EP0902804A1 - Polymerisats de styrene expansibles contenant des particules de noir de fumee - Google Patents

Polymerisats de styrene expansibles contenant des particules de noir de fumee

Info

Publication number
EP0902804A1
EP0902804A1 EP97924003A EP97924003A EP0902804A1 EP 0902804 A1 EP0902804 A1 EP 0902804A1 EP 97924003 A EP97924003 A EP 97924003A EP 97924003 A EP97924003 A EP 97924003A EP 0902804 A1 EP0902804 A1 EP 0902804A1
Authority
EP
European Patent Office
Prior art keywords
weight
expandable styrene
styrene polymers
polystyrene
foams
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.)
Ceased
Application number
EP97924003A
Other languages
German (de)
English (en)
Inventor
Klaus Hahn
Josef Lamprecht
Karl-Heinz Wassmer
Dietrich Scherzer
Frank Braun
Dieter Naegele
Gerd Ehrmann
Franz-Josef Dietzen
Rolf Henn
Frieder Hohwiller
Jürgen Fischer
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Publication of EP0902804A1 publication Critical patent/EP0902804A1/fr
Ceased 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
    • C08J9/16—Making expandable particles
    • 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
    • C08J9/0014—Use of organic additives
    • C08J9/0019—Use of organic additives halogenated
    • 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
    • C08J9/0014—Use of organic additives
    • C08J9/0023—Use of organic additives containing oxygen
    • 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
    • C08J9/0066—Use of inorganic compounding ingredients
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0066—Flame-proofing or flame-retarding additives
    • 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
    • C08J2325/00—Characterised by the use of 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 an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2325/02—Homopolymers or copolymers of hydrocarbons
    • C08J2325/04—Homopolymers or copolymers of styrene

