Title of Invention

'A PROCESS FOR THE PREPARATION OF COMPATIBILEZED POLYMER BLENDS.

Abstract A process for the preparation of compatibilized polymer blends useful for high performance applications which comprises, melt blending poly(phenylene sulphide) and an aliphatic-aromatic liquid crystalline polymer and the said poly(phenylene sulphide) to aliphatic-aromatic liquid crystalline polymer being in the range from 97 to 10% in melt in a suitable blender in an inert atmosphere and in the presence of a compatibilizer being in the range from 1 to 10% at a temperature in the range of 300 to 320°C, for a period ranging from 3 to 5 minutes, removing   the compatibilized blend in the form of lumps and allowing the product to cool to ambient temperature or by extruding the blend to get the product in the form of strands or pellets. The compatibilized blends are useful in high performance applications such as pump housing ,gears and impellers.
Full Text This invention relates to a process for the preparation of a corapatibilized polymer blend. More particularly it relates to a process for the preparation of compatibilized blend of poly(phenylene sulphide) and an aliphatic-aromatic liquid crystalline polymer using a compatibilizer. The compatibilized blends prepared by the process of this invention are useful in high performance applications such as pump housings, gears, impellers. The compatibilized blends prepared by the process of this invention are new.
Polymer blends are the resultant product of mixing two or more polymers. The conventional methods of mixing of the polymers to prepare polymer blends are solution or melt blending rather than physical blending of the individual polymers. The method of preparing the blend determines the resultant properties and hence is of paramount importance. Most polymers are not miscible and the blends are usually phase separated with the extent of phase separation dependent on the mixing mechanism and the ratio of the individual polymers that are used for the preparation of the blend. The immiscible polymers in certain cases can be made to form a miscible system with the use of modifiers called as compatibilizers. Another approach is by in situ chemical reaction during the process of blending.
Compatibilizers for polymers could be defined as materials that induce miscibility of two thermodynamically immiscible polymers. Conventionally these materials comprise of block or graft copolymers with long segments or blocks that have

characteristics of miscibility at the interface. The addition of compatibilizers reduces the interfacial energy between the immiscible phases and they also ensure finer dispersion when two immiscible phases are brought together during mixing operation. They also provide better stability against separation of the two phases and to increase the adhesion at phase boundaries giving improved stress transfer.
Compatibilization of blend components is an important factor to be considered when designing blends and is often the primary criterion for commercial success.
Blending of thermoplastic polymers are resorted when the resultant material can lead to easier processing and in situ matrix reinforcement in some cases depending on the choice of the polymers that are used for blending.
An important reason in seeking new polymer blends is cost-effectiveness, coupled with synergistic improvement in the properties of the individual polymers.
The use of liquid crystalline polymers in the preparation of blends has the following advantages :
1. Since liquid crystalline polymers have very low thermal coefficient of expansion, the problem of mold shrinkage is greatly reduced. This factor also allows a high tolerance in molded components.

2. The melt viscosity of liquid crystalline is low compared with the conventional thermoplastic polymers. Liquid crystalline polymers in blends therefore act as a processing aid thus acting as a viscosity modifier.
Poly(phenylene sulphide) has very good thermal stability and chemical resistance, potentially important characteristics for an TLCP blend. TLCPs having excellent processing characteristics and mechanical properties. Poly(phenylene sulphide and TLCPs are high strength/high temperature speciality polymers that find applications in the electrical and electronic industries. However, TLCPs are generally incompatible with PPS. The properties of blends are strongly influenced by their morphology as a consequence of incompatibility and phase separation.
The main object of this invention is to provide a process for the preparation of compatibilized polymer blends of PPS and a thermoplastic liquid polymer useful for high performance applications.
Another object of the present invention is to provide a process for the preparation of compatibilized blend of poly(phenylene sulphide) and a thermotropic liquid crystalline polymer.
Yet another object of the invention is to provide a process for the preparation of compatibilized blend of poly(phenylene sulphide) and a thermotropic liquid crystalline polymer using an aliphatic-aromatic compatibilizer.

