Title of Invention

BRANCHED POLYCARBONATE

Abstract BRANCHED POLYCARBONATE Branched polycarbonate, characterised in that, at 260°C and a shear rate of 10 s1, the polycarbonate has a melt viscosity of 6500 to 8000 Pas and, at 260°C and a shear rate of 1000 s1, a melt viscosity of 880 to 1500 Pas, and that it has an MFR (melt flow index) of 0.1 to 3.0 g/10 min.
Full Text FORM 2
THE PATENTS ACT 1970
[39 OF 1970]

THE PAT


COMPLETE

&
ENTS RULES, 2003


SPECIFICATION
[See Section 10; rule 13]

"BRANCHED

POLYCARBONATE"



BAYER AKTIENGESELLSCHAFT Leverkusen, GERMANY

, a company of Germany, of D-51368

The following specification particularly describes the invention and the manner in which it is to be performed:


The present invention relates to a process for preparing a container by the blow moulding process.
Containers of polycarbonate are known
properties such as for example e properties, elevated resistance to
Containers of polycarbonate exhibit numerous advantageous
levated transparency, good mechanical
to environmental influences and a long

service life together with low weight and straightforward, low-cost producibility.
Polycarbonate containers are produced for example, using the extrusion blow moulding process or the injection blow moulding process. In the extrusion blow moulding process, the pellets are generally melted with a single screw extruder and are shaped by a die to form a free-standing tube, which is subsequently enclosed by a blowing mould, which pinches together the bottom of the tube. The tube is inflated within the mould, thus being shaped as desired. After a cooling period,
the mould is opened and the ho detailed description may be found Polycarbonate in Becker, Braun
llow article may be removed (a more
for example, in Brinkschroder, F.J.
Kunstsoff-Handbuch, volume 3/1,

Polycarbonate, Polyacetale, Polyester, Celluloseester, Carl Hanser Verlag,

Munich, Vienna 1992, pages 257 to
(264).

It is advantageous to use a highly pseudoplastic polycarbonate for extrusion blow moulding in order to ensure elevated melt stability.
Branched polycarbonates are particularly pseudoplastic.
I
The injection blow moulding process is a combination of injection
moulding and blow moulding.

The process proceeds in three stages';: ,
1) injection moulding of the parison in the plastic temperature range of the polycarbonate
2) inflation of the parison in the thermoplastic range of the polycarbonate (the
core of the injection moulding tool is simultaneously the blowing mandrel)
i i
3) stripping of the hollow article and, optionally, cooling of the blowing
I
mandrel with air .
i
i
(a more detailed description may be found, for example, in Anders, S., Kaminski,
A., Kappenstein, R., Polycarbonate in Becker, Braun, Kunststoff-Handbuch, volume
3/1, Polycarbonate, Polyacetale, Pplyester, Celluloseester, Carl Hanser Verlag,
Munich, Vienna 1992, pages 223 to 225).



Known containers of polycarbonate exhibit the disadvantage that they do not meet
certain requirements for practical use. If known containers of polycarbonate are
subjected to severe mechanical stress, the container may burst. This may occur, for
i
example, if a liquid-filled container is dropped from some height onto the ground, for example from the loading area of a truck in which the container is being transported; Such mechanical loads may, for example, be simulated by the drop test as is described in the present text.
The object of the invention is accordingly to provide containers of polycarbonate

which have greater breaking strength subjected to severe mechanical stress.

than known containers of polycarbonate when

The object according to the invention is achieved by containers of branched polycarbonate, characterised in that' at 260°C and a shear rate of 10 s"1, the

polycarbonate has a melt viscosity of

5500 to 9000 Pas, preferably of 6000 to 8000


Pas and particularly preferably of 6500 to 8000 Pas and, at 260°C and a shear rate of

1000 s'1, a melt viscosity of 880

to 1500 Pas, preferably of 900 to 1500 Pas and

particularly preferably of 950 to 1200 Pas and that it has an MFR (melt flow index,

measured to IS01133) of 0.1 to 3

0 g/10 min, preferably of 0.5 to 2.8 g/10 min and

particularly preferably of 0.5 to 2.5 g/10 min


branched polycarbonate contains 1 3,3-bis(3-methyl-4-hydroxyphenyl) as branching agent.


