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Sommaire du brevet 1079886 

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L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 1079886
(21) Numéro de la demande: 1079886
(54) Titre français: SUBSTANCES THERMOPLASTIQUES MOULABLES DE POLYCARBONATE, PLUS FACILES A DETACHER DU MOULE
(54) Titre anglais: THERMOPLASTIC POLYCARBONATE MOULDING COMPOSITIONS WITH IMPROVED EASE OF MOULD RELEASE
Statut: Durée expirée - après l'octroi
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • C08K 5/10 (2006.01)
  • C08L 69/00 (2006.01)
(72) Inventeurs :
  • ADELMANN, SIEGFRIED
  • MARGOTTE, DIETER
  • VERNALEKEN, HUGO
  • NOUVERTNE, WERNER
(73) Titulaires :
  • BAYER AKTIENGESELLSCHAFT
(71) Demandeurs :
  • BAYER AKTIENGESELLSCHAFT (Allemagne)
(74) Agent:
(74) Co-agent:
(45) Délivré: 1980-06-17
(22) Date de dépôt:
Licence disponible: S.O.
Cédé au domaine public: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Non

(30) Données de priorité de la demande: S.O.

Abrégés

Abrégé anglais


Thermoplastic polycarbonate moulding compositions with
improved ease of mould release
Abstract of the Disclosure
The invention relates to a thermoplastic moulding composition
comprising a high molecular, thermoplastic aromatic polycarbonate
based on an aromatic dihydroxy compound and containing 0,01
to 0.5 % by weight of an ester of a saturated aliphatic carboxylic
acid with 10 to 20 C atoms per molecule and an aromatic hydroxy
compound with from 1 to 6 OH groups.
- 2 -

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.


The embodiments of the invention in which an exclusive property
privilege is claimed are defined as follows:-
WHAT WE CLAIM IS:
1. A thermoplastic moulding composition comprising
a high molecular thermoplastic aromatic polycarbonate based
on an aromatic dihydroxy compound and containing 0.01 to 0.5%
by weight of an ester of a saturated aliphatic carboxylic
acid with 10 to 20 C atoms per molecule and an aromatic
hydroxy compound with from 1 to 6 OH groups.
2. A thermoplastic moulding composition according
to Claim 1, characterized in that the esters are completely
esterified compounds.
3. A thermoplastic moulding composition according
to Claim 1, characterized in that the esters are partially
esterified compounds.
-21-

Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


o79886
The invention relates to thermoplastic moulding
compositions of high-molecular thermoplastic, aromatic
polycarbonates based on aromatic dihydroxy compounds and
containing 0.01-0.5%, preferably 0.05-0.1~ by weight of an
ester of a saturated aliphatic carboxylic acid with 10 to
20 C atoms per molecule and an aromatic hydroxy compound
with from 1 to 6 OH groups.
High-molecular, thermoplastic, aromatic polycarbon-
ates are used in numerous technical fields of use, because of
their typical tough and elastic properties. A disadvantage is
their difficulty of mould release when injection moulded,
which frequently results in relatively long cycle times.
However, for economic and technical reasons it is desirable
to shorten the cycle times as far as possible in order to
produce a larger number of mouldings per unit time on the
injection moulding machines. This can be achieved by mould
release at higher temperatures. It is therefore desirable to
modify the polycarbonate melt in such a way that the release
of the moulding from the mould wall takes place with low
release forces and at high temperatures, without sticking
: I
of the solidified melt. Ease of mould release at high temper-
atures is also particularly desirable for complicated mouldings
which are processed in moulds comprising parts which cannot
be cooled (for example webs, cores and the like). Undesirable
sticking of the mouldings and damage to the moulds on
detaching the mouldings (breakage of pins and the like) are a
frequent consequence, coupled with extended time losses.
Up until now mould release with esters of aliphatic
alcohols has been known see DOS (German Published Specifica-
30 tion) 2,064,059 (LeA 13,461), DOS (German Published Specifica-
tion) 2,220,185 (LeA 14,329) and JAS (Japanese Published
Specification)
LeA 17,847 -3-

