Flame-resistant polycarbonate molding materials

Details Flame-resistant polycarbonate molding materials Flame-resistant polycarbonate molding materials

2002-02-27

2004-06-22

Szekely, Peter (Department: 1714)

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

Synthetic resins

Processes of preparing a desired or intentional composition...

C524S139000, C524S148000

Reexamination Certificate

active

06753364

ABSTRACT:

The present invention relates to polycarbonate moulding compositions incorporating phosphonate amines, which are flame resistant and have a good level of mechanical properties, especially a high heat resistance, and are low-juicing.
U.S. Pat. Nos. 4,073,767 and 5,844,028 describe cyclic phosphorus compounds, including phosphorinane rings, as suitable flame retardants for polyurethanes, polyesters, polycarbonates and polyamides. In U.S. Pat. No. 4,397,750, certain cyclic phosphonate esters are described as efficient flame retardants for polypropylene and other polyolefins. In U.S. Pat. Nos. 5,276,066 and 5,844,028 certain (1,3,2-dioxaphosphorinane methane)amines are described which can be used as flame retardants in polyurethanes, polyesters, styrene polymers, polyvinyl chloride, polyvinyl acetate or polycarbonate.
U.S. Pat. No. 3,505,431, French Patent 1 371 139, U.S. Pat. Nos. 3,711,577, 4,054,544 describe acyclic triphosphonate amines which are partly halogenated.
In EP-A 0 640 655, moulding compositions of aromatic polycarbonate, styrene-containing copolymers and graft polymers are described, which can be rendered flame resistant with monomeric and/or oligomeric phosphorus compounds.
In EP-A 0 363 608, flame-resistant polymer mixtures of aromatic polycarbonate, styrene-containing copolymer or graft copolymer and oligomeric phosphates as flame retardants are described. For some applications, such as for example moulded parts in the interior of housing parts, the heat resistance of these mixtures is often inadequate.
In U.S. Pat. No. 5,061,745 polymer mixtures of aromatic polycarbonate, ABS graft polymer and/or styrene-containing copolymer and monophosphates as flame retardants are described. The level of the stress cracking resistance of these mixtures is often inadequate for producing thin-walled housing parts.
The object of the present invention is therefore to provide flame-resistant PC moulding compositions which have excellent heat resistance, good mechanical properties and low volatility of the phosphorus components in the moulding composition (low-juicing).
Surprisingly, it has now been found that, by using the phosphonate amines according to the invention, flame-resistant moulding compositions are obtained which give mouldings with a very good level of mechanical properties and outstanding heat resistance.
The invention therefore provides compositions containing polycarbonate and 0.1 to 30 parts by weight, preferably 1 to 25 parts by weight, particularly preferably 2 to 20 parts by weight, phosphonate amine of formula (I)
A
3−y
—N—B
y
  (I),
in which
A denotes a group of the formula (IIa)
or (IIb)
R
1
and R
2
, independently of one another, denote unsubstituted or substituted C
1
-C
10
alkyl or unsubstituted or substituted C
6
-C
10
aryl,
R
3
and R
4
, independently of one another, denote unsubstituted or substituted C
1
-C
10
alkyl or unsubstituted or substituted C
6
-C
10
aryl, or
R
3
and R
4
together denote unsubstituted or substituted C
3
-C
10
alkylene,
y signifies the numerical values 0, 1 or 2 and
B independently denotes hydrogen, optionally halogenated C
2
-C
8
alkyl, unsubstituted or substituted C
6
-C
10
aryl.
The present invention preferably provides flame-resistant blends containing
A) 5 to 95, preferably 10 to 90 parts by weight, particularly preferably 20 to 80 parts by weight, aromatic polycarbonate and/or polyester carbonate
B) 1 to 60, preferably 1 to 40 parts by weight, particularly preferably 2 to 30 parts by weight, of at least one graft polymer of
B.1 5 to 95, preferably 20 to 60 wt. % one or more vinyl monomers on
B.2 5 to 95, preferably 40 to 80 wt. % one or more polymer backbones with a glass transition temperature of <10° C., preferably 0° C., particularly preferably <−20° C. and an average particle size (d
50
