Morphology modified heterophase propylene copolymers and their products thereof

Abstract

The present invention provides a morphology modified heterophase polymer having No-Break impact strength in the range of 500 J/m-700 J/m as per ASTM standard D256, a high melt flow index in the range of 100 g/10 min as per ASTM D1238, and a balanced flexural modulus as per ASTM standard D790. More particularly, the present invention relates to a process for the modification of morphology of heterophase propylene polymer in the presence of an initiator in the form of organic peroxide and a multifunctional unsaturated organic vinyl compound on the ex-reactor Heterophase Propylene Copolymer powder and/or pellet using special extrusion device.

Claims

1. A process for preparing a morphology modified heterophase polymer, the process comprising: (i) mixing a multifunctional additive and a peroxide, and adding an organic solvent to obtain a morphology modifier composition and mixing the morphology modifier composition with a heterophase polymer to obtain a a final mixture, wherein the organic solvent is added in an amount of 0.5 to 60 ml per kg of morphology modified heterophase polymer; and (ii) extruding the final mixture to obtain the morphology modified heterophase polymer.

2. The process as claimed in claim 1, wherein the final mixture is extruded in a twin screw extruder at a temperature in a range of 160-300° C.

3. The process as claimed in claim 1, wherein the multifunctional additive is an unsaturated organic vinyl compound and selected from the group consisting of pentaerythritol triacrylate, pentaerythritol tetraacrylate, and butanediol diacrylate.

4. The process as claimed in claim 1, wherein the multifunctional additive is added in an amount of 1000 to 7500 ppm of the morphology modified heterophase polymer.

5. The process as claimed in claim 1, wherein the peroxide is selected from the group consisting of an alkyl peroxide and a peroxy ester.

6. The process as claimed in claim 1, wherein the peroxide is added in an amount of 25 to 2000 ppm of the morphology modified heterophase polymer.

7. The process as claimed in claim 1, wherein the organic solvent is selected from the group consisting of acetone, dichloromethane (DCM), paraffin oil, and ethanol.

8. The process as claimed in claim 1, wherein the mixing the multifunctional additive and the peroxide is carried out at a temperature in a range of 10 to 35° C. or at a temperature below a boiling point of the organic solvent, peroxide, or multifunctional additive.

9. The process as claimed in claim 1, wherein the mixing the multifunctional additive and the peroxide is carried out for a time in a range of 2 minutes to 30 minutes.

10. The process as claimed in claim 1, wherein the step (i) further comprises adding an antioxidant, an acid scavenger, and a nucleating agent additive package.

11. The process as claimed in claim 1, wherein the heterophase polymer has two different phases: a first phase that is a propylene phase polymer; and a second phase that is an ethylene phase polymer; wherein the propylene phase polymer comprises homo polypropylene, a copolymer of propylene and ethylene, and optionally C4-C10 alpha olefin, wherein propylene content in the propylene phase polymer is 90-95% by weight, and, wherein the ethylene phase polymer comprises homo polyethylene and co-polymers of ethylene and C3-C10 alpha olefins, wherein ethylene content in the ethylene phase polymer is in a range of 20 to 50% by weight.

Description

DETAILED DESCRIPTION OF THE INVENTION

(1) While the invention is susceptible to various modifications and alternative forms, specific embodiment thereof will be described in detail below. It should be understood, however that it is not intended to limit the invention to the particular forms disclosed, but on the contrary, the invention is to cover all modifications, equivalents, and alternative falling within the scope of the invention as defined by the appended claims.

(2) The following description is of exemplary embodiments only and is not intended to limit the scope, applicability or configuration of the invention in any way. Rather, the following description provides a convenient illustration for implementing exemplary embodiments of the invention. Various changes to the described embodiments may be made in the function and arrangement of the elements described without departing from the scope of the invention.