` 1079886
Sho-47-41092, DOS (German Published Specification) 2,507,748
(LeA 16,284); according to the latter application the polycar-
bonate compositions exhibiting ease of mould release do not
show any decrease in mechanical properties even after being
subjected to heat for a considerable length of time.
On the other hand it was surprising that according
to the present invention phenol esters are effective as mould
release auxiliaries without causing decomposition of the
polycarbonate as a result of trans-esterification. Beyond
10 this it was not to be expected that partial esters of aromatic
hydroxy compounds with aliphatic carboxylic acids are also
suitable as mould release auxiliaries because of the free
aromatic hydroxyl groupsl without adversely affecting the
properties of the polycarbonate to be released from the mould.
The subject of the present invention are thermoplastic
moulding compositions of high-molecular, thermoplastic, aromatic
polycarbonates based on aromatic dihydroxy compounds containing
; 0.01-0.5, preferably 0.05-0.1~ by weight of an ester of satur-
ated aliphatic carboxylic acids with 10 to 20 C atoms and
20 aromatic hydroxy compounds with 1 to 6 hydroxyl groups.
Esters suitable according to the invention of satur-
ated aliphatic C10-C20 carboxylic acids and aromatic hydroxy
compounds with 1 to 6 OH groups are those compounds obtainable
by esterification of the aromatic hydroxy compounds with the
25 named carboxylic acids. According to the invention these are
on the one hand those resulting from complete esterification of
the 1 to 6 OH groups of the aromatic hydroxy compound with one
or more than one of the C10-C20 carboxylic acids in question
and on the other hand the partial esters resulting from partial
30 esterification of the 1 to 6 OH groups of the aromatic
hydroxy compounds with one or
LeA 17,847 -4-
- : , :
.,
.

1079886
more than one of the C o-C20 carboxylic acids in question.
Also suitable according to the invention are mixtures of
these partial esters and the aforementioned completely
esterified compounds.
The surprising feature of the invention is that, in
contrast to the known processes, even when using mono-, di-, or
tri-phenol esters according to the present invention, small
amounts suffice to achieve an ease of mouldrelease adequate
for all fields of use.
The polycarbonate moulding compositions according to
the invention are distinguished by outstanding ease of mould
release, a particular advantage being that the mould release
can be effected over a wide temperature range. This permits
short injection cycles, regardless of temperature fluctuations
15 in the injection mould, which is a great advantage for the
plastics processor.
The mechanical properties and the long-term use
properties of the polycarbonates which have been rendered
easily releasable from the mould in accordance with the present
20 invention, are identical with those of the pure polycarbonates.
Even prolonged heat exposure (130C for more than 300 hours)
causes no observable deterioration in the mechanical properties
and no degradation of the molecular weight.
By aromatic polycarbonates, in the sense of the
25 present invention, there are understood homopolycarbonates and
' copolycarbonates which are based, for example, on one or more
of the following bisphenols: hydroquinone, resorcinol, dihy-
droxydiphenyls, bis-(hydroxyphenyl~-alkanes, bis~(hydroxyphenyl~
cycloalkanes,bis-(hydroxyphenyl)-sulphides, bis-(hydroxyphenyl)-
30 ethers, bis-(hydroxyphenyl)-ketones, bis-(hydroxyphenyl~-
--5--
LeA 17,847
. .

