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WO1987000187A1 - Microcapsules d'agents ignifuges - Google Patents

Microcapsules d'agents ignifuges Download PDF

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Publication number
WO1987000187A1
WO1987000187A1 PCT/EP1986/000370 EP8600370W WO8700187A1 WO 1987000187 A1 WO1987000187 A1 WO 1987000187A1 EP 8600370 W EP8600370 W EP 8600370W WO 8700187 A1 WO8700187 A1 WO 8700187A1
Authority
WO
WIPO (PCT)
Prior art keywords
microincapsulated
flame retarders
flame
retarders
membrane
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
PCT/EP1986/000370
Other languages
English (en)
Inventor
Danilo Cicuto
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.)
CAPSALARM Sarl
Original Assignee
CAPSALARM Sarl
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 CAPSALARM Sarl filed Critical CAPSALARM Sarl
Publication of WO1987000187A1 publication Critical patent/WO1987000187A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients

Definitions

  • the present invention relates to flame retarders for rigid and flexible synthetic foams, binding resins and plastics in general.
  • the various flame retarders are microincapsulated, that is, the particles of said retarders, at the level of each single crystal or micro ⁇ scopic drop, are completely enveloped by an inert and atoxic stable microscopic film, according to various mi- croincapsulation processes, so attaining the following advantages: - transformation of any flame retarder, independently on the nature and characteristics thereof, into a simple inert additive till the moment when temperature exerted by fire causes the microcapsules to open, so releasing the flame retarder contained therein, which only from that moment carries on its action;
  • All of the known flame retarders' may be microincap ⁇ sulated according to the present invention, particularly all the known organic and inorganic halogenated and/or phosphorated derivatives (used to this scope), such as decabromodiphenyloxide, octabro odiphenyloxide, tetrabro- moparaxylene, hexabromocyclododecane, chlorophosphorated esters in general, tris-(2, 3-dibromopropyl)phosphate, trichloroethylphosphate, tetrabromophthalic anhydride, tetrabromobisphenol, red phosphorus, ammonium polyphospha ⁇ te, dibromopropanol and mixtures thereof.
  • decabromodiphenyloxide octabro odiphenyloxide
  • tetrabro- moparaxylene hexabromocyclododecane
  • Microincapsulation of • said flame retarders may be carried out according to various techniques, such as the method based on gelatins having different viscosities, the one based on gelatins and gum arabic, those based on cel ⁇ lulose derivatives and the like.
  • 100 Ml of a 10% gelatin solution, 100 g of tetra- bromoparaxylene having a particle size of 150 to 300 mi ⁇ cron, 100 ml of gum arabic in solution and 300 ml of water were mixed in a vessel and stirred at a temperature from 45 to 50°C.
  • the pH of the solution was adjusted to 4.2 and, during stirring, temperature was slowly lowered to 25°, at which temperature a membrane formed around the particles; thereafter the vessel was quickly cooled and stirring was continued during one hour, in order to make the membrane more rigid.
  • the obtained microcapsules have a weight ratio of 5:1 with respect to the product, i.e. 20 g of material making up the membrane for 100 g of incapsulated tetrabro- moparaxylene.
  • Example 2 The above cited Example may be carried out varying the compound/membrane ratio in the following percentages: 10:1; 20:1; 40:1. The same Example may carried out, for all the above cited compound/membrane ratios, using particles of 10 to 1000 microns size. Particularly, when tetrabromoparaxylene is used as flame retarding agent in flexible polyurethan foams, the maximum effectiveness was found for crystal sizes from 50 to 250 microns. EXAMPLE 2
  • 100 Ml of a 10% gelatin solution was placed in a vessel, at a temperature from 45 to 50°C, under stirring, then 100 g of water, 15 ml of a 5% sodium hexametaphospha- te solution and 100 g of decabromodiphenyloxide having particle size of 150 to 300 microns were added, under stirring. pH was adjusted to about 4 and the temperature of the solution was first slowly lowered to 25°C, then quickly lowered to 10°, stirring for one hour at this temperature in order to make more rigid the membrane. As in Example 1, microcapsule membranes were hard ⁇ ened by addition of glutaraldehyde.
  • Example 2 Water separation and microcapsule drying were car ⁇ ried out as described in Example 1. The resulting microcapsules have a membrane/compo ⁇ und weight ratio of 1:10.
  • membrane/compound weight ratio as well as microcapsule size may be varied.
  • EXAMPLE 3 250 Ml of cyclohexane, 4 g of ethylcellulose and 4 g of carboxylated wax were placed in a vessel. Temperature was raised to 70°C, under strong stirring, to complete dissolution. Then 30 g of ammonium polyphosphate was ad ⁇ ded, and temperature was lowered to 20°C, continuing stir- ring. The reaction mixture was filtered, the filtrate was repeatedly washed with pure cyclohexane. Microincapsulated ammonium polyphosphate was then dried in oven, at a tempe ⁇ rature not higher than 40°C.
  • red phosphorus 100 Grams of red phosphorus is added to 300 g of H O, 2 g of urea, 5 g of resorcine and 40 ml of 40% for ⁇ maldehyde.
  • the pH is slowly brought down to 1.5 to obtain a polymerization yielding an urea-formaldehyde membrane including red phosphorus.
  • the water is then separated from the obtained microcapsules which are dried.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

