EP1383838A1 - Hydroxyde de magnesium a surface recouverte - Google Patents

Hydroxyde de magnesium a surface recouverte

Info

Publication number
EP1383838A1
EP1383838A1 EP02735208A EP02735208A EP1383838A1 EP 1383838 A1 EP1383838 A1 EP 1383838A1 EP 02735208 A EP02735208 A EP 02735208A EP 02735208 A EP02735208 A EP 02735208A EP 1383838 A1 EP1383838 A1 EP 1383838A1
Authority
EP
European Patent Office
Prior art keywords
magnesium hydroxide
coated
alkyl
coated magnesium
branched
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Withdrawn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
EP02735208A
Other languages
German (de)
English (en)
Inventor
Joachim Schaeling
René Herbiet
Hans Peter Hillekamps
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.)
Albemarle Corp
Original Assignee
Albemarle Corp
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 Albemarle Corp filed Critical Albemarle Corp
Priority to EP02735208A priority Critical patent/EP1383838A1/fr
Publication of EP1383838A1 publication Critical patent/EP1383838A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/028—Compounds containing only magnesium as metal

Definitions

  • the invention relates to a surface-coated magnesium hydroxide with improved efflorescence when used as a filler in polyamides, and to a process for its production.
  • Magnesium hydroxide is used as a flame-retardant filler in thermoplastics, especially in those whose processing temperature is above the decomposition temperature of other flame retardants such.
  • B. is aluminum hydroxide.
  • These plastics include, in particular, polyamides.
  • Herfur are usually used A inosilane.
  • the efflorescence consists of a whitish, adherent coating that covers the entire surface and makes the end product unsightly and gives rise to complaints.
  • the usual climate change test is that the samples are alternately exposed to 100% relative humidity for 12 hours at room temperature, then for 12 hours at 40 ° C, then again for 12 hours at room temperature, etc.
  • the whitish coating forms after a few weeks.
  • the object of the present invention was therefore to provide magnesium hydroxides with suitable coatings which do not give rise to any formation of deposits or which significantly reduce the tendency to form deposits.
  • this object is achieved by the coated magnesium hydroxide according to claim 1 and the manufacturing method according to claim 10.
  • magnesium hydroxide here and below includes not only the compound Mg (OH) but also other natural or synthetic products which contain magnesium ions and predominantly hydroxide ions as anions. Suitable ones
  • Magnesium hydroxides are, for example, brucite, natural or synthetic magnesium hydroxycarbonates such as huntite or hydromagnesite, or synthetic magnesium hydroxides as are sold, for example, by Alusuisse Martinswerk GmbH under the trademark Magnifin ® . It is of course also within the scope of the invention to use mixtures of the magnesium hydroxides mentioned above.
  • Alkyl groups here and in the following are to be understood in each case as linear or branched primary, secondary or tertiary alkyl groups with the number of carbon atoms indicated in each case.
  • Linear or single-branched primary or secondary alkyl groups such as methyl, ethyl, propyl, isopropyl, butyl, isobutyl, hexyl, octyl, isooctyl (6-methylheptyl), 2-ethylhexyl, dodecyl, tetradecyl, hexadecyl, octadecyl etc. are preferred.
  • C 8-30 acyl groups from any of the alkyl groups defined above and a carbonyl compound groups (together) from 8 to 30 carbon atoms such as, for example, octanoyl (capryloyl), decanoyl (caprinoyl), dodecanoyl (lauroyl), tetradecanoyl (myristoyl)
  • octanoyl capryloyl
  • decanoyl caprinoyl
  • dodecanoyl laauroyl
  • tetradecanoyl myristoyl
  • hexadecanoyl paltmitoyl
  • octa-decanoyl stearoyl
  • isooctadecanoyl isostearoyl
  • fatty acid, alkylsilanes, organic titanates or organic zirconates which can be used according to the invention and the aminosilanes are known compounds and are frequently commercially available.
  • Fatty acids are available, for example, from Cognis (formerly Henkel KGaA) or Unichema in pure form or as mixtures under various brand names.
  • Alkylsilanes and aminosilanes are for example from Degussa-Hüls AG under the Dynasylan ® brand and organic titanates and zirconates from DuPont under the TYZOR ® brand.
  • the commercially available compounds 3-aminopropyltrimethoxysilane and 3-aminopropyltriethoxysilane are preferably used as aminosilanes.
  • Both saturated and unsaturated fatty acids and fatty acids with additional functional groups such as amino or hydroxy fatty acids can be used as fatty acids.
  • Saturated fatty acids having 10 to 24 carbon atoms are preferably used. These can be used both as pure or technically pure substances and as homolog mixtures, as are obtained, for example, when natural fats are cleaved.
  • the preferred alkylsilanes can be represented by the formula R ! Si (OR 2 ) 3 can be described.
  • R 1 denotes a linear or branched alkyl group with 3 to
  • R is a linear or branched d- 6 alkyl group.
  • Alkylsilanes in which R is linear or branched are particularly preferred
  • organic titanates preference is given to those which have the formula