~079886
sulphoxides, bis-(hydroxyphenyl)-sulphones and ~,a-bis-
(hydroxyphenyl)-diisopropyl-benzenes, as well as their nuclear-
alkylated and nuclear-halogenated compounds. These and
further suitable aromatic dihydroxy compounds are described,
for example, in U.S. Patent Specifications 3,028,365, 2,999,835,
3,148,172, 3,271,368, 2,991,273, 3,271,367, 3,280,078,
3,014,891 and 2,999,846, in German Offenlegungsschriften
(German Published Specifications) 1,570,703, 2,063,050,
2,063,052, 2,211,956 and 2,211,957, in French Patent Specifica-
10 tion 1,561,518 and in the monograph "H. Schnell, Chemistry and
Physics of Polycarbonates, Interscience Publishers, New York,
; 1964".
Preferred bisphenols are those of the formula I
HO- ~ - X ~ ~ -OH (I)
~ R R
;~ 15 in which
R is identical or different and denotes H, Cl-C4-
alkyl, Cl or Br
and in which
X is a bond, Cl-C8-alkylene, C2-C8-alkylidene, C5-C15-
cycloalkylene, C5-C15-cyclo~slkylidene, -SO2- or
CH3 CH
- C - ~ - C,
CH3 CH3
Examples of these bisphenols are: 4,4'-dihydroxy-
:l diphenyl, 2,2-bis-(4-hydroxyphenyl)-propane, 2,4-bis-(4-hydroxy-
phenyl)-2-methylbutane, 1,1-bis-(4-hydroxyphenyl)-cyclohexane,
25 ~,~ -bis-(4-hydroxyphenyl)-p-diisopropylbenzene, 2,2-bis-(3-
-6-
LeA 17,847

10~886
methyl-4-hydroxyphenyl)-propane, 2,2-bis-(3-chloro-4-hydroxy-
phenyl)-propane, bis-(3,5-dimethyl-4-hydroxyphenyl)-methane,
2,2-bis-(3,5-dimethyl-4-hydroxyphenyl)-propane, bis-(3,5-
dimethyl-4-hydroxyphenyl)-sulphone, 2,4-bis-(3,5-dimethyl-4-
5 hydroxyphenyl)-2-methylbutane, 1,1-bis-(3,5-dimethyl-4-
hydroxyphenyl)-cyclohexane, ~,~-bis-(3,5-dimethyl-4-hydroxy-
phenyl)-p-diisopropyl-benzene, 2,2-bis-(3,5-dichloro-4-hydroxy-
phenyl)-propane and 2,2-bis-(3,5-dibromo-4-hydroxyphenyl)-
propane.
Examples of particularly preferred bisphenols are:
2,2-bis-(4-hydroxyphenyl)-propane, 2,2-bis-(3,5-dimethyl-4-
hydroxyphenyl)-propane, 2,2-bis-(3,5-dichloro-4-hydroxyphenyl)-
propane, 2,2-bis-(3,5-dibromo-4-hydroxyphenyl~-propane and
1,1-bis-(4-hydroxyphenyl)-cyclohexane.
Preferred aromatic polycarbonates are those which are
based on one or more of the bisphenols mentioned as being
preferred. Particularly preferred copolycarbonates are those
based on 2,2-bis-(4-hydroxyphenyl)-propane and one of the
other bisphenols mentioned as being particularly preferred.
20 Further particularly preferred polycarbonates are those based
solely on 2,2-bis-(4-hydroxyphenyl)-propane or 2,2-bis-(3,5-
dimethyl-4-hydroxyphenyl)-propane.
The aromatic polycarbonates can be prepared in accord-
ance withknown processes, such as, for example, in accordance
25 with the melt trans-esterication process from bisphenols and
diphenyl carbonate and the two-phase boundary process from
bisphenols and phosgene,as described in the above-mentioned
~ literature.
; The aromatic high-molecular weight polycarbonates can
30 be branched due to the incorporation of small amounts, prefer-
ably of between 0.05 and 2.0 mol% (relative to diphenols
employed),
LeA 17,847 7

