EP1287066A1 - Melanges intumescents ignifuges - Google Patents

Melanges intumescents ignifuges

Info

Publication number
EP1287066A1
EP1287066A1 EP01951480A EP01951480A EP1287066A1 EP 1287066 A1 EP1287066 A1 EP 1287066A1 EP 01951480 A EP01951480 A EP 01951480A EP 01951480 A EP01951480 A EP 01951480A EP 1287066 A1 EP1287066 A1 EP 1287066A1
Authority
EP
European Patent Office
Prior art keywords
mixture according
polymer
mixtures
weight
flame
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Withdrawn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
EP01951480A
Other languages
German (de)
English (en)
Inventor
Martin Hoch
Gert Jabs
Otto Mauerer
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.)
Lanxess Deutschland GmbH
Original Assignee
Bayer AG
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 Bayer AG filed Critical Bayer AG
Publication of EP1287066A1 publication Critical patent/EP1287066A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic

Definitions

  • the invention relates to mixtures containing
  • a polymer which can be prepared from ethylene, vinyl acetate and optionally further monomers with a vinyl acetate content in the range from 40 to 85% by weight,
  • Flame-retardant intumescent mixtures are to be understood as foaming, flame-retardant mixtures, that is to say mixtures which foam to a certain extent under the action of fire and have flame-retardant properties.
  • Such mixtures can be used, for example, in building joints and cable breakthroughs, cavities, holes, transitions and connections between building walls or fire protection components such as cladding to prevent the fire, fire gases and smoke from being transmitted in the event of a fire.
  • Components made from such mixtures therefore serve as preventive fire protection.
  • the expansion behavior of such compounds in the event of a fire can also contribute in particular to maintaining the shape or function of, for example, ceiling cladding and wall cladding, because the components are pressed together by inflating profiles and sealing pieces.
  • Such mixtures must have other properties, e.g. Water resistance. Therefore, conventional flame retardants such as water-soluble polyphosphates are mostly undesirable. The extent of foaming must remain unchanged even over very long storage times.
  • JP-B-95068362 It is known from JP-B-95068362 to use expandable graphite as a flame-retardant component in mixtures of vulcanized acrylate rubber.
  • JP-B2-95103948 describes expandable graphite acrylate rubber vulcanizates for the manufacture of flame-retardant hoses.
  • JP-A-10036572 describes expandable graphite rubber mixtures based on polychloroprene with a maximum of 30 phr (per hundred rubber) expandable graphite and thus to a small proportion of this filler.
  • the use of halogen-containing components is no longer desirable today.
  • JP-A-09176579 describes mixtures with EVA (10-50% VA) or m-PE with phosphorus and expanded graphite and mineral filler for adhesive tapes around pipes through wall openings. Red phosphorus is always used. However, processing red phosphorus is difficult. In addition, red phosphorus may continue to react even after processing.
  • the object on which this invention was based was to find a phosphorus-free, in particular red phosphorus-free, mixture which passed the required fire protection tests and had sufficient expansion behavior, waterproof and allows simple shaping, for example via extrusion, calendering, press molding, etc.
  • the moldings that can be produced should have sufficient dimensional stability, but should still be deformable to a certain extent in order to
  • a further task was therefore the provision of non-vulcanized mixtures which have sufficient dimensional stability and which can still be deformed to a certain extent by the user.
  • a polymer which can be prepared from ethylene, vinyl acetate and, if appropriate, further monomers with a vinyl acetate content in the range from 40 to 85% by weight,
  • Ethylene-vinyl acetate copolymers are preferably used as polymer a).
  • the polymers a) can be prepared by conventional methods, such as, for example, by radical copolymerization in solution, emulsion or mass.
  • the copolymerized vinyl acetate content should advantageously be in the range from 50 to 85% by weight, mixtures of these polymers with different vinyl acetate contents also being able to be used.
  • ethylene-vinyl acetate polymers which may optionally contain further co-monomers
  • ethylene-methyl acrylate polymers which may also contain further co-monomers can also be used.
  • an ethylene-vinyl acetate copolymer or an ethylene-methyl acrylate copolymer should advantageously be used.
  • the highest flame retardancy is achieved with particularly high levels of polar comonomer.
  • Possible additional comonomers which may be present are, in particular, vinyl esters of higher carboxylic acids and also longer-chain (meth) acrylates, the content of these monomers in the polymer, as a rule, the higher the more nonpolar, organic groups in the polymer in order to ensure the desired flame resistance are included. CO is also mentioned as a monomer unit.
  • the glass transition temperature of the terpolymers thus available must be taken into account. If this is at room temperature or above room temperature, mixtures made with them are usually brittle at the typical operating temperatures and are therefore problematic in use.
  • the flexibility of moldings from the mixtures according to the invention can of course also be influenced by adding plasticizing additives mentioned below.
  • expandable graphites which are formed by sulfation or nitration of graphite, can advantageously be used as expandable graphite b).
  • These expandable graphites are known to the person skilled in the art and can be used to achieve flame retardancy in sealants, coatings and in general in thermoplastics. Typical is e.g. an application with polyurethanes (see brochure short delivery program flame retardants, fire protection articles from Nordmarm and Rassmann from January 2000).
  • Expandable graphites are layered graphites that are reacted with sulfuric acid or nitric acid or generally strong acids under oxidizing conditions. Water-soluble salts are formed in the graphite layer lattice. The reaction with sulfuric acid and H 2 O 2 is typical. These reaction products are then usually washed acid-free with water, the amount of remaining acid should be measured below 1 mg / g as KOH.
  • Neutral expanded graphites are obtained by an additional neutralization (eg with sodium hydroxide solution or ammonia), this material also being washed again in order to remove adhering neutralizing agent. Neutral types have a pH of at least 6.
  • expanded graphite for fire protection is based on 1. the ability to expand when exposed to heat. This expansion can be up to over 200 ml per g and creates a large surface area. Oxidation quickly removes oxygen from the immediate surroundings, thereby extinguishing fire. 2. Expandable graphite does not generate a flame during oxidation and extinguishes immediately when the flame is removed. The expansion in the event of a fire closes joints and breakthroughs and thereby prevents the fire from spreading. In principle, the person skilled in the art is aware of the criteria according to which expanded graphites must be selected in order to determine the expandability and the start of the expansion. In this context, the particle size and the type of