Definitions

  • the invention relates to particulate, soot particles-containing expandable styrene polymers in particle form, their manufacture and foams produced therefrom.
  • Polystyrene particle foams have been known for a long time and have proven themselves in many areas. Such foams are produced by foaming polystyrene particles impregnated with blowing agents and the subsequent welding of the foam particles thus produced to shaped bodies. An important area of application is thermal insulation in construction.
  • the foams be self-extinguishing. It is known that this can be done by adding flame retardants, e.g. of bromine compounds can be achieved; However, whether a foam passes a certain fire test depends on various factors, such as the composition and density of the foam, the type and amount of flame retardant, and the type and amount of other additives.
  • flame retardants e.g. of bromine compounds
  • the foam sheets made of polystyrene particle foam used for thermal insulation mostly have densities of at least 30 g / l, since at these densities the thermal conductivity of the polystyrene particle foam has a minimum.
  • foam boards with lower densities especially ⁇ . 15 g / 1, to be used for heat insulation.
  • the production of such foams is technically not a problem.
  • foam sheets with a lower density however, have a drastically deteriorated thermal insulation capacity, so that they do not meet the requirements of thermal conductivity class 035 (DIN 18 164, part 1).
  • EP-A 372 343 describes polystyrene foams which contain 1 to 25% by weight of carbon black.
  • the carbon black has a particle size of 10 to 100 nm and a surface area of 10 to 1500 m 2 / g.
  • the polystyrene foams described there are predominantly produced by the extrusion process and preferably have a density of 32-40 g / 1, as is typical for these foams, on.
  • the addition of flame retardants is mentioned;
  • the polystyrene particle foams described in the examples with a content of 1.7% by weight of hexabromocyclododecane fail the fire test B2 (according to DIN 4102).
  • EP-A 620 246 describes moldings made of polystyrene particle foam which contain a particulate, athermanous material, in particular carbon black.
  • the density of the molded body is less than 20 g / 1.
  • the soot particles are preferably incorporated into the moldings by surface coating of the foamed polystyrene beads. However, this surface coating leads to a severe deterioration in the welding of the pre-foamed
  • the object of the invention was to provide expandable styrene polymers containing soot particles, which can be processed into polystyrene particle foams both with low density and with low thermal conductivity and which have good processing properties, good physical properties and in particular very good fire protection properties.
  • particulate, expandable styrene polymers which contain 0.05 to 25% by weight, based on the polymer, of carbon black particles in a homogeneous distribution and can be processed to give foams with a density of ⁇ 35 g / l, which are self-extinguishing and pass the fire test B2 (according to DIN 4102).
  • the invention furthermore relates to processes for producing the expandable styrene polymers and the self-extinguishing polystyrene particle foams produced from them.
  • Expandable styrene polymers are understood to mean styrene polymers containing blowing agents.
  • the expandable styrene polymers according to the invention contain, as polymer matrix, in particular homopolystyrene or styrene copolymers with up to 20% by weight, based on the weight of the polymers, of ethylenically unsaturated comonomers, in particular alkylstyrenes, divinylbenzene, acrylonitrile or ⁇ -methylstyrene.
  • Blends made of polystyrene and other polymers, in particular with rubbers and polyphenylene ether, are also possible.
  • the styrene polymers can contain the customary and known auxiliaries and additives, for example flame retardants, nucleating agents, UV stabilizers, chain transfer agents, blowing agents, plasticizers, pigments and antioxidants.
  • auxiliaries and additives for example flame retardants, nucleating agents, UV stabilizers, chain transfer agents, blowing agents, plasticizers, pigments and antioxidants.
  • the expandable particles are coated with the customary and known coating agents, for example metal stearates, glycerol esters and finely divided silicates.
  • coating agents for example metal stearates, glycerol esters and finely divided silicates.
  • the particle size is preferably in the range of 0.2-2 mm.
  • Preferred carbon black particles consist of flame black with a particle size of 60-150 nm, preferably 80-120 nm.
  • the BET surface area is preferably in the range of 10-500 mVg.
  • Soot particles are preferably contained in the styrene polymer in amounts of 2 to 8% by weight.
  • soot particles A problem with the use of soot particles is the easy flammability of the polystyrene particle foams containing soot particles. So far it has not been possible to pass the fire tests (Bl and B2 according to DIN 4102) necessary for polystyrene foams containing carbon black for use in construction.
  • the expandable styrene polymers are flame retardants, in particular those based on organic
  • the bromine compound (without synergist) should be added in an amount of more than 3% by weight, based on the weight of the expandable styrene polymers. Bl and B2 are missed with the usual amount of flame retardants.
  • the organic bromine compounds should have a bromine content of ⁇ 70% by weight.
  • the effect of the bromine-containing flame retardants is considerably improved by adding C-C- or 0-O-unstable organic compounds.
  • suitable flame retardant synergists are dicumyl and dicumyl peroxide.
  • a preferred combination consists of 0.6 to 5% by weight of organic bromine compound and 0.1 to 1.0% by weight of the C-C or O-O-unstable organic compound.
  • the expandable styrene polymers according to the invention can be prepared by various processes.
  • the soot particles are added to a melt of the styrene polymer, preferably in an extruder.
  • the blowing agent is metered into the melt.
  • the soot particles can also be incorporated into a melt of styrene polymer containing blowing agent. The polystyrene melt containing the blowing agent and soot particles is pressed out and comminuted into granules containing blowing agent.
  • blowing agent to the styrene polymers containing soot particles in a separate process step.
  • the granules are then preferably impregnated with the blowing agent in aqueous suspension.
  • the finely divided soot particles can be added directly to a polystyrene melt or preferably fed into an extruder together with solid polystyrene granules, the polystyrene granules melted and mixed with the soot particles.
  • a dispersing agent e.g. Mineral oil, a phthalic or stearic acid ester or a polyethylene glycol.
  • the soot particles can also be added to the melt in the form of a concentrate in polystyrene.
  • soot particles around the course of the suspension polymerization. They can be added to the monomeric styrene before the suspension or added to the reaction mixture in the course, preferably towards the end of the polymerization cycle.
  • the blowing agent is added during the course of the polymerization, but it can also be incorporated into the styrene polymer afterwards.
  • the blowing agent is added in the usual amounts of about 5 3 to 10% by weight, based on the weight of the polymer.
  • Aliphatic hydrocarbons having 3 to 10, preferably 4 to 6, carbon atoms are usually used as blowing agents.
  • the expandable, carbon black-containing styrene polymers according to the invention can be processed into polystyrene foams with densities of 5-35 g / 1, preferably 8 to 25 g / 1 and in particular 10-15 g / 1.
  • the expandable particles are pre-foamed. This is usually done by heating the particles with water vapor in so-called previewers.
  • the pre-foamed particles are then welded to form bodies.
  • the pre-foamed particles are brought into non-gas-tight forms and water vapor is applied. After cooling, the molded parts can be removed.
  • the foams produced from the expandable styrene polymers 25 according to the invention are notable for excellent thermal insulation. This effect is particularly evident at low densities.
  • the thermal conductivity could be reduced from 38 mW / mK to 30 30 mW / mK, a value that otherwise only of Poly ⁇ styrene foams with densities above 35 g / 1 is achieved.
  • Another object of the invention are polystyrene particle foams with a density of ⁇ 35 g / 1, containing - each 35 based on the polymer -
  • soot particles 0.05 to 25% by weight of soot particles
  • the expandable styrene polymers according to the invention can be processed into foams of low density without any problems. There is no loss of blowing agent or disruption of the cellular structure of the foams, although the person skilled in the art had to assume that the soot acts as a nucleating agent and would lead to an undesirable fine-cell nature of the foam and poor welding. In addition, despite the addition of soot particles, self-extinguishing foams can be produced which pass fire test B2 and in most cases also B1.
  • the foams according to the invention can be used for the thermal insulation of buildings and parts of buildings, for the thermal insulation of machines and household appliances and as packaging materials.
  • the flame retardant was omitted in comparison test 2V, and soot in comparison test 3V.
  • the expandable beads obtained were washed, sieved to 0.7-1 mm and dried.
  • the beads were pre-foamed by the action of water vapor and after storage for one day by further treatment with steam in a closed mold they were welded into foam blocks with a density of 15 g / l.
  • the thermal conductivity values measured at 10 ° C according to DIN 52 612 are summarized in Table 1.
  • Melted polystyrene with an average molecular weight (M w ) of 220,000 and a content of 2.1% HBCD and 0.42% dicumyl was in a heated twin-screw extruder at a melt temperature of about 210 "C flame black (as 20% igger batch in polystyrene) and 6.0% by weight of a mixture of 80% n-pentane and 20% iso-pentane, the homogenized mixture was pressed through a nozzle plate of 1 mm nozzle diameter at a melt temperature of 180 ° C. and the Polymer strand pulled directly through a 18 "C water bath.
  • the strands were cooled on the surface so quickly that they did not foam.
  • Example 4 foaming to a density of 10 g / 1, in Example 5 to a density of 15 g / 1.
  • the expandable gianulates obtained were processed into foam blocks as described in Example 1.

