GB2604463A - Low molecular weight polytetrafluoroethylene micropowder and process for preparing the same - Google Patents
Low molecular weight polytetrafluoroethylene micropowder and process for preparing the same Download PDFInfo
- Publication number
- GB2604463A GB2604463A GB2205473.8A GB202205473A GB2604463A GB 2604463 A GB2604463 A GB 2604463A GB 202205473 A GB202205473 A GB 202205473A GB 2604463 A GB2604463 A GB 2604463A
- Authority
- GB
- United Kingdom
- Prior art keywords
- ptfe
- micropowder
- molecular weight
- low molecular
- weight polytetrafluoroethylene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract 28
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract 28
- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract 10
- 238000004519 manufacturing process Methods 0.000 title claims abstract 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract 7
- 239000002245 particle Substances 0.000 claims abstract 6
- 230000000379 polymerizing effect Effects 0.000 claims abstract 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract 4
- 238000001035 drying Methods 0.000 claims abstract 3
- 230000015556 catabolic process Effects 0.000 claims abstract 2
- 230000001112 coagulating effect Effects 0.000 claims abstract 2
- 238000006731 degradation reaction Methods 0.000 claims abstract 2
- 239000012535 impurity Substances 0.000 claims abstract 2
- 239000003039 volatile agent Substances 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 3
- 239000000839 emulsion Substances 0.000 claims 3
- 239000004094 surface-active agent Substances 0.000 claims 3
- MKTOIPPVFPJEQO-UHFFFAOYSA-N 4-(3-carboxypropanoylperoxy)-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OOC(=O)CCC(O)=O MKTOIPPVFPJEQO-UHFFFAOYSA-N 0.000 claims 2
- 239000004160 Ammonium persulphate Substances 0.000 claims 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims 2
- 235000019395 ammonium persulphate Nutrition 0.000 claims 2
- 230000000977 initiatory effect Effects 0.000 claims 2
- 150000007524 organic acids Chemical class 0.000 claims 2
- 235000005985 organic acids Nutrition 0.000 claims 2
- 235000019394 potassium persulphate Nutrition 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 239000004159 Potassium persulphate Substances 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 1
- 150000001298 alcohols Chemical class 0.000 claims 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000015271 coagulation Effects 0.000 claims 1
- 238000005345 coagulation Methods 0.000 claims 1
- 238000007720 emulsion polymerization reaction Methods 0.000 claims 1
- 229930195733 hydrocarbon Natural products 0.000 claims 1
- 150000002430 hydrocarbons Chemical class 0.000 claims 1
- 239000003999 initiator Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 235000006408 oxalic acid Nutrition 0.000 claims 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims 1
- 239000001117 sulphuric acid Substances 0.000 claims 1
- 235000011149 sulphuric acid Nutrition 0.000 claims 1
- 238000010557 suspension polymerization reaction Methods 0.000 claims 1
- 239000000155 melt Substances 0.000 abstract 1
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/16—Powdering or granulating by coagulating dispersions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F14/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F14/18—Monomers containing fluorine
- C08F14/26—Tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/18—Monomers containing fluorine
- C08F114/26—Tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/18—Suspension polymerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/28—Emulsion polymerisation with the aid of emulsifying agents cationic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/32—Organic compounds
- C08F4/34—Per-compounds with one peroxy-radical
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/008—Treatment of solid polymer wetted by water or organic solvents, e.g. coagulum, filter cakes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
- C08F6/18—Increasing the size of the dispersed particles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
- C08F6/22—Coagulation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/24—Treatment of polymer suspensions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
- Polymerization Catalysts (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention relates to low molecular weight polytetrafluoroethylene (PTFE) micropowder, The present invention relates to production of low molecular weight PTFE micropowder by direct polymerization technology and overcomes limitation of the melt viscosities over prior art and that is devoid of the step of irradiation or thermal degradation and complies with regulations on PFOA restriction in substances. The present invention relates to a process for preparing a low molecular weight polytetrafluoroethylene (PTFE) micropowder, comprising the steps of:(a) polymerizing Tetrafluoroethylene (TFE); (b) coagulating the particles of PTFE to increase particle size; (c) washing the particles of PTFE to remove impurities; and (d) drying the wet PTFE micropowder to remove moisture and volatiles.
Claims (10)
1. A low molecular weight Polytetrafluoroethylene (PTFE) micropowder; wherein the low molecular weight polytetrafluoroethylene (PTFE) micropowder is having melt viscosity of 1,000,001- 999,999,999 Pascal at 380° C at 21.6 Kg load.
2. The low molecular weight Polytetrafluoroethylene (PTFE) micropowder as claimed in claim 1; wherein the low molecular weight polytetrafluoroethylene (PTFE) micropowder is produced by direct polymerization process.
3. The low molecular weight Polytetrafluoroethylene (PTFE) micropowder as claimed in claim 1 is produced without irradiation or any other forms of degradation methods.
4. The low molecular weight PTFE micropowder as claimed in claim 1 wherein specific surface area (SSA) is 3.0 to 20.0 m2/g.
5. A process for preparing a low molecular weight polytetrafluoroethylene (PTFE) micropowder, comprising the steps of: (a) polymerizing Tetrafluoroethylene (TFE); (b) coagulating the particles of PTFE to increase particle size; (c) washing the particles of PTFE to remove impurities; and (d) drying the wet PTFE micropowder to remove moisture and volatiles wherein the low molecular weight polytetrafluoroethylene (PTFE) micropowder is having melt viscosity of 1,000,001- 999,999,999 Pascal at 380°C at 21.6 Kg load
6. The process as claimed in claim 5, wherein the step of polymerizing TFE comprises: (a) forming an aqueous emulsion comprising a surfactant system and a fluoromonomer; and (b) initiating polymerization of said fluoromonomer Wherein in surfactant system comprises of fluorosurfactant or non fluoro-surfactant or a combination of these.