1079886
of trifunctional or more than trifunctional compounds,
especially compounds with three or more phenolic hydroxyl groups.
Polycarbonates of this type are described, for
example, in German Offenlegungsschriften (German Published
Specifications) 1,570,533, 1,595,762, 2,116,974 and 2,113,347,
British Patent Specification 1,079,821 and U.S. Patent
Specification 3,544,514.
Some examples of compounds with three or more than
three phenolic hydroxyl groups which can be used are phloroglu-
10 cinol, 4,6-dimethyl-2,4,6-tri-(4-hydroxyphenyl)-heptane-2,4,6-
dimethyl-2,4,6-tri-(4-hydroxyphenyl~-heptane, 1,4,5-tri-(4-
hydroxyphenyl)-benzene, l,l,l-tri-(4-hydroxyphenyl)-ethane,
tri-(4-hydroxyphenyl)-phenylmethane, 2,2-bis-[4,4 -bis-(4-
hydroxyphenyl~-cyclohexyl]-propane, 2,4-bis-(4-hydroxyphenyl-
15 isopropyl)-phenol, 2,6-bis-(2-hydroxy-5'-methyl-benzyl)-4-
methylphenol, 2-(4-hydroxyphenyl)-2-(2,4-dihydroxyphenyl)-
propane, hexa(4-(4-hydroxyphenylisopropyl)phenyl) ortho-
terephthalic acid ester, tetra-(4-hydroxyphenyl)-methane,
tetra-(4-(4-hydroxyphenylisopropyl)-phenoxy)-methane and 1,4-
20 bis-((4',4"-dihydroxytriphenyl)-methyl)-benzene. Some of the
other trifunctional compounds are 2,4-dihydroxybenzoic acid,
trimesic acid, cyanuric chloride and 3,3-bis-(4-hydroxyphenyl)-
2-oxo-2,3-dihydroindole.
The aromatic high-molecular polycarbonates should as a
25 rule have mean weight-average molecular weights Mw of at least
10,000, especially of 10,000 to 200,000, preferably of 20,000
to 80,000, determined by measuring the relative viscosity in
CH2C12 at 25C and a concentration of 0.5~ by weight.
; The esters which are effective according to the present
30 invention are reaction products of 1-6-hydric aromatic hydroxy
--8--
LeA 17,847
. . . ~
- , . , .~ . . -
- : .:, .: . , . ,- . . ~ : . . -

~0798~36
compounds, such as, for example, phenol, pyrocatechol,
resocinol, hydroquinone, phloroglucinol, pyrogallol, hydroxy-
hydroquinone, hexahydroxybenzene, 2,2-bis-(4-hydroxyphenyl)-
propane (bisphenol A), 2,2-bis-(3,5-dimethyl-4-hydroxyphenyl)-
propane (tetramethylbisphenol A), 2,2-bis-(3,5-dichloro-4-
; hydroxyphenyl)-propane (tetrachlorobisphenol A), 2,2-bis-(3,5-
dibromo-4-hydroxyphenyl)-propane (tetrabromobisphenol A), 4,4'-
dihydroxy-tetraphenylmethane, l,4-bis-(4 4"-dihydroxytriphenyl)-
methyl)benzene, naphthol, anthrahydroquinone or dihydroxy-
naphthalene, with saturated aliphatic carboxylic acids with 10
to 20 C atoms.
All aliphatic saturated monocarboxylic acids bet~reen
capric acid (C10) and eicosanoic acid (C~0) are suitable, for
example capric acid, undecanoic acid, lauric acid, tridecanoic
acid, myristic acid, pentadecanoic acid, palmitic acid,
margaric acid, stearic acid, nonadecanoic acid and eicosanoic
acid.
Myristic acid, palmitic acid and stearic acid are used
preferentially.
Small amounts of polycarboxylic acids with 2 to 20 C
atoms, for example oxalic acid, malonic acid, adipic acid,
sebacic acid, undecanedioic acid, dodecanedioic
acid, brassylic acid, thapsic acid and others c~n, if appro-
priate, be used conjointly, to increase the molecular weight
of the esters of aromatic hydroxy compounds which are effective
in accordance with the invention. For this purpcse, in
general, 5-10 mol % are employed, relative to the total molar
amount of monocarboxylic acid esters and polycarboxylic acid
esters in the particular ester which is effective according to
; 30 the invention.
Examples of esters to be used according to the invention
Le A 17 ~47 _ 9 _
.
-~ - , . . : :