value) of 0.05 to 5 &mgr;m, preferably 0.20 to 0.35 &mgr;m, particularly preferably 0.25 to 0.30 &mgr;m,
C) 0 to 50, preferably 1 to 30, particularly preferably 2 to 25, parts by weight thermoplastic vinyl (co)polymer and/or polyalkylene terephthalate,
D) 0.1 to 30 parts by weight, preferably 1 to 25 parts by weight, particularly preferably 2 to 20 parts by weight, phosphonate amine of formula (I)
A
3−y
—N—B
y
  (I),
in which
A, B and y have the meaning given above and
E) 0 to 5 parts by weight, preferably 0.1 to 1 part by weight, particularly preferably 0.1 to 0.5 parts by weight, fluorinated polyolefin,
the sum of the parts by weight of all the components A+B+C+D+E making 100.
Component A
Aromatic polycarbonates and/or aromatic polyester carbonates as in component A which are suitable according to the invention are known from the literature or can be prepared by methods known from the literature (for the preparation of aromatic polycarbonates see for example Schnell, “Chemistry and Physics of Polycarbonates”, Interscience Publishers, 1964, and DE-AS 1 495 626, DE-OS 2 232 877, DE-OS 2 703 376, DE-OS 2 714 544, DE-OS 3 000 610, DE-OS 3 832 396; for the preparation of aromatic polyester carbonates e.g. DE-OS 3 077 934).
Aromatic polycarbonates are prepared e.g. by reacting diphenols with carbonic acid halides, preferably phosgene and/or with aromatic dicarboxylic acid dihalides, preferably benzenedicarboxylic acid dihalides, by the phase boundary process, optionally using chain terminators, for example monophenols, and optionally using trifunctional or more than trifunctional branching agents, for example triphenols or tetraphenols.
Diphenols for the preparation of the aromatic polycarbonates and/or aromatic polyester carbonates are preferably those of formula (III)
wherein
A
1
is a single bond, C
1
-C
5
alkylene, C
2
-C
5
alkylidene, C
5
-C
6
cycloalkylidene, —O—, —SO—, —CO—, —S—, —SO
2
—, C
6
-C
12
arylene, which can be condensed with other aromatic rings optionally containing heteroatoms, or a group of the formula
or a group of the formula (V)
B independently of one another, is C
1
-C
8
alkyl, preferably C
1
-C
4
alkyl especially methyl, halogen, preferably chlorine and/or bromine, C
6
-C
10
aryl, preferably phenyl, C
7
-C
12
aralkyl, phenyl C
1
-C
4
alkyl, preferably benzyl,
x each independently of one another, is 0, 1 or 2,
p is 1 or 0 and
R
5
and R
6
, selectable individually for each Z, independently of one another, signify hydrogen or C
1
-C
6
alkyl, preferably hydrogen, methyl and/or ethyl,
Z signifies carbon and
m signifies an integer from 4 to 7, preferably 4 or 5,
with the proviso that, on at least one atom Z,
R
5
and R
6
are both alkyl.
Preferred diphenols are hydroquinone, resorcinol, 4,4′-dihydroxydiphenyl, bis(hydroxyphenyl) C
1
-C
5
alkanes, bis(hydroxyphenyl) C
5
-C
6
cycloalkanes, bis(hydroxyphenyl)ethers, bis(hydroxyphenyl) sulfoxides, bis(hydroxyphenyl) ketones, bis(hydroxyphenyl) sulfones and &agr;,&agr;-bis(hydroxyphenyl) diisopropylbenzenes and the ring-brominated and/or ring-chlorinated derivatives thereof.
Particularly preferred diphenols are 4,4′-diphenylphenol, bisphenol A, 2,4-bis(4-hydroxyphenyl)-2-methylbutane, 1,1-bis(4-hydroxyphenyl)cyclohexane, 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane, 4,4′-dihydroxydiphenyl sulfide, 4,4′-dihydroxydiphenyl sulfone and the di- and tetrabrominated or chlorinated derivatives thereof such as, for example, 2,2-bis(3-chloro -4-hydroxyphenyl)propane, 2,2-bis(3,5-dichloro-4-hydroxyphenyl)propane or 2,2-bis(3,5-dibromo-4-hydroxyphenyl)propane.
2,2-Bis(4-hydroxyphenyl)propane (bisphenol A) is particularly preferred.
The diphenols can be used individually or as any mixtures.
The diphenols are known from the literature or are obtainable by methods known from the literature.
Suitable chain terminators for the preparation of the thermoplastic, aromatic polycarbonates are, for example, phenol, p-chlorophenol p-tert.-butylphenol or 2,4,6-tribromophenol, but also long-chain alkylphenols, such as 4-(1,3-tetramethylbutyl)phenol according to DE-OS 2 842 005 or monoalkylphenol or dialkylphenols with a total of 8 to 20 C atoms in the alkyl substituents, such as

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