(3) The present invention intends to provide a novel and economical process for morphology modification of heterophase polypropylene copolymer using a multifunction additive and organic peroxide where the morphology modification involves enhancement of interaction of rubber phase of impact copolymer of polypropylene with the homo-polymer matrix of impact copolymer polypropylene which results in enhancement of impact properties of post reactor modified resin to several multiple folds along with increase in melt flow properties of the post reactor modified resin in multiple folds.

(4) The present invention is directed to morphology modification of heterophase copolymer of polypropylene which involves a novel and economical process of preparation of morphology modifier composition and post reactor extrusion process.

(5) Polymer:

(6) The heterophase polymer mentioned in the current invention has two different phase i.e., homo polypropylene and copolymers of ethylene and propylene which is manufactured in a two stage process, where polymerization of homo-polypropylene takes place in the first reactor and in second reactor ethylene propylene rubber polymerization takes place if required polymerization can take place in third rector as well. Catalyst used for this polymerization process can be Ziegler Natta or metallocene catalyst. The ethylene percent of ethylene propylene copolymer is in range from 10-80 wt %. The ethylene content in the final heterophase polymer is in the range of 8-20% and the Xylene content of the resulting polymer is in range of 10-25 wt % as per ASTM D5492. MFI range of heterogeneous polymer is from 3-12 g/10 min as per ASTM D1238. The flexural modulus of the heterophase polymer is in range of 700-130 MPA and impact properties defined by notched izod at room temperature measured is in range of 80-700 J/m as per ASTM standard D790 and D256 respectively. The heterophase polymer mentioned in current invention is used in ex reactor powder form or in granules form.

(7) Process:

(8) Process of the current invention involves two stages. Stage 1 includes preparation of morphology modifier composition and mixing of reactive modification additive/morphology modifier composition with heterophase polymer. Stage 2 involves reactive extrusion process where the final mixture obtained from stage 1 is extruded in a twin screw extruder in temperature range 150° C.-260° C.

(9) Stage-1

(10) Morphology Modifier Additive/Reactive Modifier Additive Mixture/Morphology Modifier Composition:

(11) Premixing of Multifunctional Additive and peroxide in an organic solvent (e.g., Acetone, DCM, paraffin oil, ethanol) of range 0-100 ml/kg or preferably in range of 5-40 ml/kg, or more preferably in range 5-20 ml/kg is carried out preferably at temperature between 10 to 35° C. or should not exceed boiling point of the organic solvent or peroxide or Multifunctional Additive. Premixing is carried out for 2 minutes or longer, preferably 5 minutes or longer, more preferably 10 mins or longer and in particular 30 minutes to 45 minutes or longer. The premixing is carried out at ambient pressure, either in presence of inert gas or in presence of air.

(12) The morphology modifier composition thus prepared is added to polyolefin's like heterophase polypropylene (Copolymer including random as well as block copolymers). The morphology modifier composition obtained by above method may be used in liquid form when adding to polyolefin's reactor powder or granules in batch mixer/high speed mixer or in liquid dosing system in twin screw extruder.

(13) Premixing of reactor powder of impact copolymer PP powder with PETA (pentaerythritol triacrylate) & Peroxide solution along with Antioxidant, Acid scavenger and Nucleating agent additive package is done in high speed mixer at room temperature and at ambient pressure with an average residence time of 5 minutes to 30 minutes or longer, more preferably 2 minutes or longer.

(14) Antioxidant (primary, secondary), Acid scavenger and Nucleating agent additive package are added along with Polypropylene reactor powder and reactive modifier additive mixer during mixing in high speed mixer at following ppm level (750, 750), 350p, 250 ppm respectively, Whereas Impact copolymer polypropylene granules contains this additive packages inherent which is added during extrusion stage of manufacturing process.

(15) The primary and secondary antioxidants used in this experiment is combination of tetrakis methylene[3,5-di-tert-butyl-4-hydroxyhydroconnamate]methane (Irganox 1010) & tris(2,4-di-tert.-butylphenyl)phosphate (Irganox 168). The nucleating agent used in this is HPN 20E, acid scavenger used in these experiment is Calcium stearate.