  • Intercalates which can mostly be sulfuric acid or nitric acid or less often acetic acid.
  • acidic expandable graphites there are still residues of acids
  • alkaline expandable graphites there are residues of bases, e.g. Sodium hydroxide solution included.
  • the mineral fillers can be freely selected, with energy-consuming fillers such as aluminum hydroxides, magnesium hydroxides or calcium carbonate making additional contributions to flame retardancy.
  • energy-consuming fillers such as aluminum hydroxides, magnesium hydroxides or calcium carbonate making additional contributions to flame retardancy.
  • talc, silicas, silicates, carbonates and sulfates can also be used. Mixtures of the fillers mentioned can of course be used.
  • Typical additives are processing aids, such as stearic acid, waxes, glide waxes, oils, and release agents or flame retardant additives are used, such as organophosphate, Ammom 'umpolyphosphate, antimony bromide, etc., halogen-containing flame retardants are less preferred. Water-soluble additives are less preferred for reasons of water resistance.
  • non-neutralized expandable graphites are used together with ethylene-vinyl acetate copolymers, partial hydrolysis can occur with the formation of acetic acid.
  • basic oxides and carbonates or other acid scavengers can advantageously be added.
  • Non-polar, essentially saturated elastomers such as EPM, EPDM, butyl rubber, hydrogenated or partially hydrogenated SBR rubbers are also suitable as additives, but advantageously up to a maximum of half the amount of a).
  • An advantage of the mixtures is that they allow a relatively wide variation in the amounts of expandable graphite and especially other mineral fillers, which are energy-consuming when exposed to fire. In this way, particularly high amounts of components b) and c) can be achieved.
  • component b) can surprisingly be used in an amount in the range from 50 to 200 parts by weight and component c) in an amount in the range from 50 to 500 parts by weight, in each case based on 100 parts by weight a), without the sacrifice good properties, especially mechanical and processing properties. This means that high fire behavior requirements can be met.
  • Mixture can be influenced favorably, since mineral fillers are usually relatively cheap.
  • the polymers a) used additionally probably have the function of an effective binder, which allows large amounts of filler, including
  • Another object of the invention is a process for the preparation of the mixtures according to the invention by the individual components in any order in a conventional mixing unit, such as an internal mixer
  • roller, a screw or a kneader mixes. It may be advantageous to cool during the mixing process to prevent the mixture from becoming too hot.
  • the polymers a) according to the invention allow the preparation of a mixture without the use of excessive shear forces which could adversely affect the structure of the expanded graphite.
  • Another object of the invention is the use of the mixture for
  • the moldings can be produced by continuous processes, since the mixtures have a sufficiently wide processing window in the processing processes. This means that premature foaming during molding can be avoided.
  • Extrusion, optionally multi-layer extrusion and calendering are preferred processing methods.
  • the shaped bodies mentioned are a further subject of the invention. It may be necessary to vulcanize the mixtures according to the invention to produce the moldings. This is done in a manner known to those skilled in the art and is e.g. in "Vulkanisation & Vulkanisationsakusstoff (W. Hofmann, Leverkusen 1965, pp. 85ff, 225 ff). The vulcanization system must be selected according to the type of polymer a).
  • Another object of the invention are flame-retardant, intumescent mixtures containing a mixture according to the invention.
  • Levapren® 700 HV ethylene-vinyl acetate copolymer with 70% by weight
  • Vinyl acetate from Bayer AG powdered with silica as granules, Mooney ML 1 + 4, 100 ° C 27 ME, MFI according to DIN 53735 (190 ° C, 2.16 kp) of approx. 2.5 g / 10 min.
  • 2.Levapren® 800 HV ethylene-vinyl acetate copolymer with 80% by weight vinyl acetate from Bayer AG, powdered with silica as granules, Mooney ML 1 + 4, 100 ° C 26 ME, MFI according to DIN 53735 (190 ° C, 2.16 kp) of approx.3.0 g / 10 min.
  • Apyral® B 120 aluminum hydroxide from United Aluminum Works
  • Buna® EP G 6170 EPDM rubber from Bayer AG with an ethylene content of approx. 70%, an ENB content of approx. 1.5% and one
  • Enerthene® 1849-1 plasticizer based on mineral oil from BP, aliphatic
  • Disflamol® DPK plasticizer from Bayer AG based on diphenyl cresyl phosphate 9.
  • Maglite D magnesium oxide from CP Hall Company
  • Rhenosorb® CaO from Rheinchemie
  • the amounts of the mixture components used were designed for a total of 200 to 300 g.
  • the mixture was mixed on a laboratory roller at approx. 20 ° C. by introducing the polymer and first subjecting it to a few roller passes, then the stearic acid, expanded graphite and apyral were added in succession and the mixture after a total mixing time of 15 min. taken off the roller.
  • Test specimens were pressed from the mixtures as indicated, two different pressing conditions being selected.
  • test specimens were flexible and could be bent without breaking.
  • Mixtures 1 a to 1 b show that mixtures of levapren and expandable graphite can also be filled with a flame-retardant filler such as Apyral. Easily processable mixtures are obtained which show a uniform intumescence in the flame test. They are particularly good here
  • Mixtures 1 c and 1 d The formation of bubbles between dents in the flame test depends on the pressing conditions.
  • the amount of apyral which can advantageously be used is obviously exceeded with 400 phr.
  • the amount preferably being 50 phr or more.
  • the mixtures were prepared as in Example 1, but the temperature was set to 50 ° C. during the preparation of the mixture.
  • Processable mixtures with EPDM can only be obtained with expandable graphite quantities below 70 phr. Acceptable moldings could only be obtained after prolonged pressing, but blistering was then observed in the flame test.
  • the mixtures were prepared as in Example 1.
  • the feed materials were mixed in on the roller in the order given in the table.
  • the rolling temperature was 20 ° C
  • the pressing temperatures were 70
  • Levapren 800 HV can be used for intumescent mixtures as well as Levapren 700 HV.
  • the quality of the plates / test specimens was more homogeneous with Levapren 700 HV.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)
  • Finishing Walls (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

