EP1034225A1 - Intumescent flame-retardant coatings - Google Patents

Intumescent flame-retardant coatings

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Publication number
EP1034225A1
EP1034225A1 EP98961186A EP98961186A EP1034225A1 EP 1034225 A1 EP1034225 A1 EP 1034225A1 EP 98961186 A EP98961186 A EP 98961186A EP 98961186 A EP98961186 A EP 98961186A EP 1034225 A1 EP1034225 A1 EP 1034225A1
Authority
EP
European Patent Office
Prior art keywords
weight
phosphoric acid
flame
intumescent
parts
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.)
Withdrawn
Application number
EP98961186A
Other languages
German (de)
French (fr)
Inventor
Bernd Pomrehn
Guido Arnsmann
Wolf-Dieter Pirig
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.)
Clariant Produkte Deutschland GmbH
Original Assignee
Clariant GmbH
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
Application filed by Clariant GmbH filed Critical Clariant GmbH
Publication of EP1034225A1 publication Critical patent/EP1034225A1/en
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
    • C09D161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C09D161/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
    • C09D161/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C09D5/185—Intumescent paints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
    • C09D161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C09D161/22—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
    • C09D161/24—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with urea or thiourea
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic

Definitions

  • the invention relates to intumescent, flame-retardant coating compositions and their use
  • Flame-retardant coating compositions based on solvent-containing binders which contain chlorine paraffms as the flame-retardant component are known (Bhatnagar and Vergnaud in "Fire Safety Journal” 4 (3), 163-7 and "Paintindia” 32 (1) 3-6, 14, 1982 )
  • Inflatable coating compositions are known from US Pat. No. 4,166,743, which consist of a film former, an ammonium polyphosphate, at least one substance that carbonizes when exposed to heat, a dispersant, a salt containing water of crystallization, a blowing agent and, if appropriate, fillers.
  • aqueous dispersions of polyvinyl acetate or a copolymer of vinyl acetate u ⁇ d ⁇ dibutyl maleate are used as substance which is carbonized during dicyandiamide, pentaerythritol or melamine
  • Suitable dispersing agents in addition to water ethyl acetate, butyl acetate, xylene or toluene in question come, while as Blowing agents chlorinated paraffins are used
  • DE 43 43 668 A1 describes inflatable, flame-retardant coating compositions which consist of a film-forming binder, ammonium polyphosphate, at least one substance which carbonizes when exposed to heat, a blowing agent and, if appropriate, dispersants and fillers
  • phosphoric acid partial esters based on polyols can only be prepared on a large scale on a large industrial scale and are therefore not available in large quantities.
  • the present systems can only achieve service lives in the minute range.
  • EP 0 417 490 B1 describes phosphoric acid esters and their salts, lacquers and molding compositions containing them, the use of these phosphoric acid esters and their salts as dispersants and the solids coated with them
  • the object of the present invention is therefore to provide intumescent coating compositions which are halogen-free and have a sufficient service life and form cured products without the addition of further (hard) substances
  • the intumescent, flame-retardant coating compositions preferably contain 50 to 90 parts by weight of an aqueous synthetic resin dispersion, 20 to 60 parts by weight of a mixture of at least two different phosphoric acid partial esters and 1 to 80 parts by weight of further ingredients
  • a mixture of 3 different phosphoric acid partial esters is preferably contained.
  • a mixture of 4 different phosphoric acid partial esters is particularly preferably contained
  • the intumescent, flame-retardant coating composition consists of a) a mixture of a phosphoric acid monoalkyl ester and a phosphoric acid dialkyl ester with the same alkyl group and b) a mixture of a phosphoric acid monoalkyl ester and a phosphoric acid dialkyl ester with the same but different a) alkyl group
  • the phosphoric acid partial esters are preferably phosphoric acid monomethyl ester, phosphoric acid monoethyl ester, phosphoric acid monopropyl ester, phosphoric acid monoisopropyl ester, phosphoric acid monobutyl ester, phosphoric acid monoisobutyl ester, phosphoric acid monopentyl ester, phosphoric acid monoisopentyl ester, phosphoric acid monoisopentyl ester, hexyl ester, phosphoric acid monooctyl ester, phosphoric acid mono (2-ethylhexyl) ester, phosphoric acid monoethylene glycol ester, phosphoric acid dimethyl ester, phosphoric acid diethyl ester,
  • Phosphoric acid dioctyl ester Phosphoric acid dioctyl ester, phosphoric acid di (2-ethylhexyl) ester and / or phosphoric acid diethylene glycol ester and mixtures thereof
  • the aqueous synthetic resin dispersion is preferably a nitrogenous synthetic resin dispersion
  • the aqueous synthetic resin dispersion is preferably a melamine and / or urea-formaldehyde resin
  • the aqueous synthetic resin dispersion is particularly preferably an etherified melamine and / or urea-formaldehyde resin
  • the aforementioned melamine resins used according to the invention are usually reaction products of melamine with formaldehyde in a molar ratio of 1 1 to 1 6 (melamine formaldehyde)
  • the melamine-formaldehyde resins can also be etherified with alcohols, chain length 1-20 C-atoms, preferably 1-4 C-atoms
  • the further ingredients are preferably dispersants, fillers, hardeners, thixotropic agents, plasticizers, acid donors, further flame retardants, surface auxiliaries and / or binders
  • Colorants in the sense of the invention are understood to be those as mentioned, for example, in Rompp's Chemie Lexikon, 9th edition 1992, page 1237. These include inorganic and organic, natural and synthetic colorants, m AW pigments and dyes
  • the intumescent flame-retardant coating compositions according to the invention are usually clear (transparent).
  • the coating compositions can also be made cloudy. It is also possible, by choosing a suitable colorant, in particular the inorganic pigments, to produce, when dry, colored, preferred white intumescent, flame-retardant coating compositions
  • the other ingredients are particularly preferably thixotropic agents and / or fillers
  • the phosphoric acid partial esters are preferably those of the formula
  • R 1 and R 2 are the same or different and H, CH 3 , C 2 H 3 , C 3 H 7 , C ⁇ Ho, C 5 Hn, C ⁇ H 13 , C 8 Hi 6 and / or CH 2 -CH 2 -OH mean, and R 1 and R 2 are not simultaneously hydrogen
  • the mixture according to the invention of at least two different phosphoric acid partial esters usually consists of 2 to 98% by weight of a phosphoric acid partial ester and 98 to 2% by weight of a different phosphoric acid partial ester
  • the ratios are usually (2 to 98) (4 to 96) • (4 to 96)% by weight
  • the ratio of mixture a) to mixture b) is (98 to 2) (2 to 98)% by weight and preferably (10 to 90) (90 to 10)% by weight for the mixture within a) or b) is the ratio of phosphoric acid monoalkyl ester to phosphoric acid dialkyl ester (2 to 98) (98 to 2)% by weight, preferably (10 to 90) (90 to 10)% by weight
  • dispersants for solids are phosphoric acid monopolyethylene glycol alkyl esters, phosphoric acid monopolyethylene glycol aryl esters, phosphoric acid dipoly- thylenglycolalkylester and / or phosphoric acid dipolyethylenglycolarylester and mixtures thereof are used
  • the phosphorus content of the intumescent, flame-retardant coating compositions is 1 to 15% by weight.
  • the phosphorus content of the intumescent, flame-retardant coating compositions is preferably 4 to 10% by weight after curing.
  • the invention also relates to the use of the coating compositions according to the invention for the production of coatings on objects made of wood, plastics, building materials, cellulose materials, rubber and metal and for the impregnation of textiles and leather.
  • ®Maprenal MF 920 (Vianova Resins) is a non-plasticized, methyl etherified melamine-formaldehyde resin.
  • ®Maprenal VMF 3921 w (Vianova Resins) is a non-plasticized methyl etherified melamine-formaldehyde resin
  • the coating compositions obtained according to the following examples are clear, smooth and free of cracks.
  • the service life is on average more than 24 hours. After less than 24 hours (on average), the coating composition applied is tack-free and hard. In fire tests of these recipes on pine wood and chipboard, Bl and B2 reached
  • intumescent flame-retardant coating composition according to the invention can be found in Tables 1 to 11. All the formulations were achieved in the fire test B1 or B2. Table 1 :
  • MDIP means: Mixture of 85% by weight ®Knapsack phosphorus85: 15 acidic MDE and 15% by weight ⁇ Knapsack phosphoric acid ester MDIP. This notation applies accordingly to the following tables.
  • Example 50 ®CAB-O-SIL TS 530 (CABOT, Hanau) was used as the highly disperse silica. Also successfully used was ⁇ Aerosil OX-50 (pyrogenic silica from Degussa AG). Example 50
  • the coating compositions obtained according to Examples 67 and 68 are smooth, white and free of cracks.