The containers of branched polycarbonate are preferably characterised in that phenol , and/or alkylphenols and/or aryl phenols are used in the production of the branched polycarbonate, with alkylphenols and/or aryl phenols being particularly preferred and alkylphenols being very particularly preferred.
The containers of branched polycarbonate are furthermore preferably characterised in that phenol is used in the production of the branched polycarbonate and that the
,l,l-tris(4-hydroxyphenyl)ethane (THPE) and/or -2-oxo-2,3-dihydroindole (TBK, isatin biscresol)






The containers of branched polycarbonate are furthermore preferably characterised in that the polycarbonate has a branching index at 260°C, defined as the quotient of melt viscosity at a shear rate of 10"' and 1000 s"1, of 6 to 12, preferably of 7 to 12 and particularly preferably of 7 to 10. The branching index is abbreviated to SV index.
The containers of branched polycarbonate are furthermore preferably characterised in that alkylphenols and/or aryl phenols are preferably used in the production of the branched polycarbonate, with alkylphenols being particularly preferred and that the branched polycarbonate contains l,].,l-tris(4-hydroxyphenyl)ethane (THPE) and/or 3,3-bis(3-methyl-4-hydroxyphenyl)-2-6xo-2,3-dihydroindole (IBK, isatin biscresol) as branching agent.
4

The containers of branched polycarbonate are particularly preferably characterised in

that p-tert.-cumylphenol is used as polycarbonate.

the arylphenol in the production of the branched

The containers of branched polycarbonate are furthermore particularly preferably characterised in that p-tert.-butylphenol or isooctylphenol is used as the alkylphenol in the production of the branched polycarbonate.
These containers are accordingly provided by the present invention.



The present invention also provides invention.

the production of the containers according to the





The present invention also provides the use of the containers according to the invention.

The present invention also provides the branched polycarbonates of which the containers consist and which have the above-stated features.
The containers according to the invention exhibit numerous advantages. They are
resistant to mechanical stress, i.e. to breakage, and furthermore exhibit an advantageous range of further mechanical properties. They have good optical.
properties, in particular exhibiting elevated transparency. They have an elevated heat

distortion temperature. Thanks to I the elevated heat distortion temperature, the
i
containers according to the invention may be cleaned with hot water or be sterilized
with steam. They have elevated resistance to conventional cleaning agents, which
are for example used for cleaning water bottles for multi-trip use, one area of
application of the containers according to the invention. They may be produced
easily and at low cost using known processes, the good processing characteristics of
the polycarbonate being of particular advantage in this connection. They exhibit
-5


slight ageing of the material in conventional multi-trip use, this

service and thus a long service life. In the case of means many usage cycles.

Branched polycarbonates suitable according to the invention are both branched

homopolycarbonates and branched, co polycarbonates. A mixture of branched
polycarbonates suitable according to the invention may also be used.
It is possible to add a small proportion of unbranched polycarbonates to the branched polycarbonates, providing that the essential properties, in particular the elevated breaking strength, of the containers produced from the polycarbonates are not impaired.
Preferred branched polycarbonates are those branched homopolycarbonates and branched copolycarbonates based on bisphenols of the general formula (I),

HO-Z-OH

(I)

in which



Z is a divalent organic residue having 6 to 30 C atoms, which contains one or more aromatic groups.





Examples of bisphenols of the general formula (I) are bisphenols which belong to
the following groups: '
dihydroxydiphenyls,
bis(hydroxyphenyl)alkanes,
bis(hydroxyphenyl)cycloalkanes,
indan bisphenols,
bis(hydroxyphenyl) sulfides,
bis(hydroxyphenyl) ethers,
bis(hydroxyphenyl) ketones,

-6-
bis(hydroxyphenyl) sulfones, bis(hydroxyphenyl) sulfoxides and a,a'-bis(hydroxyphenyl)diisopropy

benzenes.

Derivatives of the stated bispheriols, which may for example be obtained by
. ■ • j
alkylating or halogenating the aromatic rings of the stated bisphenols, are also
examples of bisphenols according to the general formula (I).
Examples of bisphenols according to the general formula (I) are in particular the
following compounds:
hydroquinone,
resorcinol,
4,4'-dihydroxydiphenyl,
bis(4-hydroxyphenyl) sulfide,
bis(4-hydroxyphenyl) sulfone,
bis(3,5-dimethyl-4-hydroxyphenyl)methane,
bis(3,5-dimethyl-4-hydroxyphenyl) sulfone,
1,1 -bis(3,5-dimethyl-4-hydroxyphehyl)-p/m-diisopropylbenzene,
1,1 -bis(4-hydroxyphenyl)-1 -phenylethane,
l,l-bis(3,5-dimethyl-4-hydroxyphehyl)cyclohexane,
l,l-bis(4-hydroxyphenyl)-3-methylcyclohexane,
l,l-bis(4-hydroxyphenyl)-3,3-dimethylcyclohexane,
1,1 -bis(4-hydroxyphenyl)-4-methylcyclohexane,
1,1-bis(4-hydroxyphenyl)cyclohexane,
l,l-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane,
2,2-bis(3,5-dichloro-4-hydroxyphenyl)propane, 2,2-bis(3-methyl-4-hydroxyphenyl)propane, 2,2-bis(3,5-dimethyl-4-hydroxyphenyl)propane, 2,2-bis(4-hydroxyphenyl)propane (i.e. bisphenol A), 2,2-bis(3-chloro-4-hydroxyphenyl)propane, 2,2-bis(3,5-dibromo-4-hydroxyphenyl)propane,


2,4-bis(4-hydroxyphenyl)-2-methylbutane,
2,4-bis(3,5-dimethyl-4-hydroxyphenyl)-2-methylbutane,
a,a'-bis(4-hydroxyphenyl)-o-diisqpropylbenzene,
a,a'-bis(4-hydroxyphenyl)-m-diisopropylbenzene (i.e. bisphenolM),
a,a'-bis(4-hydroxyphenyl)-p-diiso|propylbenzene and indan bisphenol.



