WO2006120578A2 - Synthese de phase gazeuse de polymeres de phosphore polyhydrure - Google Patents

Synthese de phase gazeuse de polymeres de phosphore polyhydrure Download PDF

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Publication number
WO2006120578A2
WO2006120578A2 PCT/IB2006/001880 IB2006001880W WO2006120578A2 WO 2006120578 A2 WO2006120578 A2 WO 2006120578A2 IB 2006001880 W IB2006001880 W IB 2006001880W WO 2006120578 A2 WO2006120578 A2 WO 2006120578A2
Authority
WO
WIPO (PCT)
Prior art keywords
polyhydride
phosphorus polymer
gas phase
phosphorus
phosphine
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/IB2006/001880
Other languages
English (en)
Other versions
WO2006120578A3 (fr
Inventor
Jason W. Flora
Daryl L. Faustini
Harvey J. Grubbs
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.)
Philip Morris Products SA
Original Assignee
Philip Morris Products SA
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 Philip Morris Products SA filed Critical Philip Morris Products SA
Publication of WO2006120578A2 publication Critical patent/WO2006120578A2/fr
Publication of WO2006120578A3 publication Critical patent/WO2006120578A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
    • C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus

Definitions

  • the invention relates to gas phase synthesis of a polyhydride phosphorus polymer, conversion thereof to a heat/fire resistant film/coating and articles incorporating same.
  • a method of making a polyhydride phosphorus polymer comprises subjecting phosphine gas to gas phase synthesis.
  • the gas phase synthesis preferably utilizes a free radical such as nitric oxide or nitrous oxide as an initiator.
  • Phosphine gas may be generated at point of use by exposure of a metal phosphide such as, for example, magnesium phosphide, calcium phosphide or aluminum phosphide, to ambient humidity.
  • the polyhydride phosphorous polymer can be formed in a sealed vessel by adjusting amounts of PH 3 and NO to deposit the polyhydride phosphorus polymer at a desired rate.
  • the polyhydride phosphorus polymer can be used as an intermediate product to make other phosphorus compounds.
  • the polyhydride phosphorus polymer can be deposited on a substrate such as an article of clothing or on a part intended for use in a high temperature environment.
  • the polyhydride phosphorus polymer can be converted to a heat/fire resistant film/coating by oxidizing the polyhydride phosphorus polymer.
  • the polyhydride phosphorus polymer can be oxidized in a gaseous environment or by contacting the polyhydride phosphorus polymer with a solution of hydrogen peroxide.
  • the coated article can be immersed in a solution of hydrogen peroxide to oxidize the polyhydride phosphorus polymer preferably to a polymeric phosphine oxide film/coating.
  • Figure 1 shows a scanning electron microscopy image of a polyhydride phosphorus polymer formed in via gas phase synthesis; and Figure 2 shows elemental analysis of the polyhydride phosphorus polymer shown in Figure 1.
  • Yellow amorphous polyhydride phosphorus polymers (P x H 1 , wherein x and y are each greater than 1) can be formed via gas phase synthesis. These solid phosphorus hydrides are highly polymeric and are insoluble in common solvents .
  • the gas phase synthesis of polyhydride phosphorus polymers involves phosphine gas interaction with an initiator such as nitric oxide (NO) and/or nitrogen dioxide (NO 2 ) (from the oxidation of NO) promoting the polymerization.
  • an initiator such as nitric oxide (NO) and/or nitrogen dioxide (NO 2 ) (from the oxidation of NO)
  • the polyhydride phosphorus polymer can be produced by any suitable gas phase synthesis technique.
  • the gas phase synthesis can be carried out by introduction of a controlled amount of NO gas into a sealed vessel containing a controlled amount of phosphine gas so as to promote formation of this yellow, amorphous and highly polymeric phosphorus polymer, P x H y . While not wishing to be bound by theory, a proposed mechanism of this free radical induced polymerization from the relatively stable NO radical is as follows:
  • nitric oxide abstracts a proton from phosphine resulting in the phosphine radical and nitrosyl hydride.
  • nitrosyl hydride ultimately becomes nitric acid and the phosphine radical polymerizes with phosphine gas upon gas phase collision with a phosphine molecule. The polymerization then continues with the collision of subsequent phosphine radicals generated from nitric oxide and or nitrogen dioxide.
  • a "living" phosphine polymer is also a possibility.
  • FIG. 1 shows a scanning electron microscopy photomicrograph of the polyhydride phosphorus polymer produced in the vessel .
  • the elemental analysis of the polyhydride phosphorus polymer is shown in Figure 1 wherein background spectra is not included.
  • phosphine gas can be subjected to gas phase synthesis with a free radical such as nitric oxide or nitrous oxide.
  • Phosphine gas may be generated at point of use by exposure of a metal phosphide such as, for example, magnesium phosphide, calcium phosphide or aluminum phosphide, to ambient humidity.
  • a metal phosphide such as, for example, magnesium phosphide, calcium phosphide or aluminum phosphide
  • the polyhydride phosphorus polymer can be formed in a sealed vessel by adjusting amounts of PH 3 and NO to deposit the polymer at a desired deposition rate.
  • the polyhydride phosphorus polymer can be used as an intermediate product to make other phosphorus compounds.
  • the polyhydride phosphorus polymer can be deposited on a substrate such as an article of flammable material or on a part intended for use in a fire hazard environment or in a high temperature environment .
  • the polyhydride phosphorus polymer can be deposited as a uniform film or coating with a thickness of a few microns or, if desired, built up to several mils, e.g., 1 to 100 ⁇ m, 100 ⁇ m to 1 mm, 1 to 10 mm.
  • the polyhydride phosphorus polymer can be converted to another phosphorus compound by oxidizing the polyhydride phosphorus polymer.
  • the polyhydride phosphorus polymer can be oxidized in a gaseous environment or by contacting the polyhydride phosphorus polymer with a solution of hydrogen peroxide.
  • the coated article can be immersed in a solution of hydrogen peroxide to convert the polyhydride phosphorus polymer to a phosphorus compound such as a polymeric phosphine oxide film/coating.
  • a preferred polymeric phosphine oxide includes phosphorus, hydrogen and oxygen. However, other constituents may also be incorporated in the phosphine oxide.
  • the polymeric phosphine oxide can be used for imparting fire retardant properties to flammable textile materials such as carpeting, drapery and clothing. Further details of such polymeric phosphine oxides can be found in U.S. Patent No. 4,072,653, the entire contents of which is hereby incorporated by reference.
  • the polymeric phosphine oxide can also be used as a heat/fire resistant coating on articles of manufacture such as oven/furnace parts, building materials, electronic components, automobile and aircraft parts, etc.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
  • Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)