Abstract

The invention relates to intumescent flame-retardant coatings, containing 10 to 150 parts by weight of an aqueous artificial resin dispersion and 10 to 80 parts by weight of a mixture of at least two different phosphoric acid partial esters.

Description

Intumeszierende, flammhemmende Überzugsmassen Intumescent, flame-retardant coating compounds
Die Erfindung betrifft intumeszierende, flammhemmende Überzugsmassen und ihre VerwendungThe invention relates to intumescent, flame-retardant coating compositions and their use
Bekannt sind flammwidrige Überzugsmassen auf der Basis von losemittelhaltigen Bindemitteln, die als flammwidrige Komponente Chlorparaffme enthalten (Bhatnagar und Vergnaud in „Fire Safety Journal" 4(3), 163-7 und „Paintindia" 32 (1) 3-6, 14, 1982)Flame-retardant coating compositions based on solvent-containing binders which contain chlorine paraffms as the flame-retardant component are known (Bhatnagar and Vergnaud in "Fire Safety Journal" 4 (3), 163-7 and "Paintindia" 32 (1) 3-6, 14, 1982 )
Nachteil dieser Systeme ist, daß wahrend der Trocknung Losungsmitteldampfe abgegeben werden, und im Brandfall korrosive und toxische halogenhaltige Brandgase freigesetzt werdenThe disadvantage of these systems is that solvent vapors are released during the drying process and that corrosive and toxic halogen-containing combustion gases are released in the event of a fire
Aus der US-PS 4 166 743 sind aufblahbare Überzugsmassen bekannt, welche aus einem Filmbildner, einem Ammoniumpolyphosphat, mindestens einer bei Hitzeeinwirkung carbo- nisierenden Substanz, einem Dispergiermittel, einem Kristallwasser aufweisenden Salz, einem Treibmittel und gegebenenfalls Füllstoffen bestehen. Dabei können als Filmbildner wäßrige Dispersionen aus Polyvinylacetat oder aus einem Copolymerisat aus Vinylacetat uπd~Dibutylmaleinat verwendet werden, wahrend als carbonisierende Substanz Dicyandia- mid, Pentaerythrit oder Melamin geeignet sind Als Dispergiermittel kommen neben Wasser Ethylacetat, Butylacetat, Xylol oder Toluol in Frage, wahrend als Treibmittel Chlorparaffine Verwendung findenInflatable coating compositions are known from US Pat. No. 4,166,743, which consist of a film former, an ammonium polyphosphate, at least one substance that carbonizes when exposed to heat, a dispersant, a salt containing water of crystallization, a blowing agent and, if appropriate, fillers. Are as film formers, aqueous dispersions of polyvinyl acetate or a copolymer of vinyl acetate uπd ~ dibutyl maleate are used as substance which is carbonized during dicyandiamide, pentaerythritol or melamine Suitable dispersing agents in addition to water ethyl acetate, butyl acetate, xylene or toluene in question come, while as Blowing agents chlorinated paraffins are used
Nach Troitzsch („International Plastics Flammability Handbook", 2 Auflage, Oxford U i- versity Press, New York, 1990, Seiten 52 und 53) sind typische Vertreter für carbonisierende Substanzen Pentaerythrit und Starke, wahrend Guanidine, Melamin und Chlorparaffi- ne den Treibmitteln zuzuordnen sind Nachteilig ist bei den vorgenannten aufblahbaren Überzugsmassen, daß sie im Treibmittel und/oder in der bei Hitzeeinwirkung carbonisierenden Substanz organisch gebundenes Halogen enthalten, wodurch bei der Zersetzung der Überzugsmassen korrosive und toxische Gase freigesetzt werdenAccording to Troitzsch ("International Plastics Flammability Handbook", 2nd edition, Oxford University Press, New York, 1990, pages 52 and 53), typical representatives of carbonizing substances are pentaerythritol and starch, while guanidines, melamine and chlorinated paraffins are the blowing agents are to be assigned A disadvantage of the abovementioned inflatable coating compositions is that they contain organically bound halogen in the blowing agent and / or in the substance which carbonizes when exposed to heat, as a result of which corrosive and toxic gases are released during the decomposition of the coating compositions
Weiterhin beschreibt die DE 43 43 668 AI aufblahbare, flammhemmende Überzugsmassen, welche aus einem filmbildenden Bindemittel, Ammoniumpolyphosphat, mindestens einer bei Hitzeeinwirkung carbonisierenden Substanz, einem Treibmittel und ggf Dispergiermittel und Füllstoffen bestehenFurthermore, DE 43 43 668 A1 describes inflatable, flame-retardant coating compositions which consist of a film-forming binder, ammonium polyphosphate, at least one substance which carbonizes when exposed to heat, a blowing agent and, if appropriate, dispersants and fillers
Die DE 43 43 669 AI beschreibt ahnlich zusammengesetzte aufblahbare, flammhemmende Überzugsmassen, die jedoch kein Ammoniumpolyphosphat enthaltenDE 43 43 669 AI describes similarly inflatable, flame-retardant coating compositions which, however, do not contain ammonium polyphosphate
Mit den vorliegenden Systemen werden jedoch nur kurze, nicht ausreichende Standzeiten erreichtWith the present systems, however, only short, inadequate service lives are achieved
Vorgeschlagen wurden auch wasserbasierende, flammwidrige Überzugsmassen, in denen Phosphorsaurepartialester auf der Basis von Polyolen als Saurespender und carbomsierende Substanzen wirken (EP 0 556 350 Bl)Water-based, flame-retardant coating compositions in which phosphoric acid partial esters based on polyols act as acid donors and carbomizing substances were also proposed (EP 0 556 350 B1)
Der Nachteil hierbei ist, daß Phosphorsaurepartialester auf der Basis von Polyolen großtechnisch nur sehr aufwendig herzustellen sind und somit in größeren Mengen nicht zur Verfügung stehen Darüber hinaus sind mit den vorliegenden Systemen nur Standzeiten im Minutenbereich zu erreichen.The disadvantage here is that phosphoric acid partial esters based on polyols can only be prepared on a large scale on a large industrial scale and are therefore not available in large quantities. In addition, the present systems can only achieve service lives in the minute range.
Schließlich beschreibt die EP 0 417 490 Bl Phosphorsaureester und deren Salze, diese enthaltenden Lacke und Formmassen, die Verwendung dieser Phosphorsaureester und deren Salze als Dispergiermittel und die damit beschichteten FeststoffeFinally, EP 0 417 490 B1 describes phosphoric acid esters and their salts, lacquers and molding compositions containing them, the use of these phosphoric acid esters and their salts as dispersants and the solids coated with them
