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DE4003718A1 - Polyurethane foam prepn. - Google Patents

Polyurethane foam prepn.

Info

Publication number
DE4003718A1
DE4003718A1 DE19904003718 DE4003718A DE4003718A1 DE 4003718 A1 DE4003718 A1 DE 4003718A1 DE 19904003718 DE19904003718 DE 19904003718 DE 4003718 A DE4003718 A DE 4003718A DE 4003718 A1 DE4003718 A1 DE 4003718A1
Authority
DE
Germany
Prior art keywords
polyurethane foam
liquid phosphorus
containing flame
weight
flame retardants
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.)
Granted
Application number
DE19904003718
Other languages
German (de)
Other versions
DE4003718C2 (en
Inventor
Hans Wilhelm Huetzen
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.)
Individual
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to DE19904003718 priority Critical patent/DE4003718A1/en
Application filed by Individual filed Critical Individual
Priority to CA002031218A priority patent/CA2031218C/en
Priority to AU54065/90A priority patent/AU638243B2/en
Priority to EP90107041A priority patent/EP0394769B1/en
Priority to US07/635,152 priority patent/US5182309A/en
Priority to JP2505620A priority patent/JPH0762090B2/en
Priority to HU903726A priority patent/HU210404B/en
Priority to SU904894218A priority patent/RU2058336C1/en
Priority to DE59010789T priority patent/DE59010789D1/en
Priority to AT90107041T priority patent/ATE161865T1/en
Priority to PCT/EP1990/000581 priority patent/WO1990012841A1/en
Priority to PT93851A priority patent/PT93851B/en
Priority to CS902006A priority patent/CZ284933B6/en
Priority to SK2006-90A priority patent/SK280709B6/en
Priority to PL90284914A priority patent/PL164531B1/en
Priority to YU00816/90A priority patent/YU81690A/en
Priority to TR42890A priority patent/TR26440A/en
Priority to NO90905528A priority patent/NO905528L/en
Publication of DE4003718A1 publication Critical patent/DE4003718A1/en
Priority to HRP920980AA priority patent/HRP920980A2/en
Priority to LVP-93-33A priority patent/LV10470B/en
Priority to GEAP19931455A priority patent/GEP19970640B/en
Publication of DE4003718C2 publication Critical patent/DE4003718C2/de
Application granted granted Critical
Granted legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/127—Mixtures of organic and inorganic blowing agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The foam (I), contg. catalysts, cell stabilisers, and/or flame retardants, has pores free from halogenated hydrocarbons but contg. minor amts. of blowing agent (II) consisting of at least 3-6C alkane with b.pt. at normal pressure (-)10 (+)70 deg. C. Pref. prepn. of (I) using (II), wherein (1) (II), in conventional amt., is finely distributed either (i) in mixt. of alcohol and isocyanate starting components in conventional ratio for (I), and other finely divided additives such as flame retardants, catalysts, and pore stabilisers, or (ii) in alcohol component, with mixing in of additives, then conventional amt. of isocyanate component for forming (I) is incorporated, finely divided, (2) components are polymerised to form (I) under conventional conditions, partic. of temp.

Description

Im Hauptpatent ... (Hauptpatentanmeldung Nr. P 39 33 705.7) ist ein Polyurethanschaumstoff, nachfolgend kurz PUR-Schaumstoff genannt, beschrieben, dessen Zellen frei von den umweltschädlichen Halogenkohlenwasserstoffen wie Fluorchlorkohlenwasserstoffe (FCKW) oder nicht voll halogenierte Kohlenwasserstoffe, sog. weiche FCKW, sind, sowie ein Verfahren zu dessen Herstellung, bei dem keine Halogenkohlenwasserstoffe als Treibmittel verwendet werden. Der PUR-Schaumstoff gemäß dem Hauptpatent ... (Hauptpatentanmeldung P 39 33 705.7) ist dadurch gekennzeichnet, daß in seinen Zellen in hohem Prozentsatz (ca. 80%) Luft vorhanden ist und geringe Mengen des in dem Herstellungsverfahren verwendeten Treibmittels, d. h. niederen Kohlenwasserstoffen mit 3-6 Kohlenstoffatomen mit einem bestimmten niedrigen Siedepunkt, wie insbesondere und bevorzugt n-Pentan, und in dem die Alkoholkomponente des herzustellenden PUR-Schaumstoffs nicht oder im wesentlichen nicht löslich ist. In the main patent ... (main patent application No. P 39 33 705.7) a polyurethane foam, hereinafter referred to as PUR foam called, described, whose cells are free from the environmentally harmful halogenated hydrocarbons such as Chlorofluorocarbons (CFCs) or not full halogenated hydrocarbons, so-called soft CFCs, are and a process for its production in which none Halogenated hydrocarbons can be used as blowing agents. The PUR foam according to the main patent ... (Main patent application P 39 33 705.7) characterized that in his cells in high percentage (approx. 80%) air is present and small amounts of that in the Manufacturing process used blowing agent, d. H. lower hydrocarbons with 3-6 carbon atoms a certain low boiling point, such as in particular and preferably n-pentane, and in which the alcohol component of not to produce PUR foam or essentially is not soluble.  

