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Scheme
1:
Preparation
of
Figure 1: FTIR
spectra of PES-I
and OES-II.
Figure
3:
TGA
thermograms
of
the
polyaryloxydiphenylsilanes
Table 2: Thermal properties of polyaryloxydiphenylsilane
polymers
molten processes, especially while the OES polymers are used as flame retardants for
(A)
(B)
Scheme 2: Synthesis of DPhPP (1), DPhPI (2), DOPP (3), DOPI (4), DMPP
(5), and DMPI (6).
The compounds 16 were blended into the epoxy resins with phosphorus
contents between 1.0 and 3.0% depending on the system and processed
as described above.
Phosphorus-containing Polysulfones A
Thorsten HoffmannStudy
Doris Pospiech, Liane Huler, Karin Sahre, hartmut
Comparative
,
from
DOPO-HQ
(phosphinate
structure
to
DPPO-HQ
Scheme 3: Synthesis route for the preparation of the phosphorus-containing P-PSU (PPSU_A, P-PSU_B)
Polysulfones (PSU), Phosphorus-Polysulfones (P-PSU)
Figure 5: TGA of P-PSU_A (dotted line) and of P-PSU_B (dashed line) in comparison
with the neat PSU (solid line) in nitrogen atmosphere.
Figure 6: Decomposition of PSU (solid line), P-PSU_A (dotted line), and P-PSU_B
(dashed line): heat release rate as function of temperature obtained by pyrolysis
combustion flow calorimeter.
The pyrolysis and fire behavior of halogen-free flame-retarded DGEBA/DMC, RTM6 and their
corresponding 60 vol.-% carbon fibers (CF) composites were investigated.
A novel phosphorous compound (DOPI) was used. Its action is dependent on the epoxy matrix.
Only flame inhibition occurs in the gas phase. RTM6 shows flame inhibition and a condensed
phase interaction increasing charring.
Both mechanisms decrease with increasing irradiance, whereas in RTM6-CF charring is
suppressed at low ones.
RTM6+DOPI shows a higher LOI (34.2%) than DGEBA/ DMC+DOPI and a V-0 classification
in UL 94.
Adding CF only enhances the LOI, DOPI+CF leads to a superposition in LOI for
DGEBA/DMC-CF+DOPI (31.8%, V-0) and a synergism for RTM6-CF+DOPI (47.7%, V-0).
Dopac-3-isocyanurate [DOPI]
Table 8: Investigated materials. The amount of CF corresponds to 60 vol.-%. And glass transition
temperatures, Tg (3 Hz), of the investigated materials with an error of 2K.
Figure 7: Mass and mass loss rate of (a) DGEBA/DMC (filled squares) and DGEBA/DMC+DOPI
(open squares) and (b) RTM6 (filled circles) and RTM6+DOPI (open circles) under nitrogen at a
heating rate of 10 K min-1.
Fire Behavior
Cone
calorimeter
measurements at different
external heat fluxes
Fire Behavior
Cone
calorimeter
measurements at different
external heat fluxes
Figure 12: TG curves of PTT and PTTEPs at the heating rate of 10 C/min in N2 (a)
and air atmosphere (b)
Table 13: TG and DTG results of PTT and
PTTEPs.
Table 14: Activation energy of PTT and PTTEPs using the FlynnWallOzawa
method.
Pyrolysis GCMS
Figure 17: GC traces for the
evolved products of PTT and
PTTEP30 during pyrolysis
Conclusions
Phosphorus flame retardants generally act in both gas and condensed
phase. They can also be chemically tailored to favor one mechanism
or the other.
Unlike other halogen-free alternatives, phosphorus compounds have
demonstrated flame retardancy with relatively low loadings,
regardless of their mode of addition.
The altered bond nature between phosphorus and adjacent atoms
(oxygen and carbon) provoked different thermal stability and
consequently changed the decomposition mechanism.
High phosphorus contents led to polymers exhibiting high activation
energy of decomposition and leading as best flame retardants in
literature.
DOPO derivatives interest because they lead to excellent flame
resistance which is caused by the rapid decomposition of the DOPO
unit, accompanied by the release of dibenzofuran and a PO radical at
increased temperatures in the case of fire.
Hence, new multifunctional reactive DOPO derivatives (like, DOPO-
Conclusions
In the DOPO-HQ as well as DPPO-HQ the phosphorus is located in the
side chain and has differed only in the number of oxygen atoms
within the environment of the phosphorus. While the oxygen O1
bound to the P atom in the DOPO unit can interact with the OH-group
(O4) to form an intramolecular hydrogen bond able to disturb the
poly-condensation, the phosphine oxide structure in DPPO-HQ seems
more suitable for poly-condensation.
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