Insgesamt ergeben sich aus dem Stand der Technik entweder Formulierungen, die halogen- haltig sind und somit im Brandfall toxische und korrosive Gase freisetzen Bei den halogenfreien Systemen sind die Standzeiten sehr kurz und es wird teilweise keine ausreichende Härtung der Produkte erreicht Bei einigen Systemen bestehen auch Probleme bei der technischen Herstellung, bei anderen ist die Anwendungsbreite geringOverall, the state of the art either results in formulations containing halogen and thus releasing toxic and corrosive gases in the event of fire. In the case of halogen-free systems, the service life is very short and in some cases insufficient Hardening of the products achieved In some systems there are also problems with the technical production, in others the range of applications is small
Der vorliegenden Erfindung liegt daher die Aufgabe zugrunde, intumeszierende Überzugsmassen zur Verfügung zu stellen, die halogenfrei sind und ausreichende Standzeiten zeigen sowie ausgehartete Produkte ohne Zugabe weiterer (Harter)Substanzen bildenThe object of the present invention is therefore to provide intumescent coating compositions which are halogen-free and have a sufficient service life and form cured products without the addition of further (hard) substances
Diese Aufgabe wird gelost durch intumeszierende, flammhemmende Überzugsmassen der eingangs beschriebenen Art, enthaltendThis object is achieved by containing intumescent, flame-retardant coating compositions of the type described above
10 bis 150 Gewichtsteile einer wäßrigen Kunstharzdispersion und 10 bis 80 Gewichtsteile einer Mischung aus mindestens zwei verschiedenen Phosphorsäurepartialestem10 to 150 parts by weight of an aqueous synthetic resin dispersion and 10 to 80 parts by weight of a mixture of at least two different phosphoric acid partial esters
Bevorzugt enthalten die intumeszierenden, flammhemmenden Überzugsmassen 50 bis 90 Gewichtsteile einer wäßrigen Kunstharzdispersion, 20 bis 60 Gewichtsteile einer Mischung aus mindestens zwei verschiedenen Phosphorsäurepartialestem und 1 bis 80 Gewichtsteile weitere InhaltsstoffeThe intumescent, flame-retardant coating compositions preferably contain 50 to 90 parts by weight of an aqueous synthetic resin dispersion, 20 to 60 parts by weight of a mixture of at least two different phosphoric acid partial esters and 1 to 80 parts by weight of further ingredients
Bevorzugt ist eine Mischung aus 3 verschiedenen Phosphorsäurepartialestem enthalten.A mixture of 3 different phosphoric acid partial esters is preferably contained.
Besonders bevorzugt ist eine Mischung aus 4 verschiedenen Phosphorsäurepartialestem enthaltenA mixture of 4 different phosphoric acid partial esters is particularly preferably contained
Insbesondere besteht die intumeszierende, flammhemmende Überzugsmasse aus a) einer Mischung aus einem Phosphorsauremonoalkylester und einem Phosphorsauredial- kylester mit gleicher Alkylgruppe und b) einer Mischung aus einem Phosphorsauremonoalkylester und einem Phosphorsauredi- alkylester mit gleicher, aber zu a) unterschiedlicher AlkylgruppeIn particular, the intumescent, flame-retardant coating composition consists of a) a mixture of a phosphoric acid monoalkyl ester and a phosphoric acid dialkyl ester with the same alkyl group and b) a mixture of a phosphoric acid monoalkyl ester and a phosphoric acid dialkyl ester with the same but different a) alkyl group
Bevorzugt handelt es sich bei den Phosphorsäurepartialestem um Phosphorsauremonome- thylester, Phosphorsauremonoethylester, Phosphorsauremonopropylester, Phosphorsaure- monoisopropylester, Phosphorsauremonobutylester, Phosphorsauremonoisobutylester, Phosphorsauremonopentylester, Phosphorsauremonoisopentylester, Phosphorsauremono- hexylester, Phosphorsauremonooctylester, Phosphorsauremono(2-ethylhexyl)ester, Phos- phorsauremonoethylenglycolester, Phosphorsauredimethylester, Phosphorsäurediethylester,The phosphoric acid partial esters are preferably phosphoric acid monomethyl ester, phosphoric acid monoethyl ester, phosphoric acid monopropyl ester, phosphoric acid monoisopropyl ester, phosphoric acid monobutyl ester, phosphoric acid monoisobutyl ester, phosphoric acid monopentyl ester, phosphoric acid monoisopentyl ester, phosphoric acid monoisopentyl ester, hexyl ester, phosphoric acid monooctyl ester, phosphoric acid mono (2-ethylhexyl) ester, phosphoric acid monoethylene glycol ester, phosphoric acid dimethyl ester, phosphoric acid diethyl ester,
Phosphorsauredipropylester, Phosphorsaurediisopropylester, Phosphorsauredibutylester,Phosphoric acid dipropyl ester, phosphoric acid diisopropyl ester, phosphoric acid dibutyl ester,
Phosphorsaurediisobutylester, Phosphorsauredipentylester, Phosphorsauredihexylester,Phosphoric acid diisobutyl ester, phosphoric acid dipentyl ester, phosphoric acid dihexyl ester,
Phosphorsauredioctylester, Phosphorsäuredi(2-ethylhexyl)ester und/oder Phosphorsaure- diethylenglycolester und Gemische derselbenPhosphoric acid dioctyl ester, phosphoric acid di (2-ethylhexyl) ester and / or phosphoric acid diethylene glycol ester and mixtures thereof
Bevorzugt handelt es sich bei der wäßrigen Kunstharzdispersion um eine stickstoffhaltige KunstharzdispersionThe aqueous synthetic resin dispersion is preferably a nitrogenous synthetic resin dispersion
Bevorzugt handelt es sich bei der wäßrigen Kunstharzdispersion um ein Melamin- und/oder Harnstoff-Formaldehyd-HarzThe aqueous synthetic resin dispersion is preferably a melamine and / or urea-formaldehyde resin
Besonders bevorzugt handelt es sich bei der wäßrigen Kunstharzdispersion um ein verether- tes Melamin- und/oder Harnstoff-Formaldehyd-HarzThe aqueous synthetic resin dispersion is particularly preferably an etherified melamine and / or urea-formaldehyde resin
Die vorgenannten erfindungsgemaß verwendeten Melaminharze sind üblicherweise Umsetzungsprodukte von Melamin mit Formaldehyd in einem Molverhaltnis von 1 1 bis 1 6 (Melamin Formaldehyd)The aforementioned melamine resins used according to the invention are usually reaction products of melamine with formaldehyde in a molar ratio of 1 1 to 1 6 (melamine formaldehyde)
Die Melamin-Formaldehyd-Harze können auch mit Alkoholen, Kettenlange 1-20 C- Atome, bevorzugt 1-4 C-Atome, verethert seinThe melamine-formaldehyde resins can also be etherified with alcohols, chain length 1-20 C-atoms, preferably 1-4 C-atoms