Das Verfahren zur Herstellung derartiger Schaumstoffe ist dadurch gekennzeichnet, daß einerseits aus einer üblichen alkoholischen Komponente der herzustellenden Weich- oder insbesondere Polyurethanhartschaumstoffe und andererseits dem bei der Ausgangstemperatur des Gemischs bei dem angewandten Druck flüssigen organischen Treibmittel in der je nach dem gewünschten Schäumungsgrad notwendigen Menge, und unter Zugabe von flüssigen phosphorhaltigen Flammschutzmitteln, ggfs. im Gemisch mit anderen Flammschutzmitteln wie festen Phosphorsäuresalzen und ggfs. unter Zusatz eines Emulgators, ausgenommen die einzusetzende übliche Isocyanat-Komponente, eine Emulsion gebildet wird, so daß sich eine sehr gleichmäßige Verteilung des Treibmittels in flüssigem Zustand im Gemisch bildet, und sodann diese Emulsion mit der Isocyanat-Komponente in üblicher Weise vermischt wird, so daß die chemische Reaktion zwischen dem Di- oder Polyol einerseits und dem Di- oder Triisocyanat andererseits in üblicher Weise beginnt. Diese Reaktion und Bildung des PUR ist exotherm und bewirkt, daß das Treibmittel verdampft und einen PUR-Schaumstoff mit besonders gleichmäßiger und damit günstiger Schaumstruktur bildet. Das verdampfende Treibmittel diffundiert während der Polymerisationsreaktion oder bei der bevorzugten kurzfristigen Lagerung nach Bildung des PUR-Schaumstoffproduktes durch die dünnen Zellwände ab und wird gegen die umgebende Luft ausgetauscht. Auf diese Weise können PUR-Schaumstoffe erzielt werden, die sofort nach der Herstellung und insbesondere nach kurzfristiger Lagerung die günstige und beim Einsatz als Baumaterial geforderte Brandklasse B2 haben.The process for making such foams is characterized in that on the one hand from a usual alcoholic component of the soft or in particular rigid polyurethane foams and on the other hand that at the starting temperature of the mixture at the applied pressure liquid organic blowing agent in the depending on the required amount of foaming, and with the addition of liquid phosphorus Flame retardants, possibly in a mixture with others Flame retardants such as solid phosphoric acid salts and possibly. with the addition of an emulsifier, except for the The usual isocyanate component to be used, an emulsion is formed so that there is a very even distribution of the blowing agent in the liquid state in the mixture, and then this emulsion with the isocyanate component in is usually mixed so that the chemical reaction between the diol or polyol on the one hand and the diol or Triisocyanate, on the other hand, begins in the usual way. These Reaction and formation of the PUR is exothermic and causes the blowing agent evaporates and a PUR foam with particularly uniform and therefore cheaper foam structure forms. The evaporating blowing agent diffuses during the Polymerization reaction or in the preferred short term storage after formation of the PUR foam product through the thin cell walls from time to time is exchanged for the surrounding air. In this way PUR foams can be obtained immediately after the Manufacture and especially after short-term storage inexpensive and required for use as a building material Fire class B2.

Der Nachteil der neuen Schaumstoffe besteht darin, daß die bei ihrer Herstellung als Brandschutzmittel eingesetzten flüssigen Phosphorsäureester eine beträchtliche Flüchtigkeit besitzen, so daß die hiermit hergestellten Schaumstoffe zwar anfangs, jedoch nicht über längere Zeit die guten Brandschutzwerte halten.The disadvantage of the new foams is that used as a fire protection agent in their manufacture liquid phosphoric acid esters have considerable volatility have so that the foams produced with it initially, but not for a long time the good ones  Keep fire protection values.