(16) Primary and secondary antioxidants are added in range of 250 ppm to 1%, preferably 250-5000 ppm and more preferably in range of 250-1500 ppm. Nucleating agent & acid scavenger is added in range of 250 ppm-2%, preferably 250-5000 ppm more preferably 250-1500 ppm.

(17) Stage 2—Reactive Extrusion Process:

(18) Premixed compound were then melt compounded in Twin screw extruder Labtech make of screw Diameter of 26 mm and Length/Diameter ratio 40:1 of and maximum screw rotating speed 800 rpm. Speed of the extruder is maintained at 100-200 rpm and barrel temperature range maintained at 100-250° C., feeding rate 8-20 Kg/hr. The extrudate of modified batches are pelletized after cooling in water bath to pellets of size 2-3 mm.

(19) The compound obtained in accordance with the present invention may be used in particular form, preferably as pellets when adding to final compounding process. Compound thus obtained may be used as fine powder.

(20) In one feature of the present invention the morphology modified heterophase polymer having an impact strength improved PP having No-Break impact strength and a very high melt flow index of 100 g/10 min(not limited to) having a balanced flexural modulus is developed by modifying a PP produced using conventional Ziegler Natta Catalyst and process where impact strength is limited to 100 J/m, MFi of 10 g/min and moderated Flexural modulus. The modification improves both melt flow index and impact strength simultaneously. The modification can be done on conventional extruder used in polymer industry with the addition of multi functional compounds in the presence of activators like peroxides and reaction stabilizers like diluents. The above said morphology modified heterophase polymer also is FDA and REACH regulation passed samples.

(21) In another feature of the present invention, the heterophase polyolefin polymer consist of two different phase first being a propylene phase polymer made of homo and copolymer of propylene and ethylene and/or C4-C10 alpha olefins where ethylene concentration can be maximum upto 50%. The second phase being an ethylene phase polymer made of homo and co polymers of ethylene and C3-C10 alpha olefins.

(22) The ethylene polymer phase may be only made of ethylene or copolymer of ethylene and C3-C10 alpha olefins based on which the ethylene content may vary from 8 to 90% by weight.

(23) Here either ethylene or propylene phase constitutes the continuous and discrete phase of the heterogeneous polymer system. The concentration of ethylene and propylene phase may vary widely dependant on the discrete or dispersion phase concentration.

(24) The propylene content of propylene phase polymer may be 80% or higher and ethylene content in the heterophase composition may be in range of 5 to 75% by weight. Similarly the ethylene polymer phase can be made of ethylene propylene copolymer or ethylene octane based elastomer.

(25) The following non-limiting examples illustrate in details about the invention. However, they are, not intended to be limiting the scope of present invention in any way.

EXAMPLES

(26) Polymer:

(27) PP1A is a reactor powder/heterophase polymer of copolymer of propylene and ethylene having a MFR2 (230° C.) of 9-11 g/10 min, Ethylene content of 14-15%, Xylene soluble of 21-23 wt %, Flexural modulus of 800-1000 MPa, Notched izod Impact strength of >500 J/m.

(28) PP1B is an extruded granule of copolymer of propylene and ethylene having a MFR2 (230° C.) of 9-11 g/10 min, Ethylene content of 14-15%, Xylene soluble of 21-23 wt %, Flexural modulus of 800-1000 MPa, Notched izod Impact strength of >500 J/m.

(29) PP2A is a reactor powder of copolymer of propylene and ethylene having a MFR2 (230° C.) of 7-9 g/10 min, Ethylene content of 8.5-10.5%, Xylene soluble of 18-20 wt %, Flexural modulus of 1000 MPa-1200 MPa, Notched izod Impact strength of 100-200 J/m.

(30) PP2B is an extruded granule of copolymer of propylene and ethylene having a MFR2 (230° C.) of 7-9 g/10 min, Ethylene content of 8.5-10.5%, Xylene soluble of 18-20 wt %, Flexural modulus of 1000 MPa-1200 MPa, Notched izod Impact strength of 100-200 J/m.