Bevorzugt handelt es sich bei den weiteren Inhaltsstoffen um Dispergiermittel, Füllstoffe, Harter, Thixotropierungsmittel, Weichmacher, Saurespender, weitere Flammschutzmittel, Oberflachenhilfsmittel und/oder BinderThe further ingredients are preferably dispersants, fillers, hardeners, thixotropic agents, plasticizers, acid donors, further flame retardants, surface auxiliaries and / or binders
Unter Farbmittel im Sinne der Erfindung sind solche zu verstehen, wie sie beispielsweise in Rompp's Chemie Lexikon, 9. Auflage 1992, Seite 1237 genannt sind Hierunter fallen anorganische und organische, naturliche und synthetische Farbmittel, m a W Pigmente und FarbstoffeColorants in the sense of the invention are understood to be those as mentioned, for example, in Rompp's Chemie Lexikon, 9th edition 1992, page 1237. These include inorganic and organic, natural and synthetic colorants, m AW pigments and dyes
Ohne den Einsatz von Farbmitteln sind die erfindungsgemäßen, intumeszierenden flammhemmenden Überzugsmassen üblicherweise klar (transparent). Durch Zugabe von Fullstof- fen, insbesondere Talkum und andere lassen sich die Überzugsmassen auch trüb einstellen Ebenso ist es möglich, durch Wahl eines geeigneten Farbmittels, insbesondere den anorganischen Pigmenten, im Trockenzustand gefärbte, bevorzugte weiße intumeszierende, flammhemmende Überzugsmassen herzustellenWithout the use of colorants, the intumescent flame-retardant coating compositions according to the invention are usually clear (transparent). By adding filler fen, in particular talc and others, the coating compositions can also be made cloudy. It is also possible, by choosing a suitable colorant, in particular the inorganic pigments, to produce, when dry, colored, preferred white intumescent, flame-retardant coating compositions
Besonders bevorzugt handelt es sich bei den weiteren Inhaltsstoffen um Thixotrophie- rungsmittel und/oder FüllstoffeThe other ingredients are particularly preferably thixotropic agents and / or fillers
Bevorzugt handelt es sich bei den Phosphorsäurepartialestem um solche der FormelThe phosphoric acid partial esters are preferably those of the formula
in der R1 und R2 gleich oder verschieden sind und H, CH3, C2H3, C3H7, CψHo, C5Hn, CβH13, C8Hi6 und/oder CH2-CH2-OH bedeuten, und R1 und R2 nicht gleichzeitig Wasserstoff sind in which R 1 and R 2 are the same or different and H, CH 3 , C 2 H 3 , C 3 H 7 , CψHo, C 5 Hn, CβH 13 , C 8 Hi 6 and / or CH 2 -CH 2 -OH mean, and R 1 and R 2 are not simultaneously hydrogen
Die erfindungsgemaße Mischung von mindestens zwei verschiedenen Phosphorsäurepartialestem besteht üblicherweise aus 2 bis 98 Gew -% eines Phosphorsaurepartialesters und 98 bis 2 Gew -% eines hiervon unterschiedlichen PhosphorsaurepartialestersThe mixture according to the invention of at least two different phosphoric acid partial esters usually consists of 2 to 98% by weight of a phosphoric acid partial ester and 98 to 2% by weight of a different phosphoric acid partial ester
Bevorzugt werden 10 bis 90 Gew -% des einen und 90 bis 10 Gew -% des anderen Phosphorsaurepartialesters eingesetzt10 to 90% by weight of one and 90 to 10% by weight of the other phosphoric acid partial ester are preferably used
Bei den Mischungen aus 3 verschiedenen Phosphorsäurepartialestem betragen die Verhaltnisse üblicherweise (2 bis 98) (4 bis 96) • (4 bis 96) Gew -%For the mixtures of 3 different phosphoric acid partial esters, the ratios are usually (2 to 98) (4 to 96) • (4 to 96)% by weight
Bei den Mischungen aus 4 verschiedenen Phosphorsäurepartialestem betragt das Verhältnis von Mischung a) zu Mischung b) (98 bis 2) (2 bis 98) Gew -% und bevorzugt (10 bis 90) (90 bis 10) Gew -% Für die Mischung innerhalb a) bzw b) ist das Verhältnis Phosphorsauremonoalkylester zu Phosphorsauredialkylester (2 bis 98) (98 bis 2) Gew -%, bevorzugt (10 bis 90) (90 bis 10) Gew.-%In the case of the mixtures of 4 different phosphoric acid partial esters, the ratio of mixture a) to mixture b) is (98 to 2) (2 to 98)% by weight and preferably (10 to 90) (90 to 10)% by weight for the mixture within a) or b) is the ratio of phosphoric acid monoalkyl ester to phosphoric acid dialkyl ester (2 to 98) (98 to 2)% by weight, preferably (10 to 90) (90 to 10)% by weight
Als Dispergiermittel für Feststoffe können beispielweise Phosphorsauremonopolyethy- lenglycolalkylester, Phosphorsauremonopolyethylenglycolarylester, Phosphorsauredipolye- thylenglycolalkylester und/oder Phosphorsauredipolyethylenglycolarylester und Gemische derselben eingesetzt werdenExamples of dispersants for solids are phosphoric acid monopolyethylene glycol alkyl esters, phosphoric acid monopolyethylene glycol aryl esters, phosphoric acid dipoly- thylenglycolalkylester and / or phosphoric acid dipolyethylenglycolarylester and mixtures thereof are used
Der Phosphorgehalt der intumeszierenden, flammhemmenden Überzugsmassen betragt nach der Aushärtung 1 bis 15 Gew -%After curing, the phosphorus content of the intumescent, flame-retardant coating compositions is 1 to 15% by weight.
Bevorzugt betragt der Phosphorgehalt der intumeszierenden, flammhemmenden Überzugsmassen betragt nach der Aushärtung 4 bis 10 Gew -%The phosphorus content of the intumescent, flame-retardant coating compositions is preferably 4 to 10% by weight after curing.
Die Erfindung betrifft auch die Verwendung der erfindungsgemäßen Überzugsmassen zur Herstellung von Beschichtungen auf Gegenständen aus Holz, Kunststoffen, Baustoffen, Cellulosematerialien, Gummi und Metall und zur Imprägnierung von Textilien und Ledern.The invention also relates to the use of the coating compositions according to the invention for the production of coatings on objects made of wood, plastics, building materials, cellulose materials, rubber and metal and for the impregnation of textiles and leather.
Die Erfindung wird durch die nachstehenden Beispiele erläutert, bei denen die folgenden Substanzen verwendet wurdenThe invention is illustrated by the following examples, in which the following substances were used
©Maprenal MF 920© Maprenal MF 920
Bei ®Maprenal MF 920 (Vianova Resins) handelt es sich um ein nichtplastifiziertes, me- thylverethertes Melamin-Formaldehyd-Harz.®Maprenal MF 920 (Vianova Resins) is a non-plasticized, methyl etherified melamine-formaldehyde resin.
®Maprenal VMF 3921 w®Maprenal VMF 3921 w
Bei ®Maprenal VMF 3921 w (Vianova Resins) handelt es sich um ein nichtplastifiziertes methyl-verethertes Melamin-Formaldehyd-Harz®Maprenal VMF 3921 w (Vianova Resins) is a non-plasticized methyl etherified melamine-formaldehyde resin