Abstract

on produit un polymère de phosphore polyhydrure en soumettant une phosphine à une synthèse de phase gazeuse. Cette synthèse de phase gazeuse est effectuée via l'utilisation d'un radical libre tel qu'un initiateur de phase gazeuse. Ce polymère phosphore polyhydrure peut être déposé sur un article de manufacture par le réglage des quantités de NO et de phosphine dans une cuve étanche afin de déposer ce polymère de phosphore polyhydrure à une vitesse souhaitée. Ce polymère de phosphore polyhydrure déposé peut être soumis à une oxydation par un support oxydant tel qu'une solution de peroxyde d'hydrogène. Un revêtement résistant à la cuisson/feu produit par cette oxydation peut être utilisé sur des articles tels que des matériaux textiles inflammables comme de la draperie, des vêtements et des tapis ou des articles de manufacture telle que des pièces d'étuve/four, des matériaux de construction, des composants électroniques, des pièces d'automobile et d'aéronef.
PCT/IB2006/001880 2005-05-10 2006-05-10 Synthese de phase gazeuse de polymeres de phosphore polyhydrure Ceased WO2006120578A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US67925705P 2005-05-10 2005-05-10
US60/679,257 2005-05-10

Publications (2)

Publication Number Publication Date
WO2006120578A2 true WO2006120578A2 (fr) 2006-11-16
WO2006120578A3 WO2006120578A3 (fr) 2007-07-12

Family

ID=37396937

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2006/001880 Ceased WO2006120578A2 (fr) 2005-05-10 2006-05-10 Synthese de phase gazeuse de polymeres de phosphore polyhydrure

Country Status (1)

Country Link
WO (1) WO2006120578A2 (fr)

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB920515A (en) * 1959-10-05 1963-03-06 Minnesota Mining & Mfg Improved polymers
US3576783A (en) * 1969-06-11 1971-04-27 Monsanto Co Organic compositions containing phosphine oxide anhydrides
JPS4833960B1 (fr) * 1969-06-30 1973-10-17
US3799738A (en) * 1972-02-17 1974-03-26 Hooker Chemical Corp Flame retardant process for cellulosics
AR205889A1 (es) * 1973-06-28 1976-06-15 American Cyanamid Co Nuevos derivados de (bis(2-cianoetil) fosfonilmetilen) areno retardadores de llama y composicion que los comprende
US4127566A (en) * 1977-12-22 1978-11-28 Monsanto Company Process for preparation of flame retardant polyesters
US4429161A (en) * 1981-08-17 1984-01-31 Union Carbide Corporation Process for preparing organic tertiary polyphosphine monooxides
FR2739381B1 (fr) * 1995-09-28 1999-06-11 Clariant Finance Bvi Ltd Stabilisation de matieres polymeres avec des derives du phosphore

Also Published As

Publication number Publication date
WO2006120578A3 (fr) 2007-07-12

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