Particularly preferred branched polycarbonates are the branched homopolycarbonate based on bisphenol A, the branched homopolycarbonate based on l,l-bis(4-hydroxy-0 phenyl)-3,3,5-trimethylcyclohexani5 and the branched copolycarbonates based on the two monomers bisphenol A and l,l-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclo-hexane.

The branched homopolycarbonate based on bisphenol A is very particularly
preferred. l
i
i i
The described bisphenols according to the general formula (I) may be produced using known processes, for example from the corresponding phenols and ketones.
!
The stated bisphenols and processes for the production thereof are described, for
■ i • .
example, in the monograph by H. Schnell, "Chemistry and Physics of Polycarbonates", Polymer Reviews, volume 9, pages 77-98, Interscience Publishers,
i
New York, London, Sydney, 1964 knd in US-A 3 028 635, in US-A 3 062 781, in US-A 2 999 835, in US-A 3 148 in, in US-A 2 991 273, in US-A 3 271 367, in 25, . US-A 4 982 014, in US-A 2 999 8^6, in DE-A 1 570 703, in DE-A 2 063 050, in DE-A 2 036 052, in DE-A 2 211 956, in DE-A 3 832 396 and in FR-A 1 561 518 and in Japanese published patent applications with the application numbers 62039/1986, 62040/1986 and 105550/1986.
I
i
l,l-Bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane and the production thereof is
described, for example, in US-A 4 982 014.





Indan bisphenols and the production thereof are described, for example, in US-A 3 288 864, in JP-A 60 035 150 and in US-A 4 334 106. Indan bisphenols may, for example, be produced from isopropenylphenol or the derivatives thereof or from dimers of isppropenylphenol or the derivatives thereof in the presence of a Friedel-Crafts catalyst in organic solvents.

The branched polycarbonates to be used according to the invention are produced in
known manner from bisphenols, carbonic acid derivatives, branching agents,
alkylphenols and/or aryl phenols, [optionally together with further substances which
may act as chain terminators.
Suitable processes for the production of polycarbonates are, for example, production from bisphenols with phosgene using the phase interface process or from bisphenols
with phosgene using the homogeneous phase process, the so-called pyridine process,
or from bisphenols with carbonic acid esters using the melt transesterification process. These production processes are described, for example, in H. Schnell, "Chemistry and Physics of Polycarbonates", Polymer Reviews, volume 9, pages 31-76, Interscience Publishers, New York, London, Sydney, 1964. The stated
production processes are also described in D. Freitag, U. Grigo, P.R. Miiller, H. Nouvertne, "Polycarbonates" in Encyclopedia of Polymer Science and Engineering, volume 11, second edition, 1988, pages 648 to 718 and in U. Grigo, K. Kircher and P.R. Miiller "Polycarbonate" in Becker, Braun, Kunststoff-Handbuch, volume 3/1, Polycarbonate, Polyacetale, Polyester, Celluloseester, Carl Hanser Verlag, Munich, Vienna 1992, pages 117 to 299 and.in D.C. Prevorsek, B.T. Debona and Y. Kesten, Corporate Research Center, Allied Chemical Corporation, Morristown, New Jersey 07960, "Synthesis of poly(estercarbonate) copolymers" in Journal of Polymer Science, Polymer Chemistry Edition, volume 19, 75-90 (1980).
The melt transesterification process is in particular described in H. Schnell,
"Chemistry and Physics of Polycarbonates", Polymer Reviews, volume 9, pages 44



to 51, Interscience Publishers, New York, London, Sydney, 1964 and in DE-A 1 031 512, inUS-A 3 022 272, inUS-A 5 340 905 and inUS-A 5 399 659.
The branched polycarbonates to be used according to the invention are preferably
produced using the phase interface process or the known melt transesterification
process. In the first case, the carbonic acid derivative is preferably phosgene, in the second case preferably diphenyl carbonate.
The polycarbonate is preferably produced using raw materials and auxiliaries which
have a low content of contaminants. In particular when production is performed
using the melt transesterification process, the introduced bisphenols and the

introduced carbonic acid derivatives should have the lowest possible content of
alkali metal ions and alkaline earth metal ions. Raw materials of such purity are, for