(31) PP3A is a reactor powder of copolymer of propylene and ethylene having a MFR2 (230° C.) of 9-12 g/10 min, Ethylene content of 8-10%, Xylene soluble of 16.5-19.5 wt %, Flexural modulus of 1000 MPa-1200 Mpa, Notched izod Impact strength of 100-200 J/m.

(32) PP3B is an extruded granule of copolymer of propylene and ethylene having a MFR2(230° C.) of 9-12 g/10 min, Ethylene content of 8-10%, Xylene soluble of 16.5-19.5 wt %, Flexural modulus of 1000 MPa-1200 Mpa, Notched izod Impact strength of 100-200 J/m.

(33) PP4 is a reactor powder of copolymer of propylene and ethylene having a MFR2(230° C.) of 3-4 g/10 min, Ethylene content of 9-10%, Xylene soluble of 15.5-18.5 wt %, Flexural modulus of 1000 MPa-1200 Mpa, Impact strength of >150 J/m.

(34) Chemical Details:

(35) The details of chemical used in the examples are as followings: Peroxide 1—Luperox 101 (2,5-dimethyl-2,5-di(tert-butylperoxy)hexane) Mw—290 g/mol, 0.877 g/ml and assay 90%. Peroxide 2—Triganox 301 (3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxonane) MFC1—PETA (Penta Erythritol Tri Acrylate) used has Mw of 298.29 g/mol, 1.18 g/ml @25° C. and contains 300-400 ppm monomethyl ether hydroquinone as inhibitor. MFC 2—PETeA (Penta Erythritol Tetra Acrylate) Solvent 1—Acetone used is of purity 990% and weight per ml at 20° C. is 0.79-0.792 g the maximum limits of impurities of non volatile matter is 0.002%, Acidity 0.015% & water 0.4%. Solvent 2—DCM (Dichloromethane) Solvent 3—LP(liquid paraffin light) used has viscosity at 25° C. 25-80 mPas, weight per ml at 25° C. 0.82-0.88 g, and max impurity of water is 0.05%
Experimental Details:

(36) The pelletized compound of reactive extrusion process is used to prepare samples for mechanical testing as per ASTM standards by injection moudling machine of L&T plastics machinery of 40 mm screw diameter, L:D ratio 20:1 and 60 tonnage locking force. The barrel temperature was maintained at 150° C.-300° C. and mould temperature was maintained at 60° C. The resulted injection molded samples were used for tensile, flexural and impact strength measurements as per ASTM standards.

(37) Melt flow rate of the compounded sample was determined according to ASTM D1238 at 230° C., 2.16 Kg load in Automatic multiload MFI machine of Gottfret make.

(38) Flexural modulus was determined as per ASTM D790 in universal testing machine of TIRA Germany make after being conditioned as per ASTM D618 standard.

(39) Notched Izod Impact strength of bars which measured as per ASTM D256 was measured at 23° C. after being conditioned as per ASTM D618 standard.

(40) Yellowness Index is a number calculated from spectrophotometric data that describes the change in color of a test sample from clear or white to yellow. This test is most commonly used to evaluate color changes in a material caused by real or simulated outdoor exposure. Yellowness index of extruded granules was determined as per ASTM E 313-10 was measured at 23° C. in—Labscan XE of Hunterlab.

Example 1

(41) The following example illustrates the reactive modification of Impact copolymer polypropylene reactor powder (PP3A) using various reactive morphology modifier composition and properties enhanced according to method of present invention.

(42) TABLE-US-00001 TABLE 1 shows the various mixtures used for reactive extrusion in PP3. Peroxide1 MFC1 MFC2 Solvent 1 S. NO ppm ppm ppm ml/kg EXP1 NIL NIL NIL 45 EXP2 25 5000 — 45 EXP3 50 5000 45 EXP4 25 5000 — 45 EXP5 50 5000 — 45 EXP6 25 7500 — 45 EXP7 50 7500 — 45 EXP8 25 — 2500 45 EXP9 50 — 2500 45 EXP10 100 — 2500 45 EXP11 25 — 5000 45 EXP12 50 — 5000 45 EXP13 100 — 5000 45 EXP14 25 — 7500 45 EXP15 50 — 7500 45 EXP16 100 — 7500 45 EXP17 — — — 45 EXP18 100 — — 45 EXP19 150 — — 45 EXP20 100 1000 — 45 EXP21 100 1500 — 45 EXP22 100 2000 — 45 EXP23 100 2500 — 45 EXP24 150 1500 — 45 EXP25 150 2500 — 45 EXP26 175 2500 — 45 EXP27 180 1500 — 45 EXP28 200 2500 — 45 EXP29 200 5000 — 45 EXP36 500 7500 — 45 EXP37 600 15000  — 45

(43) The test samples of all the above mentioned formulations were prepared and physical properties of the samples were tested according to ASTM Standards as mentioned above. Examples 1 and 17, both are neat Polypropylene material from plant but from different production lot.

(44) Table below illustrates the Melt Flow index at 230° C., 2.16 Kg load (g/10 mins), Impact strength in J/m as per ASTM D256 and Flexural modulus in MPa as per ASTM D 790 of modified batches in polypropylene PP3A.

(45) TABLE-US-00002 MFI @230° C. Flexural Modulus Impact Strength S. NO g/10 min (N/mm.sup.2) J/m EXP1 11.4 1207 115 EXP2 8.7 1163 513 EXP3 11.2 1128 508 EXP4 6 995 522 EXP5 11.4 947 523 EXP6 8.3 1068 536 EXP7 10.4 1050 522 EXP8 9.7 967 531 EXP9 12.9 973 511 EXP10 15.8 1007 519 EXP11 8.7 1035 558 EXP12 10.9 1037 516 EXP13 13.2 1012 510 EXP14 7.5 1060 536 EXP15 9.5 1018 518 EXP16 11 971 527 EXP17 11.4 892 194 EXP18 20 878 91 EXP19 22.9 888 96 EXP20 16.4 839 538 EXP21 16 875 540 EXP22 14.6 891 537 EXP23 15.3 922 530 EXP24 18.4 813 519 EXP25 17.4 902 515 EXP26 20 833 514 EXP27 15.9 1065 517 EXP28 22.3 869 517 EXP29 19.4 927 482 EXP36 31 — 176 EXP37 29.3 — 216

(46) PP3A reactor powder of MFI 11 g/10 min and impact strength around 115 J/m (EXP 1) is used for above experiments. EXP 1 is a comparative example where no peroxide and MFC is added and processed in TSE in similar process condition mentioned in reactive extrusion process.

(47) Exp 2-16 with lower peroxide concentration i.e., 25-100 ppm in combination with MFC of higher concentration range 2500-7500 ppm yielded higher Impact strength>500 J/m but maintained MFI in range of 8-15 g/10 min, i.e., flow properties are not altered.

(48) But in EXP20-29 peroxide concentration in range of 100-200 ppm in combination with MFC's of range 1000-5000 ppm yielded higher MFI of range 16-22 and impact strength is >500 J/m maintaining flexural modulus in range of 800-1060 MPa.

Example 2

(49) The following example illustrates the reactive modification of Impact copolymer polypropylene extruded granules (PP3B) using various reactive morphology modifier composition and properties enhanced according to method of present invention.

(50) TABLE-US-00003 Peroxide 1 MFC1 MFC2 Solvent 1 Solvent 3 S. NO ppm ppm ppm ml/kg ml/kg EXP38 — — — 45 — EXP39  50 5000 — 45 — EXP40 200 7500 — 45 — EXP41 200 7500 — 45 — EXP76 250 3000 — — 15 EXP77 200 2000 — — 15 EXP78 250 2500 — — 15

(51) The test samples of all the above mentioned formulations were prepared and physical properties of the samples were tested according to ASTM Standards as mentioned above.

(52) Table below illustrates the Melt Flow index at 230° C., 2.16 Kg load (g/10 mins), Impact strength in J/m as per ASTM D256 and Flexural modulus in MPa as per ASTM D 790 of modified batches in polypropylene PP3B.

(53) TABLE-US-00004 MFI @230° C. Flexural Modulus Impact Strength S. NO g/10 min (N/mm.sup.2) J/m EXP38 11.0 1200 98 EXP39 6.7 — 479 EXP40 15.2 — 543 EXP41 15.6 — 557 EXP76 20 840 608 EXP77 19 840 630 EXP78 20 837 617

(54) PP3B extruded granule material of MFI 11 g/10 min and impact strength 100 J/m (EXP 38). EXP 38 is a comparative example where no peroxide and MFC is added and processed in TSE in similar process condition mentioned in reactive extrusion process.

(55) Morphology modification is carried out in PP3B (used in EXP 38) with addition of peroxide of range 100-200 ppm and MFC of range 2500-7500 ppm (See EXP 40-41, 76-78.) resulted in MFI of range 18-20 g/10 min and impact strength>500 J/m, i.e., No break.

(56) However in EXP 39 with lower peroxide (i.e., 50 ppm) and MFC of concentration 5000 ppm it yielded no break (i.e., impact strength>500 J/m) & resulted in drop of MFI (i.e., 6.7 g/10 min).

Example 3

(57) The following example illustrates the reactive modification of Impact copolymer polypropylene reactor powder (PP2A) using various reactive morphology modifier composition and properties enhanced according to method of present invention.

(58) TABLE-US-00005 Peroxide 1 Peroxide 2 MFC 1 Solvent 1 S. NO ppm ppm ppm ml/kg EXP 42 — — — — EXP 43 200 — — 45 EXP 44 — 250 — 45 EXP 45 200 — — 60 EXP 46 — 250 — 60 EXP 47 250 — 2500 60 EXP 48 275 — 2500 60 EXP 49 300 — 2500 60 EXP 50 350 — 2500 60 EXP 51 300 — 2500 60 EXP 52 450 — 0 60 EXP 53 700 — 5000 60

(59) The test samples of all the above mentioned formulations were prepared and physical properties of the samples were tested according to ASTM Standards as mentioned above. EXP 42 is virgin polypropylene material. That is no additives added. Extruded in TSE and kept as reference.—i.e., it is PP2A material.

(60) Table below illustrates the Melt Flow index at 230° C., 2.16 Kg load (g/10 mins), Impact strength in J/m as per ASTM D256 and Flexural modulus in MPa as per ASTM D 790 of modified batches in polypropylene PP2A.

(61) TABLE-US-00006 MFI @230° C. Flexural Modulus Impact Strength S. NO g/10 min (N/mm2) J/m EXP 42 7.5 1187 381 EXP 43 17.5 1095 165 EXP 44 17.9 — 174 EXP 45 17.0 1067 172 EXP 46 18.5 — 168 EXP 47 16.7 1061 529 EXP 48 16.6 — 637 EXP 49 18.7  889 628 EXP 50 21.4  849 606 EXP 51 16.8  882 644 EXP 52 29.6 — — EXP 53 33.6 — —

(62) PP2A reactor powder (EXP 42) of MFI 8 g/10 min and impact strength of 300 J/m. EXP 42 is a comparative example where no peroxide and MFC is added and processed in TSE in similar process condition mentioned in reactive extrusion process.

(63) PP2A reactor powder (used in EXP 42) of MFI 8 g/10 min and impact strength of 300 J/m resulted in MFI of range 15-22 MFI when morphology modified using peroxide of range 200-500 ppm in combination with MFC's of lower concentration 2500 ppm (EXP 43-51).

Example 4

(64) The following example illustrates the reactive modification of Impact copolymer polypropylene granule (PP2B) using various reactive morphology modifier composition and properties enhanced according to method of present invention.

(65) TABLE-US-00007 Peroxide 1 MFC 1 Solvent 1 Solvent 2 Solvent 3 S. No Ppm Ppm ml/kg ml/kg ml/kg EXP 54 — — — — — EXP 55 300 2500 0 60 — EXP56 300 3000 0 60 — EXP79 300 3000 30  — — EXP80 300 3000 — — 15 EXP81 250 2500 — — 15 EXP82 500 3000 — — 15 EXP83 800 2500 — — 15 EXP84 1500  2000 — — 15

(66) The test samples of all the above mentioned formulations were prepared and physical properties of the samples were tested according to ASTM Standards as mentioned above.

(67) Table below illustrates the Melt Flow index at 230° C., 2.16 Kg load (g/10 mins), Impact strength in J/m as per ASTM D256 and Flexural modulus in MPa as per ASTM D 790 of modified batches in polypropylene PP2B.

(68) TABLE-US-00008 MFI @230° C. Flexural Modulus Impact Strength S. NO g/10 min (N/mm2) J/m EXP 54 9 1110 150 EXP 55 22.5 910 581 EXP56 21.2 820 475 EXP79 18.8 962 627 EXP80 23.2 804 642 EXP81 18.5 863 573 EXP82 27 751 640 EXP83 39 778 643 EXP84 61 630 583

(69) PP2B granules of properties MFI 9 g/10 min and impact strength of 150 J/m (EXP 54) is used for above experiments. EXP 54 is a comparative example where no peroxide and MFC is added and processed in TSE in similar process condition mentioned in reactive extrusion process.

(70) EXP (55-56, 79-81) performed with peroxide in range of 250-300 ppm and MFC in range of 2500-3000 ppm resulted in extruded granules with MFI of range 18-22 g/10 min & impact strength>500 J/m i.e., No break.

(71) EXP (82-84) performed with peroxide in range of 500-1500 ppm and MFC in range of 2000-3000 ppm resulted in extruded granules with MFI of range 27-60 g/10 min & impact strength>500 J/m i.e., No break.

Example 5

(72) The following example illustrates the reactive modification of Impact copolymer polypropylene reactor powder (PP1A) using various reactive morphology modifier composition and properties enhanced according to method of present invention.

(73) TABLE-US-00009 Peroxide 1 MFC 1 Solvent 1 Solvent 2 S. No. Ppm Ppm ml/kg ml/kg EXP 57 — — — — EXP58 1000 7500 45 — EXP 59 1200 9000 45 — EXP 60 750 — 45 — EXP 61 1000 — 45 — EXP 62 1600 12000 45 — EXP 63 1600 15000 45 — EXP 64 1600 20000 45 — EXP 65 350 2500 60 — EXP 66 350 2500 — 60

(74) The test samples of all the above mentioned formulations were prepared and physical properties of the samples were tested according to ASTM Standards as mentioned above.

(75) Table below illustrates the Melt Flow index at 230° C., 2.16 Kg load (g/10 mins), Impact strength in J/m as per ASTM D256 and Flexural modulus in MPa as per ASTM D 790 of modified batches in polypropylene PP1A.

(76) TABLE-US-00010 MFI @230° C. Flexural Modulus Impact Strength S. NO g/10 min (N/mm2) J/m EXP 57 11.5 — 630 EXP58 47.6 — 139 EXP 59 53.7 — — EXP 60 50.3 — — EXP 61 69.3 — 110 EXP 62 75.7 — 140 EXP 63 67.8 — 120 EXP 64 64 — 108 EXP 65 26.2 832 558 EXP 66 29.0 723 602

(77) PP1A material (EXP57) has MFI 11.5 g/10 min & impact strength 630 J/m (No break) grade. EXP 57 is a comparative example where no peroxide and MFC is added and processed in TSE in similar process condition mentioned in reactive extrusion process.

(78) EXP 65 & 66 were performed in PP1A material with peroxide of concentration 350 ppm and MFC of concentration 2500 ppm and resulted in MFI of 25-30 g/10 min & no break.

(79) In EXP (59-64) resulted in higher MFI but yield lower impact strength in a range of 100-150 J/m.

Example 6

(80) The following example illustrates the reactive modification of Impact copolymer polypropylene extruded granules (PP1B) using various reactive morphology modifier composition and properties enhanced according to method of present invention.

(81) TABLE-US-00011 Peroxide 1 MFC 1 Solvent 1 Solvent 2 S. No ppm ppm ml/kg ml/kg Solvent 3 EXP 67 350 2500 — 60 — EXP 68 350 2500 60 — — EXP 69 300 2500 — 60 — EXP 70 400 3000 — 60 — EXP 71 450 3000 — 60 — EXP 72 450 2000 — 60 — EXP 73 500 2500 — 60 — EXP 74 700 2000 — 60 — EXP 75 800 2000 — 60 — EXP85 500 2500 — — 15 EXP86 800 2000 — — 15 EXP87 500 3000 — — 10 EXP88 500 3000 — — 5 EXP89 500 3000 — — 0 EXP90 500 2500 — — 5 EXP91 500 2500 — — 10 EXP92 500 2500 — — 15 EXP93 1500 1000 — — 15 EXP94 2000 1000 — — 15 EXP95 1500 800 — — 15 EXP96 2000 1250 — — 15 EXP97 2000 1500 — — 15

(82) The test samples of all the above mentioned formulations were prepared and physical properties of the samples were tested according to ASTM Standards as mentioned above.

(83) Table below illustrates the Melt Flow index at 230° C., 2.16 Kg load (g/10 mins), Impact strength in J/m as per ASTM D256 and Flexural modulus in MPa as per ASTM D 790 of modified batches in polypropylene PP1B.

(84) TABLE-US-00012 MFI Flexural Impact @230° C. Modulus Strength Yellowness S. No g/10 min (N/mm.sup.2) J/m Index EXP 67 23.3 808 615 — EXP 68 27.4 770 632 — EXP 69 22.5 768 631 — EXP 70 25 771 582 — EXP 71 27.7 795 533 — EXP 72 27.4 971 568 — EXP 73 29.8 849 617 — EXP 74 31.1 802 587 <2 EXP 75 41.25 808 589 <2 EXP85 30 633 563 — EXP86 43 617 583 — EXP87 28 622 693 — EXP88 30 678 601 — EXP89 26 709 604 — EXP90 23 667 673 — EXP91 26 629 652 — EXP92 28 598 642 — EXP93 68 600 648 — EXP94 62 583 659 — EXP95 67 620 671 — EXP96 100 606 597 — EXP97 102 598 623 —

(85) EXP 90-92 was performed to understand effect of solvent quantity in final properties such as MFI & Impact strength. In these three examples (EXP 90-92) peroxide and MFC where used at 500 & 2500 ppm respectively. Solvents were used in range of 5, 10, 15 ml/kg (EXP 90, 91, 92 respectively). It is observed that with increase in solvent quantity the MFI is increasing and effect on impact properties is marginal. This depicts the premixed compound mixing properties enhances with increase in solvent quantity. EXP 87-89 was also performed to understand effect of solvent on final properties. The correlation exist same in this experiments where peroxide and MFC used at 500, 3000 ppm respectively. In this also it was observed that with increase in solvent quantity the MFI is increasing and effect on impact properties is marginal.

(86) EXP 93-97 were performed with higher concentration of peroxide (1500-2000) ppm and MFC's of concentration 800-1500 ppm it resulted in very high flow material of 100 g/10 min & impact strength>500 J/m, i.e. no break.

(87) EXP 67-75, 85-86 were performed with peroxide concentration of 350-800 ppm and MFC's of range 2000-2500 ppm.

Advantages of the Present Invention

(88) The following are the technical advantages of the present invention over the prior art as disclosed above: Achieving high impact and high flow from existing Impact copolymer polypropylene (ICP) produced with conventional technology. Melt Flow Index (MFI) and impact strength can be increased simultaneously without much affecting the flexural modulus. Economically viable alternate solution to produce Thermoplastic olefins (TPO) from PP produced by conventional process.