-
~7~8B6
are: phenyl stearate, bisphenol A aistearater tetramethyl-
bisphenol A dipalmitate, hydroquinone distearate, phloro-
glucinol tripalmitate, 1,4-bis-((4,4'-dihydroxy-triphenyl)-
benzene tetramyristate, 4,4'-dihydroxy-tetraphenylmethane
distearate, hexahydroxybenzene hexastearate and phloroglucinol
trilaurate.
Partial esters to be used according to the invention
are for example: phloroglucinol distearate, phloroglucinol
palmitate with an OH number of 45, - this corresponds to a
mixture of approx. 50 parts phloroglucinol palmitate and approx.
50 parts phloroglucinol tripalmitate - or 1,4-bis ((4,4'-
dihydroxy-triphenyl) methyl)benzene tetramyristate, and
hexahydroxybenzene pentastearate.
The use of single-compound esters of stearic acid
and palmitic acid with bisphenol A, tetramethylbisphenol A or
hydroquinone is preferred.
Preferred partial esters are phloroglucinol di-
stearate, tetramethyl-bisphenol A-palmitate, 1,4-bis-((4,4'-
dihydroxy-triphenyl)methyl) benzene tristearate.
; Mixtures of the esters, according to the invention, of
the saturated aliphatic C10-C20-carboxylic acids and the
aromatics containing 1-6 OH groups are also suitable, e.g.:
Mixtures of bisphenol A distearate and phloroglucinol
tripalmitate or hydroquinone distearate and phloroglucinol
'` dipalmitate or phIoroglucinol dipalmitate and 1,4-bis-((4,4'-
- 30 dihydroxy-triphenyl)-methyl) benzene tristearate.
~' The term aromatic hydroxy compounds also embraces
' oligomeric and polymeric compounds with phenolic OH groups, for
example those of the polycarbonate and novolac type with
,. ,
' molecular weights Mw (weight-average) of up to about 1,200.
The oligomeric polycarbonates are obtained, for
, example,
-10-
LeA 17,847-Ca
~, .
... ; . . . . . . . .
. .~ , .~ : . . ;

1~'7~8~6
by melt trans-esterification of bisphenols with diaryl
carbonates; thereafter, the reaction with the C10-C20-fatty
acid chlorides, to give the esters which are effective accord-
ing to the invention, is carried out.
Novolacs are prepared according to conventional pro-
cesses, by acid condensation of phenols with formaldehyde;
thereafter, a reaction with the acid chlorides of the aliphatic,
saturated C10-C20 monocarboxylic acids, to give the esters
which are effective according to the in~ention, is carried out.
The carboxylic acid esters to be used according to the
invention are prepared in accordance with customary processes,
for example in accordance with the Einhorn process, using
pyridine as the acid-binding agent, or from the aromatic
hydroxy compound and the acid chloride, in an inert solvent.
Such processes are described, for example, in
"Houben-Weyl, Methoden der organischen Chemie"(Methods of
Organic Chemistry), Georg Thieme Verlag, Stuttgart, 1952,
4th Edition, Vol. VIII, page 516 et seq~
Up to 50 carboxyl equivalents of the monocarboxylic
20 acids to be used can be replaced by carboxyl equivalents of
the above-mentioned polycarboxylic acids with 2 to 20 C atoms,
in particular those of aliphatic C2-C20 dicarboxylic acids.
Besides aliphatic polycarboxylic acids, aromatic
polycarboxylic acids, such as trimesic acid, can also be used.
25 The partial esters suitable according to the invention and
produced with the incorporation of polycarboxylic acids should
preferably have average number molecular weights Mn f less
than 5,000, in particular of less than 3,000.
The carboxylic acid esters to be used according to
30 the invention are incorporated into the high-molecular, thermo-
-1 1 -
LeA 17,847
'~ '
., - . - ~