® Plastopal BTW® Plastopal BTW
Es handelt sich um ein elastisches, urethangruppenhaltiges, methanolverethertes Harnstoff- Formaldehyd-Harz (Hersteller: BASF).It is an elastic urethane group-containing, methanol-etherified urea-formaldehyde resin (manufacturer: BASF).
®Knapsack Phosphorsaureester MDE®Knapsack phosphoric acid ester MDE
Es handelt sich um eine Mischung aus einem Phosphorsauremonoethylester und einemIt is a mixture of a phosphoric acid monoethyl ester and one
Phosphorsäurediethylester ®Knapsack Phosphorsaureester MDIPPhosphoric acid diethyl ester ®Knapsack phosphoric acid ester MDIP
Es handelt sich um eine Mischung aus einem Phosphorsauremonoisopropylester und einemIt is a mixture of a phosphoric acid monoisopropyl ester and one
PhosphorsaurediisopropylesterPhosphoric acid diisopropyl ester
©Knapsack Phosphorsaureester 122© Knapsack phosphoric acid ester 122
Es handelt sich um eine Mischung aus einem Phosphorsauremonopolyethylenglycolalkyl- ester und einem Phosphorsauredipolyethylenglycolalkylester (Dispergiermittel)It is a mixture of a phosphoric acid monopolyethylene glycol alkyl ester and a phosphoric acid dipolyethylene glycol alkyl ester (dispersant)
©Knapsack Reinigerkomponente MIS© Knapsack cleaner component MIS
Es handelt sich um eine Mischung aus Phosphorsauremonoisopropylester, Phosphorsaure- monomethylester und Phosphorsaure.It is a mixture of phosphoric acid monoisopropyl ester, phosphoric acid monomethyl ester and phosphoric acid.
®Knapsack Phosphorsaureester MOE®Knapsack phosphoric acid ester MOE
Es handelt sich um eine Mischung aus Monoethylphosphorsaureester und PhosphorsaureIt is a mixture of monoethyl phosphoric acid ester and phosphoric acid
®Knapsack Reinigerkomponente MS®Knapsack cleaner component MS
Es handelt sich um MonomethylphosphorsäureesterIt is monomethylphosphoric acid ester
©Knapsack Phosphorsaureester MDB© Knapsack phosphoric acid ester MDB
Es handelt sich um eine Mischung aus Monobutyl- und DibutylphosphorsaureesterIt is a mixture of monobutyl and dibutyl phosphoric acid esters
Die vorgenannten Handelsprodukte ©Knapsack Phosphorsaureester bzw. ®Knapsack Reinigerkomponente werden von der Clariant GmbH, Werk Knapsack hergestelltThe above-mentioned commercial products © Knapsack phosphoric acid ester or ®Knapsack cleaner component are manufactured by Clariant GmbH, Knapsack plant
®Mistrofil 500®Mistrofil 500
Es handelt sich um ein handelsübliches Talkum.It is a commercially available talc.
®Aerosil R 816®Aerosil R 816
Es handelt sich um pyrogene Kieselsaure der Fa Degussa AG. Die verschiedenen Komponenten wurden in der in den Beispielen angegebenen Reihenfolge miteinander vermischt, auf Kiefernholz bzw Spanplatte aufgetragen, getrocknet und ihr Intumeszenzverhalten bestimmt Die Reihenfolge der Auftragung der Komponenten kann beliebig erfolgen, dies hängt von der gewünschten Schichtdicke und anderen Bedingungen (Viskosität, Untergrund, Standzeit etc ) abIt is pyrogenic silica from Degussa AG. The various components were mixed together in the order given in the examples, applied to pine wood or chipboard, dried and their intumescence behavior determined. The order in which the components are applied can be as desired, depending on the desired layer thickness and other conditions (viscosity, substrate, service life) etc)
Weitere Substanzen sind ggf. in den jeweiligen Beispielen erklartFurther substances are possibly explained in the respective examples
Die gemäß den nachfolgenden Beispielen erhaltenen Überzugsmassen sind klar, glatt und rißfrei Die Standzeit betragt im Mittel mehr als 24 Stunden Nach weniger als 24 Stunden (im Mittel) ist die applizierte Überzugsmasse klebfrei und hart In Brandprufungen dieser Rezepturen auf Kiefernholz und Spanplatte wurden Bl und B2 erreichtThe coating compositions obtained according to the following examples are clear, smooth and free of cracks. The service life is on average more than 24 hours. After less than 24 hours (on average), the coating composition applied is tack-free and hard. In fire tests of these recipes on pine wood and chipboard, Bl and B2 reached
Beispiel 1example 1
68 Gewichtsteile ®Maprenal MF 92068 parts by weight ®Maprenal MF 920
25 Gewichtsteile einer Mischung aus 90 Gew -% ©Knapsack Phosphorsaureester MOE und 10 Gew -% ©Knapsack Reinigerkomponente MS25 parts by weight of a mixture of 90% by weight © Knapsack phosphoric acid ester MOE and 10% by weight © Knapsack cleaner component MS
Beispiel 2Example 2
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24.8 Gewichtstelle einer Mischung aus 80 Gew -% ©Knapsack Phosphorsaureester MOE und 20 Gew -% ©Knapsack Reinigerkomponente MS24.8 Weight point of a mixture of 80% by weight © Knapsack phosphoric acid ester MOE and 20% by weight © Knapsack cleaner component MS
Beispiel 3Example 3
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24.9 Gewichtsteile einer Mischung aus 70 Gew -% ©Knapsack Phosphorsaureester MOE und 30 Gew -% ©Knapsack Reinigerkomponente MS24.9 parts by weight of a mixture of 70% by weight © Knapsack phosphoric acid ester MOE and 30% by weight © Knapsack cleaner component MS
Eine Wiederholung der Beispiele 1 bis 3 mit 60 Gewichtsteile ©Maprenal VMF 3921 w anstatt 68 Gewichtsteile ©Maprenal MF 920 lieferte analoge Ergebnisse Beispiel 4A repetition of Examples 1 to 3 with 60 parts by weight © Maprenal VMF 3921 w instead of 68 parts by weight © Maprenal MF 920 gave analogous results Example 4
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24,9 Gewichtsteile einer Mischung aus 80 Gew -% ©Knapsack Phosphorsaureester MOE und 20 Gew -% ©Knapsack Reinigerkomponente MS24.9 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MOE and 20% by weight © Knapsack cleaner component MS
Beispiel 5Example 5
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24.8 Gewichtsteile einer Mischung aus 70 Gew -% ©Knapsack Phosphorsaureester MOE und 30 Gew -% ©Knapsack Reinigerkomponente MIS24.8 parts by weight of a mixture of 70% by weight © Knapsack phosphoric acid ester MOE and 30% by weight © Knapsack cleaner component MIS
Beispiel 6Example 6
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24.9 Gewichtsteile einer Mischung aus 90 Gew -% ©Knapsack Phosphorsaureester MOE und 10 Gew -% ©Knapsack Reinigerkomponente MIS24.9 parts by weight of a mixture of 90% by weight © Knapsack phosphoric acid ester MOE and 10% by weight © Knapsack cleaner component MIS