Abstract

L'invention concerne des polymérisats de styrène expansibles particulaires, qui contiennent, par rapport au poids des polymères, entre 0,05 et 25 % en poids de particules de noir de fumée réparties uniformément et peuvent être traités pour former des produits alvéolaires auto-extincteurs d'une masse volumique </= 35 g/l.
EP97924003A 1996-05-28 1997-05-26 Polymerisats de styrene expansibles contenant des particules de noir de fumee Ceased EP0902804A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19621299 1996-05-28
DE19621299 1996-05-28
PCT/EP1997/002684 WO1997045477A1 (fr) 1996-05-28 1997-05-26 Polymerisats de styrene expansibles contenant des particules de noir de fumee

Publications (1)

Publication Number Publication Date
EP0902804A1 true EP0902804A1 (fr) 1999-03-24

Family

ID=7795440

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97924003A Ceased EP0902804A1 (fr) 1996-05-28 1997-05-26 Polymerisats de styrene expansibles contenant des particules de noir de fumee

Country Status (3)

Country Link
EP (1) EP0902804A1 (fr)
AU (1) AU2960897A (fr)
WO (1) WO1997045477A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2431410A1 (fr) 2010-09-17 2012-03-21 Technisch Bureel Panigo N.V. Plaques de mousse de polystyrene résistant à la lumière solaire, ayant une forte capacité d'isolation thermique
EP2431148A1 (fr) 2010-09-17 2012-03-21 Technisch Bureel Panigo N.V. Production de feuilles polymérisées en styrène stratifié
WO2018069186A1 (fr) 2016-10-10 2018-04-19 Total Research & Technology Feluy Polymères aromatiques vinyliques expansibles améliorés
WO2018069178A1 (fr) 2016-10-10 2018-04-19 Total Research & Technology Feluy Polymères aromatiques de vinyle expansibles améliorés
WO2018069185A1 (fr) 2016-10-10 2018-04-19 Total Research & Technology Feluy Polymères aromatiques de vinyle expansibles améliorés
WO2021043552A1 (fr) 2019-09-04 2021-03-11 Total Research & Technology Feluy Polymères aromatiques vinyliques expansibles présentant une ininflammabilité améliorée