Aufgabe der vorliegenden Erfindung ist es, PUR-Schaumstoffe mit Hilfe des neuen Verfahrens gemäß dem Hauptpatent ... (Hauptpatentanmeldung P 39 33 705.7) herzustellen, die die anfangs guten Brandschutzwerte auch über längere Zeit, d. h. wie bei Baumaterial üblich über viele Jahre unverändert beibehalten.The object of the present invention is to provide PUR foams with the help of the new procedure according to the main patent ... (Main patent application P 39 33 705.7) to produce the initially good fire protection values over a longer period of time, d. H. unchanged over many years, as is usual with building materials maintained.

Die erfindungsgemäßen PUR-Schaumstoffe sind dadurch gekennzeichnet, daß sie wie die Schaumstoffe gemäß dem Hauptpatent ... (Hauptpatentanmeldung P 39 33 705.7) frei von FCKW oder anderen Halogenkohlenwasserstoffen sind und neben einem oder mehreren flüssigen Phosphorsäureestern als Brandschutzmittel Harnstoff, vorzugsweise in einer Menge von 10-20 Gew.-%, bezogen auf die Menge des oder der flüssigen Phosphorsäureester, ganz besonders als gesättigte Lösung von Harnstoff in diesem oder diesen flüssigen Phosphorsäureestern enthalten. Das Verfahren gemäß der vorliegenden Erfindung ist dadurch gekennzeichnet, daß gemäß dem Hauptpatent ... (Hauptpatentanmeldung P 39 33 705.7) das als Brandschutzmittel neben evtl. festen Brandschutzmitteln ein Gemisch aus dem oder den flüssigen Phosphorsäureestern und Harnstoff eingesetzt wird.The PUR foams according to the invention are thereby characterized that they like the foams according to the Main patent ... (main patent application P 39 33 705.7) free of CFCs or other halogenated hydrocarbons are and besides one or more liquid phosphoric acid esters as Fire retardant urea, preferably in an amount of 10-20 wt .-%, based on the amount of liquid or liquid Phosphoric acid esters, especially as a saturated solution of Urea in this or this liquid Contain phosphoric acid esters. The procedure according to the The present invention is characterized in that according to the main patent ... (main patent application P 39 33 705.7) the as a fire protection agent in addition to possibly solid fire protection agents a mixture of the liquid phosphoric acid esters and urea is used.

Auf diese Weise können die eingangs erzielten günstigen Brandschutzwerte dauerhaft erhalten werden.In this way, the low-cost can be achieved Fire protection values can be maintained permanently.

Die vorliegende Erfindung wird durch das folgende Beispiel erläutert: The present invention is illustrated by the following example explains:  

Beispielexample

Der PUR-Hartschaumstoff wurde wie folgt hergestellt:The rigid PUR foam was produced as follows:

Ein Gemisch ausA mixture of

50 GT eines Polyätheralkohols mit einer OH-Zahl von ca. 550 (Viskosität ca. 8000 cp bei 25°C) aus der Gruppe der CARADOL®-Produkte der Fa. Shell Chemie,
30 GT eines gesättigten Polyesters mit Quervernetzer mit einer OH-Zahl von ca- 500 (Viskosität ca. 8- 10 000 cp bei 25°C),
20 GT eines aromatischen Polyätheralkohols mit einer OH-Zahl von ca. 500 (Viskosität ca. 5000 bei 25°C),
8 GT einer gesättigten Lösung von Harnstoff in dem flüssigen Flammschutzmittel Dimethylmethylphosphonat (DMMP) mit 26% Phosphorgehalt, die 1,05 GT Harnstoff in 7 GT DMMP enthält,
5 GT des Emulgators EMULGIN® 550 der Fa. Henkel AG,
2 GT eines Silicons,
28 GT des festen Flammschutzmittels Ammoniumpolyphosphat,
3 GT eines Katalysators auf Basis eines Alkaliacetats,
18 GT n-Pentan50 pbw of a polyether alcohol with an OH number of approx. 550 (viscosity approx. 8000 cp at 25 ° C) from the group of CARADOL® products from Shell Chemie,
30 pbw of a saturated polyester with cross-linking agent with an OH number of approx. 500 (viscosity approx. 8-10,000 cp at 25 ° C.),
20 pbw of an aromatic polyether alcohol with an OH number of approx. 500 (viscosity approx. 5000 at 25 ° C),
8 pbw of a saturated solution of urea in the liquid flame retardant dimethyl methylphosphonate (DMMP) with 26% phosphorus content, which contains 1.05 pbw of urea in 7 pbw DMMP,
5 pbw of the emulsifier EMULGIN® 550 from Henkel AG,
2 pbw of a silicone,
28 pbw of the solid flame retardant ammonium polyphosphate,
3 pbw of a catalyst based on an alkali metal acetate,
18 GT n-pentane