"~ ~079t386
plastic polycarbonates by, for example, applying the substances,
which are normally in the form of powders, onto the granules of
the polycarbonate by tumbling, and then extruding the material,
by means of a twin-screw extruder, at 280C, to give a strand
which is granulated. However, the mould release agent can
already be incorporated during the preparation of the solid
polycarbonate. In that case, the ester is e ther added to
the polycarbonate, as a solution in a solvent, before the
devolatilisation screw is reached, or is metered into the poly-
carbonate melt without using a solvent.
The addition of the esters to be used according to theinvention does not have an adverse effect on either the trans-
parency or the colour. If desired, dyestuffs, pi~ments,
stabilisers, flameproofing agents or fillers, such as glass 15 fibres, can also be added to the polycarbonate without thereby
detracting from the effectiveness of the mould release agent.
The thermoplastic polycarbonate moulding compositions
~' according to the invention find use wherever mouldings are
produced fully automatically by the injection moulding process,
' 20 in long runs and with short cycle times. This is true, for
example, for use in the electrical industry and the optical
- field, for example for strips of sockets, coil bodies,
complicated housings, such as projector housings, bottoms of
switch cabinets and the like, and for particularly complicated
mouldings which are moulded in moulds in which there are
regions with greatly different temperatures. When pro-
ducing such articles, no mould release difficulties arise even
at elevated temperature.
The effectiveness of the esters to be used according
to the invention is measured in terms of the mould release
-; .
.
L,e A 17 8L~7 -12 -
. . .
, . . . .

1079886
forces required when releasing injection moulding compositions
from the mould. In the examples which follow, these forces
are measured' by rendering the pressure, which builds up in the
oil cylinder of the ejector system during mould release, visible
' 5 by means o~ an optical indicator instrument which at the same
time acts as a pen recorder.
The examples which follow are intended to explain the
subject of the invention in more detail:
I. The aromatic polycarbonates used.
~10 General instru t ons for the preparation of polycarbonates
; About 454 parts of 4,4'-dihydroxydiphenyl-2,2-propane
and 9.5 parts of p-tert.-butylphenol are suspended in 1.5 1 of
water. The oxygen is removed from the reaction mixture in
a 3-necked flask, equipped with a stirrer and gas inlet tube,
~15 by passing nitrogen through the reaction mixture for 15 min-
utes, whilst stirring. 355 parts of 45~0 strength sodium
hydroxide solution and 1,000 parts of methylene chloride are
then added. The mixture is cooled to 25C. Whilst
maintaining this temperature by cooling, 237 parts of phosgene
are added over a period of 120 minutes. An additional ~'
; amount of 75 parts of a 45% strength sodium hydroxide solution
is added after 15-30 minutes or after the absorption of phos-
' gene has started. 1.6 parts of triethylamine are added to
; the resulting solution and the mixture is stirred for a further
15 minutes. A very viscous solution is obtaired, the ;~ -
viscosity of which is regulated by adding methylene chloride.
The aqueous phase is separated off. The'organic phase is
washed with water until free from salt and alkali. The
polycarbonate is isolated from the washed solution, and dried.
~;30 The polycarbonate has a relative viscosity of 1.29-1 30,
,: I :
. ' '': '
' Le A 17 ~Z - 13 -
,. :-
t