L'invention concerne des mélanges contenant : a) un polymère pouvant être obtenu à partir d'éthylène, de vinylacétate et éventuellement d'autres monomères à teneur en vinylacétate de l'ordre de 40 à 85 % en poids ; b) au moins un graphite expansible pouvant être acide ou neutralisé ; c) au moins une charge minérale ; d) éventuellement d'autres additifs. L'invention concerne également un procédé permettant de préparer lesdits mélanges, leur utilisation pour produire des corps moulés de toutes sortes, ainsi que des mélanges intumescents ignifuges contenant un mélange selon l'invention, ainsi que des corps moulés contenant un mélange selon l'invention.
EP01951480A 2000-05-19 2001-05-07 Melanges intumescents ignifuges Withdrawn EP1287066A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10024421 2000-05-19
DE10024421A DE10024421A1 (de) 2000-05-19 2000-05-19 Flammwidrige intumeszierende Mischungen
PCT/EP2001/005144 WO2001088029A1 (fr) 2000-05-19 2001-05-07 Melanges intumescents ignifuges

Publications (1)

Publication Number Publication Date
EP1287066A1 true EP1287066A1 (fr) 2003-03-05

Family

ID=7642561

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01951480A Withdrawn EP1287066A1 (fr) 2000-05-19 2001-05-07 Melanges intumescents ignifuges

Country Status (7)

Country Link
US (1) US7087670B2 (fr)
EP (1) EP1287066A1 (fr)
JP (1) JP2003533575A (fr)
AU (1) AU2001272395A1 (fr)
CA (1) CA2409019A1 (fr)
DE (1) DE10024421A1 (fr)
WO (1) WO2001088029A1 (fr)

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Also Published As

Publication number Publication date
US7087670B2 (en) 2006-08-08
JP2003533575A (ja) 2003-11-11
CA2409019A1 (fr) 2002-11-15
US20030125447A1 (en) 2003-07-03
WO2001088029A1 (fr) 2001-11-22
AU2001272395A1 (en) 2001-11-26
DE10024421A1 (de) 2001-11-22

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