wurde bei 22°C emulgiert. Der Emulsion wurden in für die Herstellung von PUR-Schaumstoffen üblicher Weise
172 Teile Diphenylmethan-4,4′-diisocyanat
zugemischt und die erhaltene Mischung wurde in einer üblichen Schäumanlage unter Normaldruck und bei Raumtemperatur geschäumt. Der erhaltene PUR-Schaumstoff wurde anschließend bei Raumtemperatur (20°C) und Normaldruck 4 Tage gelagert. was emulsified at 22 ° C. The emulsion was prepared in the usual way for the production of PUR foams
172 parts of diphenylmethane-4,4'-diisocyanate
admixed and the mixture obtained was foamed in a conventional foaming plant under normal pressure and at room temperature. The PUR foam obtained was then stored at room temperature (20 ° C.) and normal pressure for 4 days.

Der anfänglich erzielbare Brandschutzwert in Klasse B2 wurde, auch nach längerer Lagerung über mehrere Wochen, auch bei Erhitzen auf schwach erhöhte Temperatur gehalten.The initially achievable fire protection value in class B2 has been, even after long storage for several weeks kept at slightly elevated temperature when heated.

Claims (3)

1. Polyurethanschaumstoff gemäß Patent ... (Patentanmeldung P 39 33 705.7), dessen Zellen frei von Halogenkohlenwasserstoffen sind, ca. 80% Luft und eine geringe Menge des im Herstellungsverfahren eingesetzten niederen Kohlenwasserstoffs mit 3-6 Kohlenstoffatomen sowie ein flüssiges phosphorhaltiges Flammschutzmittel und ggfs. noch übliche Zusatzstoffe wie Katalysatoren, Stabilisatoren und/oder Emulgatoren enthält, dadurch gekennzeichnet, daß das flüssige phosphorhaltige Flammschutzmittel im Gemisch mit Harnstoff in einer Menge von 5-30 Gew.-%, bezogen auf das Gewicht des flüssigen phosphorhaltigen Flammschutzmittels eingesetzt wird.1. Polyurethane foam according to patent ... (patent application P 39 33 705.7), the cells of which are free of halogenated hydrocarbons, approx. 80% air and a small amount of the lower hydrocarbon with 3-6 carbon atoms used in the manufacturing process, as well as a liquid phosphorus-containing flame retardant and if necessary still contains conventional additives such as catalysts, stabilizers and / or emulsifiers, characterized in that the liquid phosphorus-containing flame retardant is used in a mixture with urea in an amount of 5-30% by weight, based on the weight of the liquid phosphorus-containing flame retardant. 2. Polyurethanschaumstoff nach Anspruch 1, dadurch gekennzeichnet, daß das eingesetzte flüssige phosphorhaltige Flammschutzmittel Harnstoff in einer Menge von 10-20 Gew.-%, bezogen auf das Gewicht des flüssigen phosphorhaltigen Flammschutzmittels, enthält.2. polyurethane foam according to claim 1, characterized in that the liquid phosphorus-containing flame retardants used Urea in an amount of 10-20% by weight, based on the weight of the liquid phosphorus Flame retardant. 3. Polyurethanschaumstoff nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das flüssige phosphorhaltige Flammschutzmittel Harnstoff bis zur Sättigung gelöst enthält.3. polyurethane foam according to claim 1 or 2, characterized in that the liquid phosphorus-containing flame retardants up to contains dissolved for saturation.
DE19904003718 1989-04-24 1990-02-08 Polyurethane foam prepn. Granted DE4003718A1 (en)

Priority Applications (21)