example, obtained by recrystallising, washing or distilling the carbonic acid
derivatives, for example carbonic and esters, and the bisphenols.
When producing polycarbonates by the melt' transesterification process, the
bisphenol and the carbonic acid diester may be reacted continuously or
i
discontinuously, for example in stirred-tank reactors, thin film evaporators, falling
film evaporators, stirred-tank reactors connected in series, extruders, kneaders,
i simple disk reactors and high viscosity disk reactors.
Carbonic acid diesters which may be used for the production of polycarbonates are,
for example, diaryl esters of carbonic acid, wherein both of the aryl residues
preferably each have 6 to 14 C atoms. Carbonic acid diesters based on phenol or
alkyl-substituted phenols, i.e. for example diphenyl carbonate or dicresyl carbonate, are preferably used. Relative to 1 niol of bisphenol, the carbonic acid diesters are preferably used in a quantity of 1.01 to 1.30 mol, particularly preferably in a quantity of 1.02 to 1.15 mol.
--/O-




The branched polycarbonates according to the invention have a weight average
i
molar mass Mw of preferably 12000 to 120000 g/mol, particularly preferably of 26000 to 50000 g/mol and in particular of 31000 to 40000 g/mol (determined by measuring relative viscosity at 25°C in methylene chloride at a concentration of 0.5 g per 100 ml of methylene.; chloride and with calibration of the viscosity measurement by ultra centrifugation or measurement of light scattering).
The phenols, alkylphenols and/or aryl phenols used in the production of the branched polycarbonates according to the invention act as chain terminators, i.e. they limit the maximum achievable average mplar mass. They are added either together with the monomers, which are required for the production of the polycarbonate, or during a subsequent phase of polycarbonate synthesis. They act as nonfunctional compounds for the purposes of polycarbonate synthesis and thus act as chain terminators.
The phenol, alkylphenols and/or arylphenols used for the production of the branched polycarbonates are preferably used in a quantity of 0.25 to 10 mol%, relative to the total of bisphenols used in each case.

Mixtures of phenol and/or one or more alkylphenols and/or arylphenols may also be
used. !
The alkylphenols and/or arylphenols used in the production of the branched
I polycarbonate give rise to alkylphenyl end groups and arylphenyl end groups
respectively. Depending upon the production process, other end groups may also
occur in the resultant polycarbonate, such as for example phenolic OH end groups or
chlorocarbonic acid ester end groups.
! ' •
Preferably, solely phenol, alkylprenols and/or arylphenols are used, without the
addition of further substances which may act as chain terminators.

Particular preferably, solely alkylphenols and/or arylphenols are used, without the addition of further substances which may act as chain terminators.
One preferred alkylphenol is, fori example, para-tert.-butylphenol (c.f. Huston, Am.
Soc. 58, 439; US-A 2 051 300). Para-tert.-butylphenol is a commercial product and
may, for example, be obtained from Huls AG, Marl, Germany or PPG Industries,
USA. Another preferred alkylphenol is para-cumylphenol (c.f. Welsch, Am. Soc. 60,
58 (1983)). Another preferred alkylphenol is isooctylphenol (c.f. US-A 2 415 069).
Isooctylphenol is a commercial product and may, for example, be obtained from
Huls AG, Marl, Germany. These alkylphenols and the production thereof are known
to the average person skilled in ^he art. A review of the use and the production thereof is described in Houben Weyl, Methoden der organischen Chemie, G. Thieme Verlag, 4th edition (1976), volume 6/lc, pages 951 etseq..
When producing the branched polycarbonates according to the invention, further substances which may act as chain terminators may be used in addition to the alkylphenols and/or arylphenols.
Substances suitable for this purpose which may act as chain terminators are both monophenols and monocarboxylic acids. Suitable monophenols are, for example, phenol, p-chloroprene or 2,4,6-tribromophenol. Suitable monocarboxylic acids are benzoic acid, alkylbenzoic acids and halobenzoic acids.



The preferred further substance which may act as chain terminator is phenol.
I The quantity of further substances which may act as chain terminators is preferably
I between 0.25 and 10 mol%, relative to the total of the bisphenols used in each case.
i
The branched polycarbonates suitable according to the invention are branched in known manner, specifically preferably by incorporation of trifunctional or greater than trifunctional branching agents. Suitable branching agents are, for example,