Accordingly, the invention describes a process for the
preparation of compatibilized polymer blends useful for high performance applications which comprises, melt blending poly(phenylene sulphide) and an aliphatic-aromatic liquid crystalline polymer of the kind such as herein described and the said poly(phenylene sulphide) to said aliphatic-aromatic liquid crystalline polymer being in the range form 97 to 10% in melt in a suitable blender in an inert atmosphere and in the presence of a compatibilizer such as herein described being in the range from 1 to 10% at a temperature in the range of 300 to 320°C, for a period ranging from 3 to 5 minutes, removing the compatibilized blend in the form of lumps and allowing the product to cool to ambient temperature or by extruding the blend to get the product in the form of strands or pellets.
According to an embodiment of the invention, the inert gas used could be chosen from nitrogen, argon or the like.
According to another embodiment of the invention, the compatibilizer used may be prepared as described and claimed in our copending application NF-147/97application no
According to yet another embodiment of the invention, the
aliphatic-aromatic liquid polymer used may be such as
polyethylene terephthalate-co-oxy benzoate, polybutylene
terephthalate-co- oxy benzoate polymers.
According to yet another embodiment of the invention, the blend ratio of PPS to aliphatic-aromatic thermoplastic liqui According to yet another embodiment of the invention, the

amount of compatibilizer used may vary from 1 to 10 %.
The process of the present invention is described with reference to following examples which are illustrative only and should not be construed to limit the scope of this invention in any manner.
Example 1 :
48.5 grams of poly(phenylene sulphide) and 1.5 grams of poly(ethylene terephthalate-co-oxybenzoate) and 0.45 gm of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at a temperature of 300°C for 3 minutes under an atmosphere of nitrogen. After 3 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.8 grams. The blend thus produced had a melting transition of 278°C.
Example 2 :
47.5 grams of poly(phenylene sulphide), 2.5 grams of poly(ethylene terephthalate-co-oxybenzoate) and 0.0125 gm of modified oligo poly(phenylene sulphide)were blended using Brabender Plasticorder at a temperature of 310°C for 3 minutes under a atmosphere of argon. After 3 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.8 grams. The blend thus produced had a melting transition of 276°C.

Example 3 :
45.0 grams of poly(1,4-thiophenylene), 5.0 grams of poly(ethylene terephthalate-co-oxybenzoate) and 0.025 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 4 minutes under an atmosphere of nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 47.4 grams. The blend thus produced had a melting transition of 274°C.
Example 4 :
40.0 grams of poly(1,4-thiophenylene), 10.0 grams of poly(ethylene terephthalate-co-oxybenzoate) arid 0.02 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 320°C for 3 minutes under an atmosphere of nitrogen . After 3 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.2 grams. The blend thus produced had a melting transition of 271°C.
Example 5 :
35.0 grams of poly (1,4-thiophenylene) , 15.0 grams of poly(ethylene terephthalate-co-oxybenzoate) and 0.45 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 3 minutes under an atmosphere of nitrogen . After 3 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield

obtained was 49.6 grams.
The blend thus produced had a melting transition of 271°C.
Example 6 :
25.0 grams of poly(1,4-thiophenylene), 25.0 grams of poly(ethylene terephthalate-co-oxybenzoate) and 2.82 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 5 minutes under an atmosphere of nitrogen . After 5 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 48.5 grams. The blend thus produced had a melting transition of 268°C.
Example 8 :
5.0 grams of poly(1,4-thiophenylene), 45.0 grams of poly(ethylene terephthalate-co-oxybenzoate) and 2.82 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 4. minutes under an atmosphere of nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 48.6 grams. The blend thus produced had a melting transition of 261°C.
Example 9 :
48.5 grams of poly(1,4-thiophenylene), 1.5 grams of poly(butylene terephthalate-co-oxybenzoate) and 0.04 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 5 minutes under an atmosphere of

nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.6 grams. The blend thus produced had a melting transition of 278°C.
Example 10 :
47.5 grams of poly(1,4-thiophenylene), 2.5 grams of poly(butylene terephthalate-co-oxybenzoate) and 0.01 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 5 minutes under an atmosphejre of nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.2 grams. The blend thus produced had a melting transition of 275°C.
Example 11 :
45.0 grams of poly(1,4-thiophenylene), 5.0 grams of poly(ethylene terephthalate-co-oxybenzoate) and 0.45 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 310°C for 3 minutes under an atmosphere of nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 48.2 grams. The blend thus produced had a melting transition of 274°C.
Example 12 :
40.0 grams of poly(1,4 -thiophenylene) , 10.0 grams of poly(butylene terephthalate-co-oxybenzoate) and 0.02 gram of

modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 3 minutes under an atmosphere of nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.2 grams. The blend thus produced had a melting transition of 271°C.
Example 13 :
40.0 grams of poly(1,4-thiophenylene), 10.0 grams of poly(ethylene terephthalate-co-oxybenzoate) and 1.2 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 4 minutes under an atmosphere of nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.2 grams. The blend thus produced had a melting transition of 271°C.
Example 14 :
35.0 grams of poly(1,4-thiophenylene), 15.0 grams of poly(ethylene terephthalate-co-oxybenzoate) and 2.5 gram of modified oligo poly(phenylene sulphide) were blended using Brabender Plasticorder at 300°C for 5 minutes under an atmosphere of nitrogen . After 5 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 49.8 grams. The blend thus produced had a melting transition of 269°C.