Application Number Priority Date Filing Date Title
DE19904003718 DE4003718A1 (en) 1990-02-08 1990-02-08 Polyurethane foam prepn.
DE59010789T DE59010789D1 (en) 1989-04-24 1990-04-12 Process for producing a halogen-free polyurethane insulating foam
EP90107041A EP0394769B1 (en) 1989-04-24 1990-04-12 Process for the preparation of a halocarbon-free polyurethane insulating foam
US07/635,152 US5182309A (en) 1989-04-24 1990-04-12 Polyurethane foam material free of halogenated hydrocarbons and process for producing the same
JP2505620A JPH0762090B2 (en) 1989-04-24 1990-04-12 Urethane foam material containing no halogenated hydrocarbon and method for producing the same
HU903726A HU210404B (en) 1989-04-24 1990-04-12 Process for producing polyurethane foam free of halogenated hydrocarbons
SU904894218A RU2058336C1 (en) 1989-04-24 1990-04-12 Polyurethane foam with volume weight not above 30 g/cm3 and a method of its producing
AU54065/90A AU638243B2 (en) 1989-04-24 1990-04-12 Polyurethane foam material free of halogenated hydrocarbons and process for producing the same
AT90107041T ATE161865T1 (en) 1989-04-24 1990-04-12 METHOD FOR PRODUCING A HALOGEN-FREE POLYURETHANE INSULATION FOAM
PCT/EP1990/000581 WO1990012841A1 (en) 1989-04-24 1990-04-12 Polyurethane foam material free of halogenated hydrocarbons and process for producing the same
CA002031218A CA2031218C (en) 1989-04-24 1990-04-12 Polyurethane foam material free of halogenated hydrocarbons and process for producing the same
PT93851A PT93851B (en) 1989-04-24 1990-04-23 PROCESS FOR THE PREPARATION OF POLYURETHANE FOAM MATERIALS FREE OF HALOGENATED HYDROCARBONS
SK2006-90A SK280709B6 (en) 1989-04-24 1990-04-23 Process for producing blown polyurethane insulating foam
CS902006A CZ284933B6 (en) 1989-04-24 1990-04-23 Process for producing polyurethane insulating foamy material
YU00816/90A YU81690A (en) 1989-04-24 1990-04-24 Polyurethanic foamy material without halogenic hydrocarbons, and process for obtaining thereof
PL90284914A PL164531B1 (en) 1989-04-24 1990-04-24 Non-chlorinated hydrocarbon containing, polyurethane foamed plastic and method for its manufacturing
TR42890A TR26440A (en) 1989-10-09 1990-05-07 HALOGEN HYDRO CARBONS THAT DO NOT CONTAIN POLYURETHANE FOAM MATERIAL AND A PROCESS FOR THE PRODUCTION OF IT
NO90905528A NO905528L (en) 1989-04-24 1990-12-20 POLYURETHANE FOAM MATERIAL FREE OF HYDROCARBONES AND PROCEDURES FOR PRODUCING THE SAME.
HRP920980AA HRP920980A2 (en) 1989-04-24 1992-10-02 Process for producing polyurethane foam free of halogenated hydrocarbons
LVP-93-33A LV10470B (en) 1989-04-24 1993-01-15 Polyurethane foam and process for producing therof
GEAP19931455A GEP19970640B (en) 1989-04-24 1993-08-17 Polyurethane Foam Material and Method for Production thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19904003718 DE4003718A1 (en) 1990-02-08 1990-02-08 Polyurethane foam prepn.

Publications (2)

Publication Number Publication Date
DE4003718A1 true DE4003718A1 (en) 1991-08-14
DE4003718C2 DE4003718C2 (en) 1993-09-09

Family

ID=6399658

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19904003718 Granted DE4003718A1 (en) 1989-04-24 1990-02-08 Polyurethane foam prepn.

Country Status (1)

Country Link
DE (1) DE4003718A1 (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3835193A1 (en) * 1988-10-15 1990-04-19 Basf Ag METHOD FOR THE PRODUCTION OF MOLDED BODIES WITH A COMPRESSED EDGE AND CELLULAR CORE, PREFERABLY SHOULDER HEADS

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3835193A1 (en) * 1988-10-15 1990-04-19 Basf Ag METHOD FOR THE PRODUCTION OF MOLDED BODIES WITH A COMPRESSED EDGE AND CELLULAR CORE, PREFERABLY SHOULDER HEADS

Also Published As

Publication number Publication date
DE4003718C2 (en) 1993-09-09

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