1079886
measured on an 0.5% strength methylene chloride solution at
20C. This corresponds approximately to a molecular weight
of 32,000. The polycarbonate thus obtained is extruded and
granulated.
A.) An aromatic polycarbonate based on 4,4'-dihydroxydiphenyl-
propane-2,2 (bisphenol A) having a relative vis:cosity of nrel=
1.80, MLS = 28,000.
The viscosities are measured at 25C in methylene
chloride at a concentration of 5 g/l.
10 B.) An aromatic polycarbonate based on 90 mol ~ of bisphenol A
and 10 mol % of 4,4'-dihydroxy-3,3',5,5'-tetrabromodiphenyl-
propane-2,2 (tetrabromobisphenol A) having a relative viscoslty
of nrel=1.33, MLs=37,000.
C.) An aromatic polycarbonate based on 70 mol ~ of bisphenol A
15 and 30 mol % of 4,4'-dihydroxy-3,3',5,5'-tetramethyl-diphenyl-
propane-2,2 (tetramethylbisphenol A) having a relative viscosity
f nrel=l-2~, MLs=30,000-
II. The mould release agents used
D.) Bisphenol A distearate, melting point 67C
20 E.) Hydroquinone dipalmitate, melting point 90C
F.) Phloroglucinol trilaurate, melting point 64C
G.) Tetramethylbisphenol A distearate, melting point 63C
G.l) Phloroglucinol distearate melting point 72C
G.2) 1,4-bis((4,4'-dihydroxy- melting point 89C
triphenyl)methyl)benzene tristearate
H.) (Comparative example) Triglyceride with acid groups of
palmitic acid, stearic acid and myristic acid in the ratio of
1:1:0.1, melting point 48C. (Compare DT-OS (German Published
Specification) 2,064,095).
30 H.l) (Comparative example)
Pentaerythritol tetrastearate melting point 76C
-14-
LeA 17,847

~079886
Example of the preparation of a mould release
auxiliary:
Phloroglucinol distearate
37.8 g (0.3 mol) phloroglucinol are dissolved in 0.9 1
5 toluene and 60 ml pyridine and heated to 100C. 181.8 g (0.6
mol) stearoylic chloride are added dropwise to this within
40 min. The solution is boiled (approx. 110C) for an hour with
refluxing. After cooling, the mixture is acidified with dilute
hydrochloric acid, subsequently washed with water until neutral
10 and dried with anhydrous sodium sulphate. After concentration
of the organic phase the phloroglucinol distearate crstallizes
out. It is recrystallized from ethanol. A product is obtained
with a melting-point of 72C, an acid number of approx. 1 and an
OH number of 88 (-approx. 2.67~ OH).
15 Examples 1 to 13
Examples 1, 4 and 6 correspond to the polycarbonates
A, B and C without mould release auxiliaries.
The mould release behavior of the polycarbonates of
Examples 1-13 is tested on a conical cylinder of 35 mm length,
20 diameters 40-42 mm and wall thickness 2 mm, by measuring the
pressure which builds up in theejector system. The mould
release pressures and temperatures are shown in Table 1.
Mouldings injection-moulded from the polycarbonates
of Examples 1-13 at 270C have the properties described in
25 Table 2.
Example 2
0.1 kg of mould release auxiliary D is applied to
99.9 kg of polycarbonate A by tumbling in a drum at room
~, temperature and the material is then extruded on an extruder
30at 280C to give a strand which is granulated. The mold
release behavior is tested as in Example 1. The proper-
-15-
LeA 17,847
'
: . , ,: : - ~ . .
.,
... , . . ~ , -
., ' .: :

