyanate and polyether from tri:ol and propylene oxide, by stepwise heating and cooling in mould |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE4202707C1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2083029A1 (en) * | 2006-11-17 | 2009-07-29 | Mitsui Chemicals, Inc. | Optical polyurethane resin composition and optical polyurethane resin |
-
1992
- 1992-01-31 DE DE19924202707 patent/DE4202707C1/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2083029A1 (en) * | 2006-11-17 | 2009-07-29 | Mitsui Chemicals, Inc. | Optical polyurethane resin composition and optical polyurethane resin |
| EP2083029A4 (en) * | 2006-11-17 | 2013-04-10 | Mitsui Chemicals Inc | Optical polyurethane resin composition and optical polyurethane resin |
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| 8100 | Publication of the examined application without publication of unexamined application | ||
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