Eine Wiederholung der Beispiele 4 bis 6 mit 60 Gewichtsteile ©Maprenal VMF 3921 w anstatt 68 Gewichtsteile ©Maprenal MF 920 lieferte analoge ErgebnisseA repetition of Examples 4 to 6 with 60 parts by weight © Maprenal VMF 3921 w instead of 68 parts by weight © Maprenal MF 920 gave analogous results
Beispiel 7Example 7
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
26,1 Gewichtsteile einer Mischung aus 90 Gew.-% ©Knapsack Phosphorsaureester MOE und 10 Gew.-% ©Knapsack Phosphorsaureester MDIP26.1 parts by weight of a mixture of 90% by weight © Knapsack phosphoric acid ester MOE and 10% by weight © Knapsack phosphoric acid ester MDIP
Beispiel 8Example 8
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
26,4 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Phosphorsaureester MOE und 20 Gew.-% ©Knapsack Phosphorsaureester MDIP26.4 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MOE and 20% by weight © Knapsack phosphoric acid ester MDIP
Beispiel 9Example 9
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
28,7 Gewichtsteile einer Mischung aus 70 Gew -% ©Knapsack Phosphorsaureester MOE und 30 Gew.-% ©Knapsack Phosphorsaureester MDIP Beispiel 1028.7 parts by weight of a mixture of 70% by weight © Knapsack phosphoric acid ester MOE and 30% by weight © Knapsack phosphoric acid ester MDIP Example 10
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
26,4 Gewichtsteile einer Mischung aus 90 Gew.-% ©Knapsack Phosphorsaureester MOE und 10 Gew.-% ©Knapsack Phosphorsaureester MDB26.4 parts by weight of a mixture of 90% by weight © Knapsack phosphoric acid ester MOE and 10% by weight © Knapsack phosphoric acid ester MDB
Beispiel 11Example 11
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
27,9 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Phosphorsaureester MOE und 20 Gew.-% ©Knapsack Phosphorsaureester MDB27.9 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MOE and 20% by weight © Knapsack phosphoric acid ester MDB
Beispiel 12Example 12
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
29,6 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Phosphorsaureester MOE und 20 Gew.-% ©Knapsack Phosphorsaureester MDB29.6 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MOE and 20% by weight © Knapsack phosphoric acid ester MDB
Eine Wiederholung der Beispiele 7 bis 12 mit 60 Gewichtsteile ©Maprenal VMF 3921 w anstatt 68 Gewichtsteile ©Maprenal MF 920 lieferte analoge Ergebnisse.A repetition of Examples 7 to 12 with 60 parts by weight © Maprenal VMF 3921 w instead of 68 parts by weight © Maprenal MF 920 gave analogous results.
Beispiel 13Example 13
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24.3 Gewichtsteile einer Mischung aus 90 Gew.-% ©Knapsack Reinigerkomponente MS und 10 Gew.-% ©Knapsack Reinigerkomponente MIS24.3 parts by weight of a mixture of 90% by weight © Knapsack cleaner component MS and 10% by weight © Knapsack cleaner component MIS
Beispiel 14Example 14
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24.4 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Reinigerkomponente MS und 20 Gew.-% ©Knapsack Reinigerkomponente MIS24.4 parts by weight of a mixture of 80% by weight © Knapsack cleaner component MS and 20% by weight © Knapsack cleaner component MIS
Beispiel 15Example 15
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
24,3 Gewichtsteile einer Mischung aus 70 Gew.-% ©Knapsack Reinigerkomponente MS und 30 Gew.-% ©Knapsack Reinigerkomponente MIS Beispiel 1624.3 parts by weight of a mixture of 70% by weight © Knapsack cleaner component MS and 30% by weight © Knapsack cleaner component MIS Example 16
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
25,5 Gewichtsteile einer Mischung aus 90 Gew.-% ©Knapsack Reinigerkomponente MS und 10 Gew.-% ©Knapsack Phosphorsaureester MDIP25.5 parts by weight of a mixture of 90% by weight © Knapsack cleaning component MS and 10% by weight © Knapsack phosphoric acid ester MDIP
Beispiel 17Example 17
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
26,7 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Reinigerkomponente MS und 20 Gew.-% ©Knapsack Phosphorsaureester MDIP26.7 parts by weight of a mixture of 80% by weight © Knapsack cleaner component MS and 20% by weight © Knapsack phosphoric acid ester MDIP
Beispiel 18Example 18
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
28,0 Gewichtsteile einer Mischung aus 70 Gew.-% ©Knapsack Reinigerkomponente MS und 30 Gew.-% ©Knapsack Phosphorsaureester MDIP28.0 parts by weight of a mixture of 70% by weight © Knapsack cleaner component MS and 30% by weight © Knapsack phosphoric acid ester MDIP
Beispiel 19Example 19
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
25,7 Gewichtsteile einer Mischung aus 90 Gew.-% ©Knapsack Reinigerkomponente MS und 10 Gew.-% ©Knapsack Phosphorsaureester MDB25.7 parts by weight of a mixture of 90% by weight © Knapsack cleaner component MS and 10% by weight © Knapsack phosphoric acid ester MDB
Beispiel 20Example 20
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
27,2 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Reinigerkomponente MS und 20 Gew.-% ©Knapsack Phosphorsaureester MDB27.2 parts by weight of a mixture of 80% by weight © Knapsack cleaner component MS and 20% by weight © Knapsack phosphoric acid ester MDB
Beispiel 21Example 21
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
29,0 Gewichtsteile einer Mischung aus 70 Gew.-% ©Knapsack Reinigerkomponente MS und 30 Gew.-% ©Knapsack Phosphorsaureester MDB Beispiel 2229.0 parts by weight of a mixture of 70% by weight © Knapsack cleaner component MS and 30% by weight © Knapsack phosphoric acid ester MDB Example 22
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
30,1 Gewichtsteile einer Mischung aus 90 Gew,-% ©Knapsack Phosphorsaureester MDE und 10 Gew.-% ©Knapsack Reinigerkomponente MS30.1 parts by weight of a mixture of 90% by weight © Knapsack phosphoric acid ester MDE and 10% by weight © Knapsack cleaner component MS
Beispiel 23Example 23
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
30,1 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Phosphorsaureester MDE und 20 Gew.-% ©Knapsack Reinigerkomponente MS30.1 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MDE and 20% by weight © Knapsack cleaner component MS
Beispiel 24Example 24
68 Gewichtsteile ©Maprenal MF 92068 parts by weight © Maprenal MF 920