~12~

those having three or more than three phenolic groups or those having three or more than three carboxylic acid groups.
Suitable branching agents are, for example, phloroglucinol, 4,6-dimethyl-2,4,6-tri-
(4-hydroxyphenyl)-2-heptene, 4,6-dimethyl-2,4,6-tri-(4-hydroxyphenyl)heptane,
. l,3,5-tri-(4-hydroxyphenyl)benzene, l,l,l-tris(4-hydroxyphenyi)ethane, tri-(4-
hydroxyphenyl)phenylmethane, 2,2-bis [4,4-bis(4-
hydroxyphenyl)cyclohexyl]propane, 2,4-bis(4-hydroxyphenylisopropyl)phenol, 2,6-
bis(2-hydroxy-5,-methylbenzyl)-4Tmethylphenol, 2-(4-hydroxyphenyl)-2-(2,4-
dihydroxyphenyl)propane, hexa-(4-(4-hydroxyphenylisopropyl)phenyl)terephthalic
acid , ester, tetra-(4-hydroxyphenyl)rnethane, tetra-(4-(4-
hydroxyphenylisopropyl)phenoxy)methane and l,4-bis(4',4"-dihydroxy-
triphenyl)methylbenzene as well as 2,4-dihydroxybenzoic acid, trimesic acid, cyanuric chloride, 3,3 -bis(3 -methyl-4-hydroxyphenyl)-2-oxo-2,3-dihydroindole, 15 trimesic acid trichloride and a,a',a"-tris(4-hydroxyphenol)-1,3,5-triisopropylbenzene.
Preferred branching agents are l,l,l-tris(4-hydroxyphenyl)ethane (THPE) and 3,3-bis(3-methyl-4-hydroxyphenyl)-2-oxo-2,3-dihydroindole (IBK, isatin biscresol).

The quantity of the optionally used branching agents is preferably 0.05 mol% to 2 mol%, more preferably Ul mol% to 0.8 mol% and very particularly preferably 0.25 mol% to 0.6 mol%, relative to the moles of bisphenols used.
The branching agents may, for example when producing the polycarbonate by. the
phase interface process, be initially introduced into the aqueous alkahne phase
together with the bisphenols and the chain terminators or be added as a solution in
an organic solvent together with the carbonic acid derivatives. In the case of the
transesterification process, the branching agents are preferably apportioned together
J, I
with the dihydroxyaromatics or bisphenols.
13-



The properties of the branched polycarbonates according to the invention may be
modified by incorporating conventional additives and/or by applying them onto the
surface. Conventional additives are, for example: fillers (for example mineral
fillers), reinforcing agents (for example glass fibres), stabilisers (for example UV
|stabilisers, heat stabilisers, gamma radiation stabilisers), antistatic agents, flow
auxiliaries, mould release agents, flam e retardants, dyes and pigments, providing
that they do not impair the good mechanical properties of the moulding
compositions. The stated and further suitable additives are described, for example, in
Gachter, Miiller, Kunststoff-Additive, 3rd edition, Hanser Verlag, Munich, Vienna,
1989.
Other polymers may be mixed with the branched polycarbonates according to the invention, resulting in so-called polymer blends, providing that the essential properties, in particular the elevated breaking strength of the containers produced lj) from the polycarbonates, are not impaired. Blends may, for example, be produced from the polycarbonates according to the invention and ABS polymers or from the polycarbonates according to the invention and polyesters, such as for example polyethylene terephthalate or polybutylene terephthalate.



Containers for the purposes of the present invention may be used for the packaging, storage or transport of liquids, solids or gases. Contamers for the packaging, storage or transport of liquids (liquid containers) are preferred, with contamers for the packaging, storage or transport of water (water bottles) being particularly preferred.
Containers for the purposes of the invention are hollow articles having a volume of preferably 0.1 L to 50 L, more preferably from 0.5 L to 50 L, with volumes of 1 L, 5
L, 12 L and 20 L being very particularly preferred.
[ ■ Water bottles having a volume of 3 to 5 gallons are very particularly preferred.





14





The containers have an empty weight of preferably 0.1 g to 3000 g, more preferably of 50 g to 2000 g and particularly preferably of 650 g to 900 g.
The wall thicknesses of the containers are preferably 0.5 mm to 5 mm, more preferably 0.8 mm to 4 mm.
Containers for the purposes of the present invention have a length of preferably 5 mm to 2000 mm, particularly preferably from 100 mm to 1000 mm.
The containers have a maximum circumference of preferably 10 mm to 250 mm, more preferably from 50 mm to 150 mm and very particularly preferably from 70 to 90 mm.

Containers for the purposes of the invention preferably have a bottle neck of a length 15| of preferably 1 mm to 500 mm, more preferably of 10 mm to 250 mm, particularly preferably of 50 mm to 100 mm and very particularly preferably of 70 to 80 mm.
The wall thickness of the bottle neck of the container preferably ranges between 0.5 mm and 10 mm, particularly preferably from 1 mm to 10 mm and very 20 particularly preferably from 5 mm to 7 mm.



The diameter of the bottle neck ranges between preferably 5 mm and 200 mm; 10 mm to 100 mm are particularly preferred and 45 mm to 75 mm are very particularly preferred.
The bottom of the containers according to the invention has a diameter of preferably • 10 mm to 250 mm, more preferably of 50 mm to 150 mm and very particularly preferably of 70 to 90 mm.