-
107g886
ties are described in Tables l and 2.
Example 3
0.01 kg of mould release auxiliary D is applied to
99.9 kg of polycarbonate A by tumbling in a drum at room
5 temperature and the material is then extruded on an extruder
at 280C to give a strand which is granulated. The mould
release behavior is tested as in Example l. The properties
are described in Tables l and 2.
Example 5
0.1 kg of mould release auxiliary E is applied to
99.9 kg of polycarbonate B by tumbling in a drum at room
temperature and the material is then extruded on an extruder
at 310C to give a strand which is granulated. The mould
release behavior is tested as in Example 1. The properties
15 are described in Tables 1 and 2.
Example 7
~' 1
0.1 kg of mould release auxiliary F is applied to
99.9 kg of polycarbonate C by tumbling in a drum at room
temperature and the material is then extruded on an extruder
20 at 300C to give a strand which is granulated. The mould
release behavior is tested as in Example 1. The properties
are described in Tables l and 2.
Example 8
0.1 kg of mould release auxiliary G is applied to
25 99.9 kg of polycarbonate A by tumbling in a drum at room
temperature and the material is then extruded on an extruder
at 280C to give a strand which is granulated. The mould
release behavior is tested as in Example 1. The properties
are described in Tables 1 and 2.
16-
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Example 9 (Comparative Example)
0.5 kg of mould release auxiliary H is applied to
99.5 kg of polycarbonate A by tumbling in a drum at room
temperature and the material is then extruded on an extruder
5 at 280C to give a strand which is granulated. The mould
release behavior is tested as in Example 1. The properties
are described in Tables 1 and 2.
Example 10 (Comparative F.xample)
0.1 kg mould release auxiliary H is applied to
10 99.9 kg of polycarbonate A by tumbling in a drum at room
temperature and the material is then extruded on an extruder
at 280C to give a strand which is granulated. The mould
release behavior is tested as in Example 1. The properties
are described in Tables 1 and 2.
15 Example 11 (Comparative Example)
0.1 kg mould release auxiliary Hl is applied to
99.9 kg of polycarbonate A by tumbling in a drum at room
temperature and the material is then extruded on an extruder
at 280C to give a strand which is granulated. The mould
1 20 release behavior is tested as in Example 1. The properties
:i are described in Tables 1 and 2.
Example 12
0.1 kg mould release auxiliary Gl is applied to
; 99.9 kg of polycarbonate A by tumbling in a drum at room
25 temperature and the material is then extruded on an extruder
at 280C to give a strand which is granulated. The mould
~~ release behavior is tested as in Example 1. The properties
: are described in Tab3es 1 and 2.
Example 13
0.1 kg mould release auxiliary G2 is applied to
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99.9 kg of polycarbonate A by tumbling in a drum at room
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at 280C to give a strand which is granulated. The mould
release behavior is tested as in Example 1. The properties
5 are described in Tables 1 and 2.
-18-
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Dessin représentatif

Désolé, le dessin représentatif concernant le document de brevet no 1079886 est introuvable.

États administratifs

2024-08-01 : Dans le cadre de la transition vers les Brevets de nouvelle génération (BNG), la base de données sur les brevets canadiens (BDBC) contient désormais un Historique d'événement plus détaillé, qui reproduit le Journal des événements de notre nouvelle solution interne.

Veuillez noter que les événements débutant par « Inactive : » se réfèrent à des événements qui ne sont plus utilisés dans notre nouvelle solution interne.

Pour une meilleure compréhension de l'état de la demande ou brevet qui figure sur cette page, la rubrique Mise en garde , et les descriptions de Brevet , Historique d'événement , Taxes périodiques et Historique des paiements devraient être consultées.

Historique d'événement

Description Date
Inactive : Périmé (brevet sous l'ancienne loi) date de péremption possible la plus tardive 1997-06-17
Accordé par délivrance 1980-06-17

Historique d'abandonnement

Il n'y a pas d'historique d'abandonnement

Titulaires au dossier

Les titulaires actuels et antérieures au dossier sont affichés en ordre alphabétique.

Titulaires actuels au dossier
BAYER AKTIENGESELLSCHAFT
Titulaires antérieures au dossier
DIETER MARGOTTE
HUGO VERNALEKEN
SIEGFRIED ADELMANN
WERNER NOUVERTNE
Les propriétaires antérieurs qui ne figurent pas dans la liste des « Propriétaires au dossier » apparaîtront dans d'autres documents au dossier.
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Description du
Document 
Date
(aaaa-mm-jj) 
Nombre de pages   Taille de l'image (Ko) 
Revendications 1994-04-06 1 20
Page couverture 1994-04-06 1 23
Abrégé 1994-04-06 1 18
Dessins 1994-04-06 1 7
Description 1994-04-06 18 655