29,3 Gewichtsteile einer Mischung aus 70 Gew.-% ©Knapsack Phosphorsaureester MDE und 30 Gew.-% ©Knapsack Rei igerkomponente MS29.3 parts by weight of a mixture of 70% by weight of Knapsack phosphoric acid ester MDE and 30% by weight of Knapsack cleaner component MS
Eine Wiederholung der Beispiele 13 bis 24 mit 60 Gewichtsteile ©Maprenal VMF 3921 w anstatt 68 Gewichtsteile ©Maprenal MF 920 lieferte analoge Ergebnisse.A repetition of Examples 13 to 24 with 60 parts by weight © Maprenal VMF 3921 w instead of 68 parts by weight © Maprenal MF 920 gave analogous results.
Beispiel 25Example 25
60 Gewichtsteile ©Maprenal MF 3921 w 27 Gewichtsteile ©Knapsack Phosphorsaureester MDE 7 Gewichtsteile ©Knapsack Phosphorsaureester MDIP60 parts by weight © Maprenal MF 3921 w 27 parts by weight © Knapsack phosphoric acid ester MDE 7 parts by weight © Knapsack phosphoric acid ester MDIP
Beispiel 26Example 26
60,0 Gewichtsteile ©Maprenal MF 92060.0 parts by weight © Maprenal MF 920
24,0 Gewichtsteile ® Knapsack Phosphorsaureester MDE24.0 parts by weight ® Knapsack phosphoric acid ester MDE
6,0 Gewichtsteile ©Knapsack Phosphorsaureester MDIP6.0 parts by weight © Knapsack phosphoric acid ester MDIP
3,0 Gewichtsteile ©Aerosil R 8163.0 parts by weight © Aerosil R 816
7,0 Gewichtsteile ©Mistrofil 500 Beispiel 277.0 parts by weight © Mistrofil 500 Example 27
60 Gewichtsteile ©Maprenal MF 92060 parts by weight © Maprenal MF 920
27, 1 Gewichtsteile ©Knapsack Phosphorsaureester MDE27, 1 parts by weight © Knapsack phosphoric acid ester MDE
6,8 Gewichtsteile ©Knapsack Phosphorsaureester MDIP6.8 parts by weight © Knapsack phosphoric acid ester MDIP
0,6 Gewichtsteile ©Knapsack Phosphorsaureester 1220.6 parts by weight © Knapsack phosphoric acid ester 122
3,0 Gewichtsteile ©Aerosil R 8163.0 parts by weight © Aerosil R 816
7,2 Gewichtsteile ©Mistrofil 5007.2 parts by weight © Mistrofil 500
Beispiel 28Example 28
60 Gewichtsteile ©Maprenal VMF 3921 w60 parts by weight © Maprenal VMF 3921 w
34.5 Gewichtsteile einer Mischung aus 75 Gew -% ©Knapsack Phosphorsaureester MDE und 25 Gew -% ©Knapsack Phosphorsaureester MDIP34.5 parts by weight of a mixture of 75% by weight © Knapsack phosphoric acid ester MDE and 25% by weight © Knapsack phosphoric acid ester MDIP
Beispiel 29Example 29
80 Gewichtsteile ©Maprenal VMF 3921 w80 parts by weight © Maprenal VMF 3921 w
44.6 Gewichtsteile einer Mischung aus 85 Gew -% ©Knapsack Phosphorsaureester MDE und 15 Gew -% ©Knapsack Phosphorsaureester MDIP44.6 parts by weight of a mixture of 85% by weight © Knapsack phosphoric acid ester MDE and 15% by weight © Knapsack phosphoric acid ester MDIP
Beispiel 30Example 30
80 Gewichtsteile ©Maprenal VMF 3921 w80 parts by weight © Maprenal VMF 3921 w
46,5 Gewichtsteile einer Mischung aus 70 Gew -% ©Knapsack Phosphorsaureester MDE und 30 Gew.-% ©Knapsack Phosphorsaureester MDIP46.5 parts by weight of a mixture of 70% by weight © Knapsack phosphoric acid ester MDE and 30% by weight © Knapsack phosphoric acid ester MDIP
9,6 Gewichtsteile ©Mistrofil 5009.6 parts by weight © Mistrofil 500
4 Gewichtsteile hochdisperse Kieselsaure4 parts by weight of highly disperse silica
Weitere Beispiele für die erfindungsgemaße intumeszierende flammhemmende Überzugsmasse finden sich in den Tabellen 1 bis 11 Mit allen Rezepturen wurde in der Brandpru- fung Bl bzw. B2 erreicht. Tabelle 1 :Further examples of the intumescent flame-retardant coating composition according to the invention can be found in Tables 1 to 11. All the formulations were achieved in the fire test B1 or B2. Table 1 :
*) MDE : MDIP bedeutet: Mischung aus 85 Gew.-% ®Knapsack Phosphor85 : 15 saureester MDE und 15 Gew.-% ©Knapsack Phos phorsäureester MDIP. Diese Schreibweise gilt entsprechend für die nachfolgenden Tabellen.*) MDE: MDIP means: Mixture of 85% by weight ®Knapsack phosphorus85: 15 acidic MDE and 15% by weight © Knapsack phosphoric acid ester MDIP. This notation applies accordingly to the following tables.
Tabelle 2:Table 2:
Tabelle 3:Table 3:
Tabelle 4: Table 4:
Tabelle 5 :Table 5:
In dieser Versuchsreihe wurde als hochdisperse Kieselsäure ®CAB-O-SIL TS 530 (Fa. CABOT, Hanau) verwendet. Erfolgreich eingesetzt wurde ebenso ©Aerosil OX-50 (pyrogene Kieselsäure der Fa. Degussa AG). Beispiel 50In this series of experiments, ®CAB-O-SIL TS 530 (CABOT, Hanau) was used as the highly disperse silica. Also successfully used was © Aerosil OX-50 (pyrogenic silica from Degussa AG). Example 50
90 Gewichtsteile ©Maprenal VMF 3921 w90 parts by weight © Maprenal VMF 3921 w
45,15 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Phosphorsaureester MDE und 20 Gew.-% ©Knapsack Reinigerkomponente MIS 11,7 Gewichtsteile ©Mistrofil 500 0,9 Gewichtsteile ©Knapsack Phosphorsaureester 12245.15 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MDE and 20% by weight © Knapsack cleaning component MIS 11.7 parts by weight © Mistrofil 500 0.9 parts by weight © Knapsack phosphoric acid ester 122
Tabelle 6:Table 6:
Tabelle 7:Table 7:
Tabelle 8: Table 8:
Tabelle 9:Table 9:
Tabelle 10: Table 10:
Eine Wiederholung der Beispiele 61 bis 64 mit ©Maprenal MF 920 anstatt ©Maprenal VMF 3921 w lieferte analoge Ergebnisse.Repeating examples 61 to 64 with © Maprenal MF 920 instead of © Maprenal VMF 3921 w gave analog results.
Tabelle n:Table n:
Beispiel 67 Example 67
80 Gewichtsteile ©Maprenal VMF 3921 w80 parts by weight © Maprenal VMF 3921 w
45,2 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Phosphorsaureester MDE und 20 Gew.-% ©Knapsack Phosphorsaureester MDIP 4 Gewichtsteile Titandioxid (®Kronos 2300)45.2 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MDE and 20% by weight © Knapsack phosphoric acid ester MDIP 4 parts by weight titanium dioxide (®Kronos 2300)
Beispiel 68Example 68
80 Gewichtsteile ©Maprenal VMF 3921 w80 parts by weight © Maprenal VMF 3921 w
45,2 Gewichtsteile einer Mischung aus 80 Gew.-% ©Knapsack Phosphorsaureester MDE und 20 Gew.-% ©Knapsack Phosphorsaureester MD EP45.2 parts by weight of a mixture of 80% by weight © Knapsack phosphoric acid ester MDE and 20% by weight © Knapsack phosphoric acid ester MD EP
0,9 Gewichtsteile ©Knapsack Phosphorsaureester 1220.9 parts by weight © Knapsack phosphoric acid ester 122
4 Gewichtsteile Titandioxid (©Kronos 2300)4 parts by weight of titanium dioxide (© Kronos 2300)
Die nach Beispiel 67 und 68 erhaltenen Überzugsmassen sind glatt, weiß und rißfrei. The coating compositions obtained according to Examples 67 and 68 are smooth, white and free of cracks.

