Process for flame-proofing organic polymeric materials

Details Process for flame-proofing organic polymeric materials Process for flame-proofing organic polymeric materials

1996-06-14

1999-01-05

Sanders, Kriellion A

Synthetic resins or natural rubbers -- part of the class 520 ser

Synthetic resins

Processes of preparing a desired or intentional composition...

428704, 427447, 4273935, 4272556, C08J 328, B32B 904

Patent

active

058563806

DESCRIPTION:

BRIEF SUMMARY
The present invention relates to a process for flame-proofing organic polymeric materials by means of a plasma treatment in the presence of at least one phosphorus-containing, low-molecular compound, to the organic material treated with said novel process as well as to a process for the preparation of phosphorus-containing, halogen-free films of polymeric structure.
Polymeric material can usually be flame-proofed by impregnating a copolymer of phosphorus-containing monomers. Such treatment of fibre materials with compositions containing phosphorus compounds is disclosed, inter alia, in U.S. Pat. Nos. 2,926,145 and 2,733,229. To achieve effective flame-proofing in these processes, it is necessary to use a large amount of active substance which, however, may adversely affect the properties of the organic substrate, for example the photochemical stability or the mechanical properties.
In the known plasmachemical flame-proofing methods described, inter alia, by G. Akovali and G. Gundogan in J. Appl. Polym. Sci. 41, 2011 (1990), G. Alkovali and F. Takrouri in J. Appl. Polym. Sci. 42, 2717 (1991) and C. I. Simionescu et al. in ACS Symp. Ser. 187, 57 (1982), the volatile low-molecular compounds are always halogenated compounds, such as halogenated hydrocarbons or phosphorus trichloride.
Surprisingly, it has now been found that effective flame-proofing is achieved in a plasmachemical process using at least one halogen-free, low-molecular phosphorus compound. In this process, the consumption of active substance is markedly lower than in the typical conventional wet-chemical processes.
Accordingly, the invention relates to a process for flame-proofing organic polymeric materials by means of a low temperature plasma treatment in the presence of at least one low-molecular, volatile compound, which process comprises subjecting the volatile compound, selected from a halogen-free phosphorus compound, to the low temperature plasma, such that a polymeric structure forms on the organic material.
The principles of gas discharge and, in particular, of plasma chemistry are known and described, inter alia, by A. T. Bell, "Fundamentals of Plasma Chemistry" in "Technology and Application of Plasma Chemistry", ed. J. R. Hollahan and A. T. Bell, Wiley, New York (1974) or by H. Suhr, Plasma Chem. Plasma Process. 3(1), 1, (1983).
Suitable low-molecular compounds for the process of this invention are primarily halogen-free, phosphorus compounds which can be volatilised or sublimed without decomposition, i.e. which are stable at 10.sup.-4 bar to normal pressure and at room temperature of up to 250.degree. C.
Preferred phosphorus compounds which fulfill these requirements are primarily unsaturated organophosphorus acids and the derivatives thereof. Exemplary of these compounds are the following compounds: or C.sub.6 H.sub.5 CH.dbd.CHCOCH.sub.2 CH(C.sub.6 H.sub.5)P(O)(OH).sub.2 ; H.sub.2 C.dbd.CHP(O)(OH).sub.2 ; as H.sub.2 C.dbd.C(C.sub.6 H.sub.5)P(O)(OH).sub.2 ; C.dbd.CHCH.sub.2 P(O)(OH).sub.2 ; H.sub.5 CH.dbd.CHCH.dbd.CHP(O)(OH).sub.2 ; C.dbd.C(CN)CH.sub.2 P(O)(NHCH.sub.3)(OC.sub.2 H.sub.5); C.dbd.CHP(O)(OCH.sub.3).sub.2, H.sub.2 C.dbd.(OC.sub.2 !P(O)(OC.sub.2 H.sub.5).sub.2, C.sub.2 H.sub.5 OCH.dbd.CHP(O)(OCH.sub.3).sub.2, CH.sub.3 OC.sub.2 H.sub.4 OCH.dbd.CHP(O)(OCH.sub.3).sub.2, C.sub.2 H.sub.5 SCH.dbd.CHP(O)(OC.sub.3 H.sub.7).sub.2, H.sub.2 C.dbd.C(CH.sub.3)P(O)(OCH.sub.3).sub.2, H.sub.2 C.dbd.C(CN)P(O)(OCH.sub.3).sub.2, H.sub.2 H.sub.4 C(O)OC.sub.2 H.sub.5 !P(O)(OCH.sub.3).sub.2, H.sub.3 CCH.dbd.CHP(O)(OCH.sub.3).sub.2, H.sub.5 C.sub.2 CH.dbd.CHP(O)(OCH.sub.3).sub.2, H.sub.3 CO(O)CCH.dbd.CHP(O)(OCH.sub.3).sub.2, C.sub.6 H.sub.5 CH.dbd.CHP(O)(OCH.sub.3).sub.2, C.sub.6 H.sub.5 CCH.sub.3 .dbd.CHP(O)(OCH.sub.3).sub.2, C.sub.6 H.sub.5 C.dbd.CHP(O)(OCH.dbd.CH.sub.2).sub.2 ; C.dbd.CHCH.sub.2 P(O)(OCH.sub.3).sub.2, H.sub.3 CP(O)(OCH.sub.2 CH.dbd.CH.sub.2).sub.2 or H.sub.2 C.dbd.CHCH.sub.2 P(O)(OCH.sub.2 CH.dbd.CH.sub.2).sub.2 ; H.sub.2 C.dbd.CH(OH)CHP(O)(OCH.sub.3).sub.2 or H.sub.2 C.dbd.CH(O)CP(O)(OC.sub.2 H.sub.5).sub.2 ; such as H.sub.

REFERENCES:
Akovali et al., "Studies on Flame Retardancy of Polyacrylonitrile Fiber Treated by Flame Retardant Monomers in Cold Plasma", J. App. Polym. Sci., vol. 41, 2011-2019 (1990).
Simionescu et al., ACS Symp. Ser 187, 57 (1982).

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