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DE19812856A1 (de) * 1998-03-24 1999-09-30 Basf Ag Verfahren zur Herstellung wasserexpandierbarer Styrolpolymerisate
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DE10226749B4 (de) 2002-06-14 2014-09-04 Basf Se Verfahren zur Herstellung von expandierbarem Polystyrol
DE102004028768A1 (de) 2004-06-16 2005-12-29 Basf Ag Styrolpolymer-Partikelschaumstoffe mit verringerter Wärmeleitfähigkeit
DE102004034527A1 (de) * 2004-07-15 2006-02-16 Basf Ag Verfahren zur Herstellung von expandierbaren Styrolpolymeren mit verbesserter Expandierbarkeit
DE102004034515A1 (de) * 2004-07-15 2006-02-02 Basf Ag Selbstverlöschender Styrolpolymer-Partikelschaumstoff
DE102004034516A1 (de) 2004-07-15 2006-02-16 Basf Ag Verfahren zur Herstellung von flammgeschütztem, expandierbarem Polystyrol
DE102004034514A1 (de) * 2004-07-15 2006-02-16 Basf Ag Synergistische Flammschutzmischungen für Polystyrolschaumstoffe
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DE102005027549A1 (de) * 2005-06-14 2006-12-21 Basf Ag Mehrkomponentenformkörper mit Polyesterschichten
PL2062935T3 (pl) 2007-11-21 2012-09-28 Basf Se Sposób wprowadzania cząstek substancji stałych do stopów polimerowych
CN101868496A (zh) 2007-11-21 2010-10-20 巴斯夫欧洲公司 防火的可发性苯乙烯聚合物及其制备方法
ES2561206T5 (es) 2008-05-02 2023-09-20 Basf Se Espumas de poliestireno con un bajo contenido de metal
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IT1392391B1 (it) 2008-12-19 2012-03-02 Polimeri Europa Spa Composizioni di polimeri vinilaromatici espansibili a migliorata capacita' di isolamento termico, procedimento per la loro preparazione ed articoli espansi da loro ottenuti
IT1396193B1 (it) 2009-10-07 2012-11-16 Polimeri Europa Spa Composizioni polimeriche nanocomposite termoplastiche espansibili con migliorata capacita' di isolamento termico.
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WO2012032022A1 (fr) 2010-09-10 2012-03-15 Total Petrochemicals Research Feluy Polymères aromatiques de vinyle expansibles
CN103703062B (zh) 2011-06-23 2015-08-05 道达尔研究技术弗吕公司 改进的能膨胀的乙烯基芳族聚合物
EP2683763A1 (fr) 2011-06-27 2014-01-15 Total Research & Technology Feluy Polymères aromatiques vinyliques expansibles contenant du graphite
ES2632477T3 (es) 2012-12-28 2017-09-13 Total Research & Technology Feluy Polímeros vinil aromáticos expansibles que comprenden partículas de coque en agujas plaquetarias
KR101782702B1 (ko) 2013-02-05 2017-09-27 에스지엘 카본 에스이 경성 발포 폴리스티렌
FR3009561B1 (fr) 2013-08-06 2017-12-22 Arkema France Procede de preparation de polystyrene expansible noir
BR112016007331B1 (pt) 2013-10-04 2021-01-12 Orion Engineered Carbons Gmbh uso de um material de carbono particulado
DE102014213685A1 (de) 2014-07-15 2016-01-21 Sgl Carbon Se Neuartige Polystyrolhartschaumstoffe
MA41339B1 (fr) 2015-01-14 2019-05-31 Synthos Sa Granulés de polymère vinylique aromatique expansible et mousse de polymère aromatique de vinyle expansé comprenant de composites géopolymères, ainsi que leur utilisation
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2431410A1 (fr) 2010-09-17 2012-03-21 Technisch Bureel Panigo N.V. Plaques de mousse de polystyrene résistant à la lumière solaire, ayant une forte capacité d'isolation thermique
EP2431148A1 (fr) 2010-09-17 2012-03-21 Technisch Bureel Panigo N.V. Production de feuilles polymérisées en styrène stratifié
WO2018069186A1 (fr) 2016-10-10 2018-04-19 Total Research & Technology Feluy Polymères aromatiques vinyliques expansibles améliorés
WO2018069178A1 (fr) 2016-10-10 2018-04-19 Total Research & Technology Feluy Polymères aromatiques de vinyle expansibles améliorés
WO2018069185A1 (fr) 2016-10-10 2018-04-19 Total Research & Technology Feluy Polymères aromatiques de vinyle expansibles améliorés
US11834563B2 (en) 2016-10-10 2023-12-05 Totalenergies Onetech Belgium Expandable vinyl aromatic polymers
WO2021043552A1 (fr) 2019-09-04 2021-03-11 Total Research & Technology Feluy Polymères aromatiques vinyliques expansibles présentant une ininflammabilité améliorée

Also Published As

Publication number Publication date
AU2960897A (en) 1998-01-05
WO1997045477A1 (fr) 1997-12-04

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