Claims

Intumeszierende, fiammhemmende ÜberzugsmassenPatentansprüche Intumescent, flame retardant coating compositions
1. Intumeszierende, flammhemmende Überzugsmassen, enthaltend1. Containing intumescent, flame-retardant coating compositions
10 bis 150 Gewichtsteile einer wäßrigen Kunstharzdispersion und 10 bis 80 Gewichtsteile einer Mischung aus mindestens zwei verschiedenen10 to 150 parts by weight of an aqueous synthetic resin dispersion and 10 to 80 parts by weight of a mixture of at least two different ones
Phosphorsäurepartialestem.Phosphoric acid partial esters.
2. Intumeszierende, flammhemmende Überzugsmassen nach Anspruch 1, dadurch gekennzeichnet, daß sie2. Intumescent, flame-retardant coating compositions according to claim 1, characterized in that they
50 bis 90 Gewichtsteile einer wäßrigen Kunstharzdispersion, 20 bis 60 Gewichtsteile einer Mischung aus mindestens zwei verschiedenen Phosphorsäurepartialestem und 1 bis 80 Gewichtsteile weitere Inhaltsstoffe enthalten.Contain 50 to 90 parts by weight of an aqueous synthetic resin dispersion, 20 to 60 parts by weight of a mixture of at least two different phosphoric acid partial esters and 1 to 80 parts by weight of further ingredients.
3. Intumeszierende, flammhemmende Überzugsmassen nach Anspmch 1 oder 2, dadurch gekennzeichnet, daß sie eine Mischung aus 3 verschiedenen Phosphorsäurepartialestem enthalten. Third Intumescent, flame-retardant coating compositions according to Claim 1 or 2, characterized in that they contain a mixture of 3 different phosphoric acid partial esters.
4. Intumeszierende, flammhemmende Überzugsmassen nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß sie eine Mischung aus 4 verschiedenen Phosphorsäurepartialestem enthalten. 4. Intumescent, flame-retardant coating compositions according to claim 1 or 2, characterized in that they contain a mixture of 4 different phosphoric acid partial esters.
5. Intumeszierende, flammhemmende Überzugsmassen nach Anspmch 4, dadurch gekennzeichnet, daß die Mischung der 4 verschiedenen Phosphorsaurepartialester aus a) einer Mischung aus einem Phosphorsauremonoalkylester und einem Phosphorsäuredi- alkylester mit gleicher Alkylgruppe und b) einer Mischung aus einem Phosphorsauremonoalkylester und einem Phosphorsäuredi- alkylester mit gleicher, aber zu a) unterschiedlicher Alkylgruppe besteht.5. Intumescent, flame-retardant coating compositions according to Anspmch 4, characterized in that the mixture of the 4 different phosphoric acid partial esters from a) a mixture of a phosphoric acid monoalkyl ester and a phosphoric acid dialkyl ester with the same alkyl group and b) a mixture of a phosphoric acid monoalkyl ester and a phosphoric acid dialkyl ester with the same, but different to a) alkyl group.
6. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß es sich bei der wäßrigen Kunstharzdispersion um eine stickstoffhaltige Kunstharzdispersion handelt.6. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 5, characterized in that it is a nitrogen-containing synthetic resin dispersion in the aqueous synthetic resin dispersion.
7. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß es sich bei der wäßrigen Kunstharzdispersion um ein Melamin- und/oder Harnstoff-Formaldehyd-Harz handelt.7. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 6, characterized in that it is a melamine and / or urea-formaldehyde resin in the aqueous resin dispersion.
8. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß es sich bei der wäßrigen Kunstharzdispersion um ein verethertes Melamin- und/oder Hamstoff-Formaldehyd-Harz handelt.8. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 7, characterized in that it is an etherified melamine and / or urea-formaldehyde resin in the aqueous synthetic resin dispersion.
9. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, daß es sich bei den weiteren Inhaltsstoffen um Dispergiermittel, Füllstoffe, Härter, Thixotropierungsmittel, Weichmacher, Säurespender, weitere Flammschutzmittel, Oberflächenhilfsmittel und/oder Binder handelt.9. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 8, characterized in that the other ingredients are dispersants, fillers, hardeners, thixotropic agents, plasticizers, acid donors, further flame retardants, surface auxiliaries and / or binders.
10. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, daß es sich bei den weiteren Inhaltsstoffen um Thixotropierungsmittel und/oder Füllstoffe handelt.10. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 9, characterized in that the other ingredients are thixotropic agents and / or fillers.
11. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 10, dadurch gekennzeichnet, daß es sich bei den Phosphorsäurepartialestem um solche der Formel O-R1 I11. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 10, characterized in that the phosphoric acid partial esters are those of the formula OR 1 I
0=P-0H0 = P-0H
0 ' -R 2 handelt, in der R1 und R2 gleich oder verschieden sind und H, CH3, C2H5, C3H7, C4H9, C5H11, C6Hι3, C8H16 und/oder CH2-CH2-OH, und R1 und R2 nicht gleichzeitig Wasserstoffbedeuten.0 '-R 2, in which R 1 and R 2 are identical or different and H, CH 3 , C 2 H 5 , C 3 H 7 , C 4 H 9 , C5H11, C 6 Hι 3 , C 8 H 16 and / or CH 2 -CH 2 -OH, and R 1 and R 2 do not simultaneously mean hydrogen.
12. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 11, dadurch gekennzeichnet, daß ihr Phosphorgehalt nach der Aushärtung 1 bis 15 Gew.-% beträgt.12. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 11, characterized in that their phosphorus content after curing is 1 to 15 wt .-%.
13. Intumeszierende, flammhemmende Überzugsmassen nach mindestens einem der Ansprüche 1 bis 11, dadurch gekennzeichnet, daß ihr Phosphorgehalt nach der Aushärtung 5 bis 10 Gew.-% beträgt.13. Intumescent, flame-retardant coating compositions according to at least one of claims 1 to 11, characterized in that their phosphorus content after curing is 5 to 10 wt .-%.
14. Intumeszierende, flammhemmende Überzugsmasse nach mindestens einem der Ansprüche 1 bis 13, dadurch gekennzeichnet, daß sie nach Auftragen und Trocknung transparent ist.14. Intumescent, flame-retardant coating composition according to at least one of claims 1 to 13, characterized in that it is transparent after application and drying.
15. Verwendung der Überzugsmassen nach mindestens einem der Ansprüche 1 bis 14 zur Herstellung von Beschichtungen auf Gegenständen aus Holz, Kunststoffen, Baustoffen, Cellulosematerialien, Gummi und Metall und zur Imprägnierung von Textilien und Ledern. 15. Use of the coating compositions according to at least one of claims 1 to 14 for the production of coatings on objects made of wood, plastics, building materials, cellulose materials, rubber and metal and for impregnation of textiles and leather.
EP98961186A 1997-11-20 1998-11-12 Intumescent flame-retardant coatings Withdrawn EP1034225A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19751434 1997-11-20
DE19751434A DE19751434A1 (en) 1997-11-20 1997-11-20 Intumescent, flame-retardant coating compounds
PCT/EP1998/007239 WO1999027021A1 (en) 1997-11-20 1998-11-12 Intumescent flame-retardant coatings

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EP1034225A1 true EP1034225A1 (en) 2000-09-13

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JP (1) JP2001524571A (en)
KR (1) KR20010032236A (en)
AR (1) AR016690A1 (en)
AU (1) AU1669699A (en)
BR (1) BR9814673A (en)
CA (1) CA2310438A1 (en)
DE (1) DE19751434A1 (en)
TW (1) TW419513B (en)
WO (1) WO1999027021A1 (en)

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Publication number Priority date Publication date Assignee Title
DE10221222A1 (en) * 2002-05-13 2003-11-27 Basf Ag Flame retardant finishing of objects containing organic latent heat storage materials
DE10261213B4 (en) 2002-12-20 2006-08-17 Raymaster Holding Ag Intumescent textile
DE10305548A1 (en) * 2003-02-10 2004-08-26 Basf Ag Flame retardant molded plastic parts
DE102010054341B3 (en) 2010-09-27 2012-01-26 Lufthansa Technik Ag Method of applying a fire-resistant coating to a substrate and substrate with a fire-resistant coating
DE102013202493A1 (en) * 2013-02-15 2014-08-21 Lufthansa Technik Ag Flame retardant wood substrate
TW202122516A (en) 2019-08-30 2021-06-16 瑞士商克萊瑞特國際股份有限公司 Intumescent flame-retardant clearcoat formulations
DE102021111074A1 (en) * 2021-04-29 2022-11-03 Lufthansa Technik Aktiengesellschaft Flame retardant wooden substrate

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AT400570B (en) * 1991-09-09 1996-01-25 Budenheim Rud A Oetker Chemie Polymeric composition with integrated intumescent properties, coating material and process for the preparation of phosphoric acid partial esters
US5387655A (en) * 1991-09-09 1995-02-07 Chemische Fabrik Budenheim Composition with integral intumescence properties
DE4307406A1 (en) * 1993-03-09 1994-09-15 Akro Fireguard Prod Inc Intumescent composition of the two-component type
DE4343669A1 (en) * 1993-12-21 1995-06-22 Hoechst Ag Clear, inflatable, flame-retardant coating compounds

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Title
See references of WO9927021A1 *

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WO1999027021A1 (en) 1999-06-03
CA2310438A1 (en) 1999-06-03
BR9814673A (en) 2000-10-03
AU1669699A (en) 1999-06-15
JP2001524571A (en) 2001-12-04
AR016690A1 (en) 2001-07-25
TW419513B (en) 2001-01-21
DE19751434A1 (en) 1999-07-29

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