Containers for the purposes of the present invention may have any desired geometric shape, they may for example be'round, oval or polygonal or multi-sided having for example 3 to 12 sides. Round, oval and hexagonal shapes are preferred.
The design of the containers may be based on any desired surface textures. The surface textures are preferably smooth or ridged. The containers according to the invention may also exhibit two of more different surface textures. Ribs or beads may run around the circumference of the containers. They may be spaced at will or have any two or more differing spacings. The surface textures of the containers according to the invention may comprise roughened or integrated textures, symbols, ornaments, coats of arms, brands, trademarks, monograms, manufacturer's details, material designations or volume details.
The containers according to the invention may have any desired number of handles,
which may be located on the sides, top or bottom of the container. The handles may
' be external or incorporated into the outline of the contamer. The handles may be
collapsible or fixed. The handles may have any desired outline, for example oval,
round or polygonal. The handles preferably have a length of 0.1 mm to 180 mm,
preferably 20 mm to 120 mm.
Apart from the polycarbonate according to the invention, the containers according to
the invention may additionally contain small quantities of other substances, for
example seals of rubber or handles; of other materials.
The containers according to the invention are preferably produced using the

extrusion blow moulding process or using the injection blow moulding process.
i
In a preferred embodiment of the process for the production of the containers according to the invention, the polycarbonates according to the invention are processed in extruders having a smooth or grooved feed zone, preferably a smooth feed zone.


The drive power of the extruder is selected in accordance with the screw diameter.
■ By way of example, at a screw diameter of 60 mm, the drive power of the extruder is approx. 30 to 40 kW, while at a screw diameter of 90 mm it is approx. 60 to 70 kW.
Multipurpose, three section screws as are conventional for processing industrial thermoplastics are suitable.
A screw diameter of 50 to 60 miri is preferred for the production of containers of a volume of 1 L. A screw diameter of 70 to 100 mm is preferred for the production of containers of a volume of 20 L. The length of the screws is preferably 20 to 25 times the diameter of the screw.
In the case of the blow moulding process, the blowing mould is preferably adjusted
to a temperature of 50 to 90°C in order to obtain a glossy, high quality surface on the
container.
In order to ensure uniform and effective temperature control of the blowing mould, the temperatures of the base area and the jacket area are separately controllable.

The blowing mould is preferably closed with a pinch force of 1000 to 1500 N per cm of pinch seam length.
The polycarbonate according to the invention is preferably dried before processingto ensure that the optical quality of the containers is not impaired by streaks or
bubbles and the polycarbonate is hot hydrolysed during processing. The residual
moisture content after drying is preferably less than 0.01 wt.%. A drying temperature
of 120°C is preferred. Lower temperatures do not ensure adequate drying, while at
higher temperatures there is a risk of the individual polycarbonate pellets sticking
together, thus rendering them unprocessable. Dry air dryers are preferred.
-I7-



The preferred melt temperature during processing of the polycarbonate according to the invention is 230 to 300°C.
The containers according to the invention may be used for the packaging, storage or b transport of liquids, solids or gases. The embodiment as containers which are used for example for the packaging, storage or transport of liquids is preferred. The embodiment as a water bottle, which may for example be used for the packaging, storage or transport of water, is particularly preferred.
A preferred embodiment of the invention is that in which the container of branched polycarbonate is characterised in that the branched polycarbonate contains THPE and/or IBK as branching agent and in which alkylphenols are used in the production of the branched polycarbonate and in which the container is a water bottle.
A particularly preferred embodiment of the invention is that in which the container
of branched polycarbonate is characterised in that the branched polycarbonate contains THPE and/or IBK as branching agent and in which phenol is used in the production of the branched polycarbonate and in which, at 260°C and a shear rate of 10 s"1, the polycarbonate has a melt viscosity of 5500 to 7000 Pas, and, at 260°C and
a shear rate of 1000 s"1, a melt viscosity of 900 to 1100 Pas and has an MFR (melt flow index, measured to IS01133) of A particularly preferred embodiment of the invention is furthermore that in which
the container of branched polycarbonate is characterised in that the branched
polycarbonate contains l,l,l-tris(4|-hydroxyphenyl)ethane (THPE) and/or 3,3-bis(3-methyl-4-hydroxyphenyl)-2-oxo-2,3-dihydroindole (IBK, isatin biscresol) as branching agent and in which para-tert.-butylphenol and/or para-cumylphenol and/or para-isooctylphenol are used in the production of the branched polycarbonate and in which the container is a water bottle.
-18