7. The process as claimed in any of the claims 5 to 6, wherein the aqueous emulsion comprises an initiator for initiating the polymerization process, selected from the group consisting of Disuccinic Acid Peroxide (DSAP), Ammonium Persulphate (APS), Potassium Persulphate (KPS) and combinations thereof and the aqueous emulsion comprises chain transfer agents selected from the group consisting of alcohols, hydrocarbons and combinations thereof.
8. The process as claimed in claim 5, wherein the step of polymerizing TFE comprises suspension polymerization or emulsion polymerization.
9. The process as claimed in claim 5, wherein the step of coagulation is induced by adding organic acids or inorganic acidswherein the organic acids comprises of group consisting of phosphoric acid, oxalic acid, nitric acid, sulphuric acid, hydrochloric acid and combination thereof.
10. The process as claimed in claim 5, wherein the step of drying the wet PTFE micropowder is carried out at less than or equal to 450 °C and step of polymerizing TFE is carried out at a temperature of 20 to 120 °C, pressure of 8 to 25 Bar and for a period of 60 to 400 minutes.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IN201911037462 | 2019-09-17 | ||
| PCT/IB2020/058608 WO2021053531A1 (en) | 2019-09-17 | 2020-09-16 | Low molecular weight polytetrafluoroethylene micropowder and process for preparing the same |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB202205473D0 GB202205473D0 (en) | 2022-05-25 |
| GB2604463A true GB2604463A (en) | 2022-09-07 |
| GB2604463B GB2604463B (en) | 2024-02-28 |
Family
ID=74884009
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB2205473.8A Active GB2604463B (en) | 2019-09-17 | 2020-09-16 | Low molecular weight polytetrafluoroethylene micropowder and process for preparing the same |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP4031589A4 (en) |
| JP (1) | JP2023501048A (en) |
| KR (1) | KR20220065003A (en) |
| CN (1) | CN114450317A (en) |
| GB (1) | GB2604463B (en) |
| WO (1) | WO2021053531A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7385150B2 (en) * | 2022-04-18 | 2023-11-22 | ダイキン工業株式会社 | Method for producing purified polytetrafluoroethylene powder and low molecular weight polytetrafluoroethylene powder |
| WO2024172080A1 (en) * | 2023-02-16 | 2024-08-22 | ダイキン工業株式会社 | Method for producing low molecular weight polytetrafluoroethylene aqueous dispersion |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004050727A1 (en) * | 2002-11-22 | 2004-06-17 | E.I. Du Pont De Nemours And Company | Directly polymerized low molecular weight granular polytetrafluoroethylene |
| EP2267047B1 (en) * | 2008-04-14 | 2012-01-18 | Asahi Glass Company, Limited | Production method of polytetrafluoroethylene fine powder |
| US20130122302A1 (en) * | 2010-09-30 | 2013-05-16 | Daikin Industries, Ltd. | Process for producing polytetrafluoroethylene fine powder |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6395848B1 (en) * | 1999-05-20 | 2002-05-28 | E. I. Du Pont De Nemours And Company | Polymerization of fluoromonomers |
| US8071198B2 (en) * | 2006-11-17 | 2011-12-06 | E.I. Du Pont De Nemours And Company | Glass articles with adhesion and stain resistant non-stick coatings |
| CN102369221B (en) * | 2009-03-31 | 2014-03-12 | 大金工业株式会社 | Low molecular weight polytetrafluoroethylene powder and preparation method therefor |
| US9175110B2 (en) * | 2012-05-09 | 2015-11-03 | The Chemours Company Fc, Llc | Fluoropolymer resin treatment employing melt extrusion and exposure to oxygen source to reduce discoloration |
-
2020
- 2020-09-16 JP JP2022516619A patent/JP2023501048A/en active Pending
- 2020-09-16 GB GB2205473.8A patent/GB2604463B/en active Active
- 2020-09-16 EP EP20866024.1A patent/EP4031589A4/en active Pending
- 2020-09-16 CN CN202080064703.4A patent/CN114450317A/en active Pending
- 2020-09-16 KR KR1020227012593A patent/KR20220065003A/en unknown
- 2020-09-16 WO PCT/IB2020/058608 patent/WO2021053531A1/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004050727A1 (en) * | 2002-11-22 | 2004-06-17 | E.I. Du Pont De Nemours And Company | Directly polymerized low molecular weight granular polytetrafluoroethylene |
| EP2267047B1 (en) * | 2008-04-14 | 2012-01-18 | Asahi Glass Company, Limited | Production method of polytetrafluoroethylene fine powder |
| US20130122302A1 (en) * | 2010-09-30 | 2013-05-16 | Daikin Industries, Ltd. | Process for producing polytetrafluoroethylene fine powder |
Also Published As
| Publication number | Publication date |
|---|---|
| EP4031589A1 (en) | 2022-07-27 |
| EP4031589A4 (en) | 2023-10-04 |
| KR20220065003A (en) | 2022-05-19 |
| CN114450317A (en) | 2022-05-06 |
| WO2021053531A1 (en) | 2021-03-25 |
| GB202205473D0 (en) | 2022-05-25 |
| JP2023501048A (en) | 2023-01-18 |
| GB2604463B (en) | 2024-02-28 |
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