  • R 3 OTi (OR 4 ) 3 can be described.
  • R 3 is a linear or branched one
  • R 4 is a linear or branched C-5_ 12 alkyl or C 8 _ 30 acyl group.
  • the organic titanate in which R 3 is isopropyl and t is isostearoyl is particularly preferred.
  • R 4 are the same and isooctyl or 2-ethylhexyl.
  • the organic zirconates used are preferably those which can be described by the formula R 5 OZr (OR 6 ) 3 .
  • R 5 is linear or branched C ⁇ _ ⁇ 2 alkyl and R 6 linear or branched Cs- 12 alkyl or C 8 -3 0 -acyl.
  • the surface-coated magnesium hydroxides according to the invention can thereby be prepared using an untreated magnesium hydroxide in a suitable mixing device
  • Components (a) and (b) can be coated either successively or simultaneously (by using a mixture of the components). If the coating is carried out in two steps, component (a) and then component (b), ie the aminosilane, are preferably applied first.
  • the surface-coated magnesium hydroxides according to the invention are preferably used as fillers in polyamides.
  • polyamide compounds characterized by a content of the surface-coated magnesium hydroxides according to the invention for example with polyamide 6 as the polyamide component, are likewise a subject of the invention.
  • the following examples show the production and use of the surface-coated magnesium hydroxides according to the invention, without any restriction to the specific embodiments being implemented.
  • the coating was carried out in a Henschel mixer using a method known per se.
  • the compounding was carried out on a Buss kneader in a manner customary for highly filled plastic systems.
  • the undyed type Ultramid ® B3L (polyamide 6) from BASF AG was used as the polyamide.
  • the commercially available magnesium hydroxide type MAGNIFIN H 5 IV from Alusuisse Martinswerk GmbH was used, coated exclusively with an aminosilane.
  • the number 5 denotes a magnesium hydroxide with an average BET value (specific surface area) of 5 m z / g.
  • the magnesium hydroxide MAGNIFIN H 5 from Alusuisse Martinswerk GmbH was used as the uncoated substrate. led coating agents was surface modified. The surface modification was carried out according to known methods, such as. B. in WO-A-00/15710 or WO-A-96/26240. A Henschel mixer was used in each of the examples. The filler was used in an amount of 55% by weight of magnesium hydroxide to 45% by weight of polyamide. Polyamide platelets with a thickness of 3 mm and a surface of 3x3 cm 2 were produced by injection molding and exposed to the changing climate described above. The whitish efflorescence was assessed after 30, 60 and 90 days by visual assessment. 4 classes were distinguished and rated as follows: 1 (very little topping), 2 (little topping), 3 (a lot of topping) and 4 (very much topping).
  • the filler coating of Compound No. 2 consisted of 1.0% (based on the filler) of a commercially available lauric acid (Edenor ® C12 98-100 from Cognis Deutschland GmbH (formerly Henkel KGaA)) and 3-aminopropyltriethoxysilane (Dynasylan ® AMEO from Degussa -Hüls AG).
  • the filler coating of Compound No. 3 consisted of 1.0% (based on the filler) of isopropoxytris (isostearoyloxy) titanium (TYZOR ® ISTT from DuPont de Nemours (Germany) GmbH) and 3-aminopropyltriethoxysilane (Dynasylan ® AMEO from Degussa-Hüls AG).
  • the filler coating of Compound No. 4 consisted of 1.0% (based on the filler) of a longer-chain alkylsilane (hexadecyltrimethoxysilane, Dynasylan ® 9116 from Degussa-Hüls AG) and 3-aminopropyltriethoxysilane (Dynasylan ® AMEO from Degussa-Hüls AG).
  • a longer-chain alkylsilane hexadecyltrimethoxysilane, Dynasylan ® 9116 from Degussa-Hüls AG
  • 3-aminopropyltriethoxysilane Dynasylan ® AMEO from Degussa-Hüls AG.
  • Table 2 shows the influence of the coating sequence on the efflorescence after 30 days. 0.5% (based on the filler) of a technical behenic acid (docosanic acid, Prifrac ® 2987 from Unichema Chemie GmbH) and 3-aminopropyltriethoxysilane (Dynasylan ® AMEO from Degussa-Hüls AG) were used here.
  • a technical behenic acid docosanic acid, Prifrac ® 2987 from Unichema Chemie GmbH
  • 3-aminopropyltriethoxysilane Dynasylan ® AMEO from Degussa-Hüls AG

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

L'invention concerne des hydroxydes de magnésium à surface recouverte d'un revêtement constitué de: (a) 0,2 à 5 % en poids, par rapport au poids de l'hydroxyde de magnésium, d'au moins un composé du groupe comprenant (i) des acides gras présentant 8 à 30 atomes de carbone, (ii) des alkylsilanes comportant au moins un groupe alkyle présentant 3 atomes de carbone, (iii) des titanates organiques et (iv) des zirconates organiques; et (b) 0,2 à 5 % en poids, par rapport au poids de l'hydroxyde de magnésium, d'un aminosilane. Les hydroxydes de magnésium selon l'invention se caractérisent par une tendance réduite à "exsuder" lorsqu'ils sont utilisés comme matières premières de charge retardatrice de combustion dans des polyamides.
EP02735208A 2001-04-05 2002-04-02 Hydroxyde de magnesium a surface recouverte Withdrawn EP1383838A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP02735208A EP1383838A1 (fr) 2001-04-05 2002-04-02 Hydroxyde de magnesium a surface recouverte