L'invention concerne des microcapsules d'agents ignifuges tels que l'oxyde de bromodiphényle, l'oxyde d'octabromodiphényle, le tétrabromoparaxylène, l'hexabromocyclododécane, les esters chlorophosphorés en général, le tris-(2,3-dibromopropyle)phosphate, le phosphate de trichloroéthyle, l'anhydride tetrabromophtalique, le tétrabromobisphénol, le phosphore amorphe, le polyphosphate d'ammonium, le dibromopropanol et similaires, de même que des microcapsules contenant des mélanges de ceux-ci. Ces agents ignifuges sont pourvus d'une membrane inerte et imperméable qui isole chaque cristal ou goutte de liquide de l'environnement ambiant, en empêchant ainsi l'occurrence de réactions chimiophysiques indésirables et en éliminant la toxicité des agents ignifuges eux-mêmes.
PCT/EP1986/000370 1985-06-26 1986-06-24 Microcapsules d'agents ignifuges Ceased WO1987000187A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT21292A/85 1985-06-26
IT21292/85A IT1201424B (it) 1985-06-26 1985-06-26 Ritardanti di fiamma microincapsulati

Publications (1)

Publication Number Publication Date
WO1987000187A1 true WO1987000187A1 (fr) 1987-01-15

Family

ID=11179641

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1986/000370 Ceased WO1987000187A1 (fr) 1985-06-26 1986-06-24 Microcapsules d'agents ignifuges

Country Status (3)

Country Link
EP (1) EP0227764A1 (fr)
IT (1) IT1201424B (fr)
WO (1) WO1987000187A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2210377A (en) * 1987-09-25 1989-06-07 Plessey Co Plc Microencapsulated flame retardant: encapsulated semiconductor
DE4300390A1 (en) * 1992-08-22 1993-07-01 Tech Wissenschaftliche Ges Thi Preventing burning of plastics materials or plastics composites - by incorporating conventional flame retardant as microcapsules
WO2000014094A1 (fr) * 1998-09-08 2000-03-16 Isle Firestop Limited Ralentisseur de combustion de materiaux polymeres
EP1262453A2 (fr) 2001-06-01 2002-12-04 Bayer Ag Microencapsulation de phosphore rouge
EP1262452A3 (fr) * 2001-06-01 2003-10-15 Bayer Ag Phosphore rouge microencapsulé
US7585443B2 (en) 2004-05-20 2009-09-08 Albemarle Corporation Pelletized brominated anionic styrenic polymers and their preparation and use

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5543447A (en) * 1994-09-28 1996-08-06 Southwest Research Institute Stabilization of red amorphous phosphorus by ordered polymeric structures for the manufacture of non-emissive fire retardant plastics
CN107022205B (zh) * 2017-04-28 2018-10-09 四川理工学院 一种表面疏水改性聚磷酸铵的制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4138356A (en) * 1973-08-22 1979-02-06 Champion International Corporation Encapsulated flame retardant system
US4208317A (en) * 1975-06-10 1980-06-17 Rhone-Poulenc Industries Flameproofed plastic compositions
EP0083768A1 (fr) * 1981-12-19 1983-07-20 Kanegafuchi Kagaku Kogyo Kabushiki Kaisha Composition de résine résistant à la flamme
EP0033361B1 (fr) * 1979-12-08 1984-01-18 Hoechst Aktiengesellschaft Agent ignifuge à base de polyphosphates d'ammonium

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4138356A (en) * 1973-08-22 1979-02-06 Champion International Corporation Encapsulated flame retardant system
US4208317A (en) * 1975-06-10 1980-06-17 Rhone-Poulenc Industries Flameproofed plastic compositions
EP0033361B1 (fr) * 1979-12-08 1984-01-18 Hoechst Aktiengesellschaft Agent ignifuge à base de polyphosphates d'ammonium
EP0083768A1 (fr) * 1981-12-19 1983-07-20 Kanegafuchi Kagaku Kogyo Kabushiki Kaisha Composition de résine résistant à la flamme

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2210377A (en) * 1987-09-25 1989-06-07 Plessey Co Plc Microencapsulated flame retardant: encapsulated semiconductor
DE4300390A1 (en) * 1992-08-22 1993-07-01 Tech Wissenschaftliche Ges Thi Preventing burning of plastics materials or plastics composites - by incorporating conventional flame retardant as microcapsules
WO2000014094A1 (fr) * 1998-09-08 2000-03-16 Isle Firestop Limited Ralentisseur de combustion de materiaux polymeres
US6863846B1 (en) 1998-09-08 2005-03-08 Isle Firestop Limited Combustion retardant for polymeric materials
EP1262453A2 (fr) 2001-06-01 2002-12-04 Bayer Ag Microencapsulation de phosphore rouge
EP1262452A3 (fr) * 2001-06-01 2003-10-15 Bayer Ag Phosphore rouge microencapsulé
EP1262453A3 (fr) * 2001-06-01 2003-10-15 Bayer Ag Microencapsulation de phosphore rouge
US6765047B2 (en) 2001-06-01 2004-07-20 Bayer Aktiengesellschaft Microencapsulation of red phosphorus
US6846854B2 (en) 2001-06-01 2005-01-25 Bayer Aktiengesellschaft Microencapsulated red phosphorus
US7585443B2 (en) 2004-05-20 2009-09-08 Albemarle Corporation Pelletized brominated anionic styrenic polymers and their preparation and use

Also Published As

Publication number Publication date
EP0227764A1 (fr) 1987-07-08
IT8521292A0 (it) 1985-06-26
IT1201424B (it) 1989-02-02

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