One particularly preferred embodiment within the latter stated embodiment is that in which the branched polycarbonate contains solely l,l,l-tris(4-hydroxyphenyl)ethane (THPE) and/or 3,3-bis(3-methyl-4-hydroxyphenyl)-2-oxo-2,3-dihydroindole (TBK, isatin biscresol) as branching agent and in which para-tert.-butylphenol and/or para-cumylphenol and/or para-isooc'tylphenol are used in the production of the branched polycarbonate.
One particularly preferred embodiment within the latter stated embodiment is that in
which the branched polycarbonate contains solely l,l,l-tris(4-hydroxyphenyl)ethane
(THPE) and/or 3,3-bis(3-methyl-4-hydroxyphenyl)-2-oxo-2,3-dihydroindole (TBK,
isatin biscresol) as branching agent and in which para-isooctylpheno.l is used in the production of the branched polycarbonate.
Breaking strength of the containers is preferably evaluated using the drop test, which
is described below.
Preparation for the actual measurement proceeds such that the shape and mass of the container are determined before the measurement. The test only compares containers of identical shape and identical mass. The mass of containers compared in the drop test may only differ by a maximum of 5 %.
The container is filled with distilled water at room temperature and then placed on a
trapdoor platform, the floor of which takes the form of a trapdoor. For the first
measurement, the trapdoor platform is raised until its floor is 0.5 m above the floor
beneath, which consists of a thick steel plate. The trapdoor is then opened such that
the water-filled container falls on me floor. If the container is not broken, the same container is put back on the trapdoor platform and raised to a height of 1 m for a second measurement by the container being dropped again in the described manner. Further measurements are made, with the drop height being raised by 0.5 m in each case. In this manner, a failure drop height is determined, which is defined as the height at which the hollow article breaks and the water runs out. An average failure
19


drop height, a mean from ten drop tests, is used as a measure of the mechanical strength of the containers.
The container according to the invention is illustrated in greater detail below by means of a drawing (Fig. 1) which merely represents a preferred example.
Fig. 1 is a cross-section through a rotationally symmetrical container (a water bottle). The container has a weight of 780 g ± 15 g, a height of approx. 485 mm and a neck diameter of approx. 54.8 mm, circumference approx. 855 mm. It consists of branched polycarbonate. The container holds a volume of 18.9 L (5 gallons).
The following examples illustrate the invention in greater detail.
A container according to the invention according to Fig. 1 was produced by the extrusion blow moulding process using a blow moulding machine from Krupp-Kautex Maschinenbau GmbH, Bonn, Germany (extruder: screw diameter: 90 mm, effective screw length: 22D, head: 3.5 L Fifo, closing force: 300 kN, cycle time: 31s to 32 s, ejection time: 5.3 s to 5.6 s) at a melt temperature of 260°C and a blowing mould temperature of approx. 90°C from branched bisphenol A polycarbonates (Examples 1 to 7, Table 1 and Comparative Examples 1 to 5, Table 2). These bisphenol A polycarbonates were produced using the phase interface process. The chain terminators and branching agents used are shown in Tables 1 and 2. The branching agent content was 0.30 mol% in all the Examples and Comparative Examples. The same tables state the associated MFR values, melt viscosity at shear rates of 10 s'1 and 1000 s"1 at a temperature of 260°C and the SV index (= branching index).
The containers according to the invention were subjected to the drop test described in the present text.
20
Ten tests were performed per container and an average failure drop height, corresponding to a mean value; from the ten values, was calculated from the ten measurements.
The container used in the tests was of the form shown in Fig. 1.
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Table 1

Example Chain terminator Branching agent MFR Shear rates at 260°C 10 s'1 1000 s_1 SV . index

1 phenol ; IBK 2.5 6653 , 953 7.0
2 phenol THPE 2.7 6414 954 6.7
3 p-tert.-butylphenol ! BK . 2.8 6616 976 6.6
4 p-tert.-butylphenol THPE 2.7 6390 996 6.4
5 p-cumylphenol BK 2.0 7212 980 7.4
6 p-cumylphenol THPE 2.3 6862 1041 6.6
7 . isooctylphenol BK 2.2 6905 968 7.1
Table 2

Comparative Example Chain terminator Branching agent MFR Shear rate 10 s"1 s at 260°C 1000 s"1 SV index

. 1 phenol BK 3.2 5220 870 6.0
2 phenol THPE 3.5 4912 847 5.8
3 p-tert.-butylphenol BK 3.7 4876 855 5.7
4 p-tert.-butylphenol THPE ... 3.4 4998 841 5.9
5 p-cumylphenol• i THPE 3.7 4896 874 5.6

Results of the drop test:
Table 3

Example Average failure drop height in m
1 2.8
2 2.9
3 3.2
4 3.3
5 i 3.8
6 3.6
7 3.6
.5
Table 4

Comparative Example Average failure drop height in m
1 1.5i
2 17
3 2.1
4 2.3
5 22
The examples demonstrate the superior breaking strength of the containers according
ID to the invention.

We claim:

1. Branched polycarbonate, characterised in that, at 260°C and a shear rate of 10 s_1, the polycarbonate has a melt viscosity of 6500 to 8000 Pas and, at 260°C and a shear rate of 1000 s1, a melt viscosity of 880 to 1500 Pas, and that it has an MFR (melt flow index) of 0.1 to 3.0 g/10 min.
2. Branched polycarbonate as claimed in claim 1, wherein phenol and/or alkylphenols and/or arylphenols are used iii the production of the branched polycarbonate.
3. Branched polycarbonate as claimed in claim 1, wherein phenol is used in the production of the branched polycarbonate and that the branched polycarbonate contains 1,1,1- tris(4-hydroxyphenyl)ethane (THPE) and/or 3, 3- bis(3-methyl-4- hydroxyphenyl)-2-oxo-2,3-dihydroindole (IBK, isatin biscresol) as branching agent.
4. Branched polycarbonate as claimed in claim 1, wherein alkylphenols and/or arylphenols are used in the production of the branched polycarbonate, and that the branched polycarbonate contains 1,1,1 -tris(4-hydroxyphenyl)ethane (THPE) and/or 3, 3-bis(3-methyl-4-hydroxyphenyl)-2-oxo-2,3-dihydroindole (IBK, isatin biscresol) as branching agent.
Dated this 26th the day of July, 2005.





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ABSTRACT
BRANCHED POLYCARBONATE
Branched polycarbonate, characterised in that, at 260°C and a shear rate of 10 s1, the polycarbonate has a melt viscosity of 6500 to 8000 Pas and, at 260°C and a shear rate of 1000 s1, a melt viscosity of 880 to 1500 Pas, and that it has an MFR (melt flow index) of 0.1 to 3.0 g/10 min.

Documents:

831-mumnp-2005-abstract(12-03-2007).doc

831-mumnp-2005-abstract(12-03-2007).pdf

831-mumnp-2005-abstract.doc

831-mumnp-2005-abstract.pdf

831-mumnp-2005-cancelled pages(12-03-2007).pdf

831-mumnp-2005-claims(granted)-(12-03-2007).doc

831-mumnp-2005-claims(granted)-(12-03-2007).pdf

831-mumnp-2005-claims.doc

831-mumnp-2005-claims.pdf

831-mumnp-2005-correspondence(29-11-2007).pdf

831-mumnp-2005-correspondence-(ipo)-(04-07-2007).pdf

831-mumnp-2005-correspondence-others.pdf

831-mumnp-2005-correspondence-received-ver-020106.pdf

831-mumnp-2005-correspondence-received-ver-080506.pdf

831-mumnp-2005-correspondence-received-ver-120307.pdf

831-mumnp-2005-correspondence-received-ver-130306.pdf

831-mumnp-2005-correspondence-received-ver-250705.pdf

831-mumnp-2005-description (complete).pdf

831-mumnp-2005-drawing(12-03-2007).pdf

831-mumnp-2005-drawings.pdf

831-mumnp-2005-form 1(26-07-2005).pdf

831-mumnp-2005-form 18(05-01-2006).pdf

831-mumnp-2005-form 2(granted)-(12-03-2007).doc

831-mumnp-2005-form 2(granted)-(12-03-2007).pdf

831-mumnp-2005-form 3(12-03-2007).pdf

831-mumnp-2005-form 3(25-07-2005).pdf

831-mumnp-2005-form 5(12-03-2007).pdf

831-mumnp-2005-form-1.pdf

831-mumnp-2005-form-18.pdf

831-mumnp-2005-form-2.doc

831-mumnp-2005-form-2.pdf

831-mumnp-2005-form-26.pdf

831-mumnp-2005-form-3-ver-250705.pdf

831-mumnp-2005-form-3.pdf

831-mumnp-2005-form-5-ver-250705.pdf

831-mumnp-2005-form-5.pdf

831-mumnp-2005-power of authority(12-03-2007).pdf

831-mumnp-2005-power of authority(26-07-2005).pdf

abstract1.jpg


Patent Number 218646
Indian Patent Application Number 831/MUMNP/2005
PG Journal Number 24/2008
Publication Date 13-Jun-2008
Grant Date 04-Apr-2008
Date of Filing 26-Jul-2005
Name of Patentee BAYER AKTIENGESELLSCHAFT
Applicant Address D-51368 LEVERKUSEN,
Inventors:
# Inventor's Name Inventor's Address
1 KLAUS HORN BAHNHOFSTR 13, D-41539 DORMAGEN, GERMANY
2 WOLFGANG ALEWELT Stratumer Feld 17 D-47809 Krefeld
3 FRANK BRUYNSEELS Oude Molenstraat 9G, B-9170 Sint-Gillis-Waas
4 RALF HUFEN Zum Roltgenhof 25, D-47239
5 PETER GEBAUER Alternrather Str.100, D-53797, Lohmar
PCT International Classification Number C08G64/14
PCT International Application Number PCT/EP00/08471
PCT International Filing date 2000-08-31
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 199 43 642.8 1999-09-13 Germany