Example 15 :
12.5 grams of poly(1,4 -thiophenylene) , 37.5 grams of poly ( e thy lene t erephtha 1ate co- oxyberizoate ) and 4.6 qi'am of compatibilizer were blended vising Brabender Plasticorder at 300°C for 3 minutes under an atmosphere of nitrogen . After 4 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 52.2 grams. The blend thus produced had a melting transition of 276°C.
Example 16 :
5.0 grains of poly (1 , 4 - thiophenylene) , 45.0 grams of poly ( ethy lene te rephthalate - co - oxybenzoat.e ) and 5.02 qram of compatibilizer were blended using Brabender Plasticorder at. 300°C for 5 minutes under an atmosphere o of nitrogen . After 5 minutes of mixing, the product was removed in the form of lumps and cooled to ambient temperature. The yield obtained was 53.2 grams.
The blend thus produced had a melting transition of 274°C. The advantages of the process of this invention are :
1. The blend will have better processing characteristics.
2. The mechanical properties of the blend are better than the
uncompatibi1ized blends .
3. The mold shrinkage of the blend is reduced.
4. Heat -distortion temperature of the blend is increased.





We claim:
1. A process for the preparation of compatibilized polymer blends useful for high
performance applications which comprises, melt blending poly(phenylene
sulphide) and an aliphatic-aromatic liquid crystalline polymer of the kind such as
herein described and the said poly(phenylene sulphide) to said aliphatic-aromatic
liquid crystalline polymer being in the range form 97 to 10% in melt in a suitable
blender in an inert atmosphere and in the presence of a compatibilizer such as
herein described being in the range from 1 to 10% at a temperature in the range of
300 to 320°C, for a period ranging from 3 to 5 minutes, removing the
compatibilized blend in the form of lumps and allowing the product to cool to
ambient temperature or by extruding the blend to get the product in the form of
strands or pellets.
2. A process as claimed in claim 1, wherein the inert gas used is selected from
nitrogen, argon.
3. A process as claimed in claim 1, wherein the compatibilizer used is an aliphatic-
aromatic compatibiliser such as herein described
4. A process as claimed in claims 1 to 3, wherein the aliphatic-aromatic liquid
polymer used is such as polyethylene terephthalate-co-oxy benzoate, polybutylene
terephthalate-co-oxy benzoate polymers.
5. A process for the preparation of compatibilized polymer blends substantially as
herein described with reference to the examples.


Documents:

1298-del-1998-abstract.pdf

1298-del-1998-claims.pdf

1298-del-1998-correspondence-others.pdf

1298-del-1998-correspondence-po.pdf

1298-del-1998-description (complete).pdf

1298-del-1998-form-1.pdf

1298-del-1998-form-19.pdf

1298-del-1998-form-2.pdf


Patent Number 215019
Indian Patent Application Number 1298/DEL/1998
PG Journal Number 10/2008
Publication Date 07-Mar-2008
Grant Date 20-Feb-2008
Date of Filing 15-May-1998
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI 110001.
Inventors:
# Inventor's Name Inventor's Address
1 THOTTUPURATHU THEKKETHIL GOPIKUTT AN NAIR GOPAKUMAR NATIONAL CHEMICAL LABORATORY, PUNE-411008, MAHARASHTRA, INDIA.
2 SURENDRA PONRATHNAM NATIONAL CHEMICAL LABORATORY, PUNE-411008, MAHARASHTRA, INDIA.
3 CHELANATTU KHIZHAKKE MADATH RAMAN RAJAN NATIONAL CHEMICAL LABORATORY, PUNE-411008, MAHARASHTRA, INDIA.
4 ALAIN FRADET LABORATOIRE DE SYNTHESE MACROMOLECULAIRE, 4, PLACE JUSSIEU, 75252 PARIS CEDEX 05.
PCT International Classification Number C08L
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA