Abstract: This invention discloses a process of activated monomer ring opening mode of polymerization for producing a polymer/copolymer from a corresponding cyclic monomer such as lactide and lactones with an active catalyst selected from simple halides containing Group 8 metals along with mediating agents. The synthesized polymer/copolymer was analyzed and found to have high number average molecular weight (Mn) with desired physical properties.
1. A process of activated monomer ring opening mode of polymerization for producing a polymer from a corresponding cyclic monomer such as lactide and lactones with an active catalyst to achieve high number average molecular weight (Mn) polymer having desired physical properties, the process characterized in the selected catalyst being simple halldes containing Group 8 metals.
2. The process as claimed In Claim 1 further characterized in the catalyst used along with a mediating agent, which is water.
3. The process as claimed in Claim 1 further characterized in the catalyst used along with a mediating agent, which are nucleophlles such as alcohols.
4. The process as claimed in Claim 1 further characterized in the catalyst used along with mediating agents, which are water and nucleophlles.
5. The process as claimed in Claims 1 to 4, wherein the said selected metals are environmentally benign metals that are constituents in the mammalian anatomy thereby the catalyst residues are potentially harmless.
6. The process as claimed in Claims 1 to 4, wherein the monomer and the metal halide feed ratio is generally 200:1 molar ratio.
7. The process as claimed in Claims 1 to 4, wherein the metal halide catalyst selected is for use with lactone monomers such as e - caprolactone (CL), 6 -vaierolactone (VL) ,p - butyrolactone (BL) and lactide (LA).
8. The process as claimed in Claims 1 to 4, wherein theiatio of the monomer and the halide for CL polymers is 0.5 mL of CL (0.54 g, 4.71 mmol) and 23.6 pmol of metal halide.
9. The process as claimed in Claims 1 to 4, wherein the ratio of the monomer and the halide for VL polymers is 0.25 mL of VL (0.27 g, 2.69 mmol) and 13.5 pmoi of metal halide.
10. The process as claimed in Claims 1 to 4, wherein the ratio of the monomer and the halide for BL polymers is 0.25 mL of BL (0.26 g, 3.06 mmol) and 15.3 pmol of metal halide.
11. The process as claimed in Claims 1 to 4, wherein the molecular weight Mn is further varied by varying the feed ratio of the monomer and the mediating agents.
12. The process as claimed in Claims 1 to 4, wherein polymerization of BL Is faster than the polymerization of VL and the polymerization of VL Is faster than polymerization of CL.
13. The process as claimed in Claims 1 to 4, wherein the process of polymerization comprises of: a. introducing a selected metal halide catalyst Into an enclosed nitrogen atmosphere; b. adding a selected monomer into the enclosure under mixture stirring condition at a given temperature thereby achieving a rise in viscosity of the mixture; c. observing the reduction of monomer until its disappearance; d. quenching by pouring the contents into cold heptane; e. isolating the polymer by filtration; f. drying the filtered polymer; and g. collecting polymer of a constant weight.
14. The process as claimed in Claim 13, wherein the observation of polymerization is done using TLC technique through the disappearance of the monomer.
15. The process as claimed in Claim 13, wherein the catalyst is a metal halide per se.
16. The process as claimed in Claim 13, wherein the catalyst is a metal halide with predetermined amount of nucleophiles such as alcohol.
17. The process as claimed in Claim 13, wherein the catalyst is a metal halide with predetermined amount of nucleophiles such as alcohols and also a predetermined amount of dry toluene'
18. The process as claimed in Claim 13, wherein FeCia is selected as a catalyst comprising of additional steps of performing of ste|a>(a)and (b) below prior to step (a) of claim 13 and performing step (c) below alongwith step (b) of claim 13 wherein the steps (a), (b) and (c) is as follows : a. selecting anhydrous FeCIa; b. contaminating the anhydrous FeCia with a known stoichiometric of water to form metal halide catalyst; and c. polymerizing a selected monomer with the catalyst under rapid stirring at a given temperature, characterized in the selection of the catalyst and the ratio of the monomer and metal halide catalyst.
19. A process of activated monomer ring opening mode of polymerization for producing a copolymer from corresponding plurality of cyclic monomers such as lactide and lactones with an active catalyst to achieve high number average molecular weight (Mn) polymers having desired physical properties, the process characterized in the selected catalyst being simple halides containing Group 8 metals.
20. The process as claimed in Claim 19 further characterized in the catalyst used along with a mediating agent, which is water.
21. The process as claimed in Claim 19 further characterized in the catalyst used along with a mediating agent, which are nucieophrle& such as alcohols.
22. The process as claimed in Claim 19 further characterized in the catalyst used along with mediating agents, which are water and nucleophiles.
23. The process as claimed in Claims 19 to 22, wherein the said metals are environmentally benign metals that are constituents in the mammalian anatomy thereby the catalyst residues are potentially harmless.
24. The process as claimed in Claims 19 to 22, wherein the mixture of monomers and the metal halide feed ratio selected may be 200:1,100:1, or 50:1 molar ratio.
25. The process as claimed in Claims 19 to 22, wherein the metal halide catalyst selected is for a mixture of some or all of lactone monomers such as £ -caprolactone (CL), 5 - valerolactone (VL) ,p - butyrolactone (BL) and lactide (LA).
26. The process as claimed in Claims 19 to 22, wherein the molecular weight IVIn is varied by varying the feed ratio of the mixture of monomers and the mediating agents.
27. The process as claimed in Claims 19 to 22, wherein the process of polymerization comprises of: a. introducing a selected metal halide catalyst into an enclosed nitrogen atmosphere; b. adding a selected plurality of said monomers into the enclosure under mixture stirring condition at a given temperature thereby achieving a rise in viscosity of the mixture; c. observing the reduction of monomers until their disappearance; d. quenching by pouring the contents into cold heptane; e. isolating the copolymer by filtration; f. drying the filtered copolymer; and * g. collecting copolymer of a constant weight.
28. The process as claimed in Claim 28, wherein the observation of polymerization is done using TLC technique through the disappearance of the monomers.
29. The process as claimed in Claim 28, wherein the catalyst is metal halide per se.
30. The process as claimed in Claim 28, wherein the catalyst is metal halide with predetermined amount of nucleophiles such as alcohol.
31. The process as claimed in Claim 28, wherein the catalyst is metal halide with predetermined amount of nucleophiles such as alcohol and also a predetermined amount of dry toluene.
32. The process as claimed In Claims 28, wherein FeCIs is selected as a catalyst comprising of additional steps of performing of step (a) and (b) below prior to step (a) of claim 28 and performing step (c) below alongwith step (b) of claim 28 wherein the steps (a), (b) and (c) is as follows : a. selecting anhydrous FeCis; b. contaminating the anhydrous FeCis with a known stoichiometric of water to form metal halide catalyst; and c. polymerizing a mixture of selected monomers with the catalyst under rapid stirring at a given temperature, characterized in the selection of the catalyst and the ratio of the mixture of monomers and metal halide catalyst.
| # | Name | Date |
|---|---|---|
| 1 | 3099-che-2009 power of attorney 15-12-2009.pdf | 2009-12-15 |
| 1 | 3099-CHE-2009-EDUCATIONAL INSTITUTION(S) [16-10-2023(online)].pdf | 2023-10-16 |
| 2 | 3099-che-2009 form-5 15-12-2009.pdf | 2009-12-15 |
| 2 | 3099-CHE-2009-RELEVANT DOCUMENTS [25-09-2023(online)].pdf | 2023-09-25 |
| 3 | 3099-CHE-2009-EDUCATIONAL INSTITUTION(S) [28-11-2022(online)].pdf | 2022-11-28 |
| 3 | 3099-che-2009 form-3 15-12-2009.pdf | 2009-12-15 |
| 4 | 3099-CHE-2009-RELEVANT DOCUMENTS [28-09-2022(online)].pdf | 2022-09-28 |
| 4 | 3099-che-2009 form-2 15-12-2009.pdf | 2009-12-15 |
| 5 | 3099-CHE-2009-EDUCATIONAL INSTITUTION(S) [10-12-2021(online)].pdf | 2021-12-10 |
| 5 | 3099-che-2009 form-1 15-12-2009.pdf | 2009-12-15 |
| 6 | 3099-CHE-2009-OTHERS [10-12-2021(online)].pdf | 2021-12-10 |
| 6 | 3099-che-2009 drawings 15-12-2009.pdf | 2009-12-15 |
| 7 | 3099-CHE-2009-RELEVANT DOCUMENTS [30-09-2021(online)].pdf | 2021-09-30 |
| 7 | 3099-che-2009 description (complete) 15-12-2009.pdf | 2009-12-15 |
| 8 | 3099-CHE-2009-RELEVANT DOCUMENTS [20-03-2020(online)].pdf | 2020-03-20 |
| 8 | 3099-che-2009 correspondence-others 15-12-2009.pdf | 2009-12-15 |
| 9 | 3099-che-2009 claims 15-12-2009.pdf | 2009-12-15 |
| 9 | 3099-CHE-2009-RELEVANT DOCUMENTS [04-04-2019(online)].pdf | 2019-04-04 |
| 10 | 3099-che-2009 abstract 15-12-2009.pdf | 2009-12-15 |
| 10 | Form27_Licence_01-04-2019.pdf | 2019-04-01 |
| 11 | 3099-CHE-2009 FORM-18 21-01-2010.pdf | 2010-01-21 |
| 11 | Correspondence by Applicant_Renewal Fees_25-10-2018.pdf | 2018-10-25 |
| 12 | 3099-CHE-2009 EXAMINATION REPORT REPLY RECIEVED 23-09-2014.pdf | 2014-09-23 |
| 12 | Form27_Licence_28-03-2018.pdf | 2018-03-28 |
| 13 | 3099-CHE-2009 AMENDED PAGES OF SPECIFICATION 23-09-2014.pdf | 2014-09-23 |
| 13 | correspondence by applicant_Renewal_15-12-2017.pdf | 2017-12-15 |
| 14 | 3099-CHE-2009 FORM-5 23-09-2014.pdf | 2014-09-23 |
| 14 | Form 27_License_31-03-2017.pdf | 2017-03-31 |
| 15 | 3099-CHE-2009 FORM-3 23-09-2014.pdf | 2014-09-23 |
| 15 | Correspondence by Applicant_Renewal_08-12-2016.pdf | 2016-12-08 |
| 16 | 3099-CHE-2009 AMENDED CLAIMS 23-09-2014.pdf | 2014-09-23 |
| 17 | Correspondence by Applicant_Renewal_08-12-2016.pdf | 2016-12-08 |
| 17 | 3099-CHE-2009 FORM-3 23-09-2014.pdf | 2014-09-23 |
| 18 | Form 27_License_31-03-2017.pdf | 2017-03-31 |
| 18 | 3099-CHE-2009 FORM-5 23-09-2014.pdf | 2014-09-23 |
| 19 | 3099-CHE-2009 AMENDED PAGES OF SPECIFICATION 23-09-2014.pdf | 2014-09-23 |
| 19 | correspondence by applicant_Renewal_15-12-2017.pdf | 2017-12-15 |
| 20 | 3099-CHE-2009 EXAMINATION REPORT REPLY RECIEVED 23-09-2014.pdf | 2014-09-23 |
| 20 | Form27_Licence_28-03-2018.pdf | 2018-03-28 |
| 21 | 3099-CHE-2009 FORM-18 21-01-2010.pdf | 2010-01-21 |
| 21 | Correspondence by Applicant_Renewal Fees_25-10-2018.pdf | 2018-10-25 |
| 22 | 3099-che-2009 abstract 15-12-2009.pdf | 2009-12-15 |
| 22 | Form27_Licence_01-04-2019.pdf | 2019-04-01 |
| 23 | 3099-che-2009 claims 15-12-2009.pdf | 2009-12-15 |
| 23 | 3099-CHE-2009-RELEVANT DOCUMENTS [04-04-2019(online)].pdf | 2019-04-04 |
| 24 | 3099-CHE-2009-RELEVANT DOCUMENTS [20-03-2020(online)].pdf | 2020-03-20 |
| 24 | 3099-che-2009 correspondence-others 15-12-2009.pdf | 2009-12-15 |
| 25 | 3099-CHE-2009-RELEVANT DOCUMENTS [30-09-2021(online)].pdf | 2021-09-30 |
| 25 | 3099-che-2009 description (complete) 15-12-2009.pdf | 2009-12-15 |
| 26 | 3099-CHE-2009-OTHERS [10-12-2021(online)].pdf | 2021-12-10 |
| 26 | 3099-che-2009 drawings 15-12-2009.pdf | 2009-12-15 |
| 27 | 3099-CHE-2009-EDUCATIONAL INSTITUTION(S) [10-12-2021(online)].pdf | 2021-12-10 |
| 27 | 3099-che-2009 form-1 15-12-2009.pdf | 2009-12-15 |
| 28 | 3099-CHE-2009-RELEVANT DOCUMENTS [28-09-2022(online)].pdf | 2022-09-28 |
| 28 | 3099-che-2009 form-2 15-12-2009.pdf | 2009-12-15 |
| 29 | 3099-CHE-2009-EDUCATIONAL INSTITUTION(S) [28-11-2022(online)].pdf | 2022-11-28 |
| 29 | 3099-che-2009 form-3 15-12-2009.pdf | 2009-12-15 |
| 30 | 3099-CHE-2009-RELEVANT DOCUMENTS [25-09-2023(online)].pdf | 2023-09-25 |
| 30 | 3099-che-2009 form-5 15-12-2009.pdf | 2009-12-15 |
| 31 | 3099-che-2009 power of attorney 15-12-2009.pdf | 2009-12-15 |
| 31 | 3099-CHE-2009-EDUCATIONAL INSTITUTION(S) [16-10-2023(online)].pdf | 2023-10-16 |
| 32 | 3099-CHE-2009-EDUCATIONAL INSTITUTION(S) [11-12-2024(online)].pdf | 2024-12-11 |