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP01108643 2001-04-05
EP01108643 2001-04-05
PCT/EP2002/003641 WO2002081574A1 (fr) 2001-04-05 2002-04-02 Hydroxyde de magnesium a surface recouverte
EP02735208A EP1383838A1 (fr) 2001-04-05 2002-04-02 Hydroxyde de magnesium a surface recouverte

Publications (1)

Publication Number Publication Date
EP1383838A1 true EP1383838A1 (fr) 2004-01-28

Family

ID=8177060

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02735208A Withdrawn EP1383838A1 (fr) 2001-04-05 2002-04-02 Hydroxyde de magnesium a surface recouverte

Country Status (3)

Country Link
US (1) US20040127602A1 (fr)
EP (1) EP1383838A1 (fr)
WO (1) WO2002081574A1 (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7601780B2 (en) * 2005-07-18 2009-10-13 E.I. Du Pont De Nemours And Company Increased bulk density of fatty acid-treated silanized powders and polymers containing the powders
US7686986B2 (en) * 2006-01-05 2010-03-30 Headwaters Technology Innovation, Llc Magnesium hydroxide nanoparticles, methods of making same and compositions incorporating same
US20070287773A1 (en) * 2006-06-13 2007-12-13 Ramdatt Philbert E Surface-modified non-halogenated mineral fillers
US20070287791A1 (en) * 2006-06-13 2007-12-13 Ramdatt Philbert E Polymer compositions containing surface-modified non-halogenated mineral fillers
AU2007270757A1 (en) * 2006-06-21 2008-01-10 Martinswerk Gmbh Coated magnesium hydroxide particles produced by mill-drying
EP2029486A2 (fr) * 2006-06-21 2009-03-04 Martinswerk GmbH Procédé servant à produire des particules d'hydroxyde d'aluminium
DE102008031361A1 (de) * 2008-07-04 2010-01-14 K+S Aktiengesellschaft Verfahren zur Herstellung von grob- und/oder nanoskaligen, gecoateten, desagglomerierten Magnesiumhydroxiparikeln
DE102008031360A1 (de) * 2008-07-04 2010-01-14 K+S Ag Verfahren zum Herstellen von aushärtbaren Massen, enthaltend grob- und/oder nanoskalige, gecoatete, desagglomerierte und bevorzugt funktionalisierte Magnesiumhydroxidpartikel, sowie von ausgehärteten thermoplastischen oder duroplastischen Polymeren bzw. Kompositen, enthaltend desagglomerierte und homogen verteilte Magnesiumhydroxidfüllstoffpartikel
DE102008038667A1 (de) 2008-08-12 2010-02-25 K+S Ag Herstellungsverfahren von thermoplastischen Polymeren enthaltend grobskalige und/oder nanoskalige, gecoatete, desagglomerierte Magnesiumhydroxidpartikel und eine Vorrichtung hierzu
KR20210099613A (ko) 2018-12-04 2021-08-12 바스프 에스이 폴리에틸렌 또는 폴리프로필렌 물품

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CS241640B1 (cs) * 1984-02-02 1986-04-17 Tomas Sverak Práškové plnivo na bázi hydroxidu horečnatého z přírodních karbonátů
JPH0354233A (ja) * 1989-04-19 1991-03-08 Furukawa Electric Co Ltd:The 複合難燃剤およびそれを含有する難燃性樹脂組成物
IE64663B1 (en) * 1989-11-01 1995-08-23 Lonza Ag Surface-modified fillers
JP3901752B2 (ja) * 1995-07-20 2007-04-04 出光興産株式会社 難燃性ポリスチレン系樹脂組成物及びポリスチレン系樹脂成形体
SK282487B6 (sk) * 1997-04-17 2002-02-05 Duslo, A. S. Hydroxid horečnatý s povrchom upraveným povrchovo aktívnym činidlom, spôsob jeho prípravy a polymérny kompozitný materiál so zvýšenou odolnosťou proti horeniu s jeho obsahom
JP3904170B2 (ja) * 1998-02-12 2007-04-11 住友ベークライト株式会社 難燃性組成物
US6376077B1 (en) * 1998-04-10 2002-04-23 Kyowa Chemical Industry Co., Ltd. Process for the production of coupling agent-treated inorganic particles and use thereof
EP1124895B1 (fr) * 1998-09-14 2004-05-19 Albemarle Corporation Composition de charge modifiee en surface

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO02081574A1 *

Also Published As

Publication number Publication date
WO2002081574B1 (fr) 2003-01-16
US20040127602A1 (en) 2004-07-01
WO2002081574A1 (fr) 2002-10-17

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