GB1590281A - Method of and apparatus for extruding thermoplastics material - Google Patents
Method of and apparatus for extruding thermoplastics material Download PDFInfo
- Publication number
- GB1590281A GB1590281A GB34202/77A GB3420277A GB1590281A GB 1590281 A GB1590281 A GB 1590281A GB 34202/77 A GB34202/77 A GB 34202/77A GB 3420277 A GB3420277 A GB 3420277A GB 1590281 A GB1590281 A GB 1590281A
- Authority
- GB
- United Kingdom
- Prior art keywords
- orifice
- extrusion
- outlet end
- reservoir
- coolant
- 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.)
- Expired
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/86—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling at the nozzle zone
- B29C48/87—Cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/05—Filamentary, e.g. strands
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/06—Rod-shaped
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/30—Extrusion nozzles or dies
- B29C48/345—Extrusion nozzles comprising two or more adjacently arranged ports, for simultaneously extruding multiple strands, e.g. for pelletising
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/86—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling at the nozzle zone
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Description
(54) IMPROVED METHOD OF AND APPARATUS FOR EXTRUDING
THERMOPLASTICS MATERIAL
(71) We, LEESONA CORPORATION, a corporation existing under the laws of the
Commonwealth of Massachusetts United
States of America of Warwick State of Rhode
Island United States of America, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:- This invention relates to a method of extruding thermoplastics material.
U.S. Patent 3,981,959 discloses a system which permits drastically increased pelleting operation efficiencies by means of the introduction of liquid coolant under pressure into direct contact with the outer surface of polymeric material passing through its containing die orifice, vaporizing a part of said coolant immediately upon entrance thereof to said orifice to form at least a solidified outer wall of the material surrounding an inner core thereof, while simultaneously lubricating the wall of the orifice by non-vaporized coolant to facilitate the passage of the material therethrough.
Upon emergence of such partially solidified material at the die exit, in rod or strand-like form, such may be cut by rotating knives without the need of additional cooling to produce individual pellets at a higher operational speed with significant reduction of smearing or the tendency of pellets to string together in the form of clumps. While such apparatus and the method of accomplishing such pelletizing represents significant advance over the prior art by reason of its highly efficient heat transfer mechanisms, such does on occasion produce freeze-ups, that is, slugs of solidified polymer which block individual orifices or bores of the many such orifices utilized in production type equipment. Once such a freeze-up has occurred in an individual extrusion bore, the coolant medium in the form of partially vaporized liquid coolant is blocked in the extrusion passage behind such blockage and eventually it is possible by reason of its softening effect upon the frozen plug will melt or soften the plug to an extent to enable resumption of polymer extrusion within such orifice. The present invention is directed to a method and apparatus for reducing the frequency of such freeze-ups and for providing a more efficient and assured manner of extrusion resumption after such freeze-offs take place.
Accordingly the primary object of the present invention is to provide an improved method for melting solidified polymer plugs which have frozen in an individual extrusion bore of a pelletizing apparatus of the aforementioned type which utilizes a combination coolant and lubricating medium of pressurized liquid coolant.
Such is accomplished in the present invention by the provision of a method comprising heating the material to make it fluid; conveying the material into the inlet end of an extrusion orifice in an extrusion die; forcing the material through the orifice and outward from an outlet end thereof in rod or strandlike form of which an outer wall structure at least is solidified; directing a liquid coolant under pressure into the extrusion orifice at a location intermediate the ends thereof to contact the outer surface of the material passing therethrough while at least partially vaporizing said coolant simultaneously to form said solidified wall structure and to provide a lubricating film between the inner wall of the orifice and the material to facilitate passage of material through the orifice; providing a heat reservoir adjacent the outlet end of the orifice downstream from said location at a significantly higher temperature than the softening temperature range of the material and maintaining the partially vaporized coolant between the outer wall structure and the inner wall of the orifice whereby said structure is thermally insulated from the reservoir while the extrusion continues and in thermal contact therewith when the coolant flow is discontinued by a material freeze-off at the outlet end of the orifice.
The invention will now be described by way of example with reference to the accompanying drawings in which: Figure 1 is a cross sectional view in stylized form of an extrusion die similar to that disclosed in the above mentioned U S patent.
Figure 2 is a partial sectional view showing a heat reservoir according to the present invention and
Figure 3 is a view similar to Figure 2 showing a modified construction.
Turning now to the drawing and in particular Fig. 1 thereof, an extrusion die 10 representative of those described in the aforementioned patent is depicted. Such die 10 is generally of ring-like configuration and includes a plurality of extrusion orifices 12 adapted for operative engagement generally with an extruder as is known in the art. The die includes an initial zone for feeding a thermoplastics resinous material such as polypropylene, polyethylene, or the like in a heated fluid condition and forcing such material through the plurality of such extrusion orifices 12. Such zone is bracketed and indicated by the reference numeral 14 in Fig. I of the drawing. Thereafter, the material passes through an intermediate zone 16 wherein coolant under pressure i.e., water is introduced as through opening 15 into direct contact with the outer surface of the resinous material filling the extrusion orifice 12 as through body 18 preferably of open porous metal construction as depicted. As soon as the coolant comes in contact with the material, by reason of an accompanying pressure reduction, a part of the coolant is immediately vaporized and accordingly quickly by heat of vaporization,and temperature reduction transfer, removes an extensive amount of heat from the material contained therein. Although the system is hydraulically open, that is, the extrusion orifice 12 exits at the die face 20 of the die 10 in an unrestrained manner, a portion of the liquid coolant is maintained in liquid state as it passes along the extrusion orifice 12 to the exit face thereof inasmuch as a pressure gradient is set up within the extrusion orifice 12 from the high pressure end at the initial zone 14 thereof to the ambient or low pressure end at the exit end thereof establishes cooling gradients at surfaces of the polymer strand and orifice wall and in turn cooling to take place thereat. Such higher than ambient pressures within the extrusion orifice 12 permits such liquid phase to be present even though temperatures considerably higher than would permit liquid phase presence at normal atmospheric pressures are maintained in the orifice 12. It is thus believed that a combination of vapor, that is, vaporized water and liquid phase water are present between the outside surface of the material being extruded and the inside surface of the orifice 12 in such a manner so as to form an effective combination coolant and lubrication film or medium as the material passes therethrough. The above explanation is believed to be that which takes place within the extrusion orifice 12 although other explanations consistent with the effective passage of the material therethrough and the formation of a solidified and cooled skin surrounding an inner core of material as the material in rod or strand-like form emerges from the die face may exist.
The porous member 18 may be secured to the die 10 by means of an insert 22 threadably or otherwise positioned within an outer section 24 of the die body. Appropriate seals 25 may be provided therebetween as is known.
The portion of the die downstream from the die body portion 24, provides a final extrusion zone 28 downstream of the aforementioned intermediate zone in which the material is contained in the form of rod or strand-like configurations having an outer solidified surface during its passage through the die.
Upon emergence from the die face, a cutter is positioned to cut the rod or strand-like material into discrete separate pellets.
With such systems one or more of the extrusion orifices 12 by reason of the strong cooling action provided by the depressurized coolant and particularly by reason of the induced ebullition (heat of vaporization effect) upon the aforementioned surface of such material and for other reasons may become blocked or plugged with chilled soldified masses of material so that strand emergence from such extrusion orifice or orifices is temporarily blocked. While the plugging of one or even several of such extrusion orifices 12 in a die body having many such orifices is not a particularly serious problem, there does become a point where the efficiency of the operation is hindered. It would, of course, be desirable to pinpoint such plugs and direct heat specifically thereto to melt the same; however, such is not practical due to the great number of orifices generally utilized, at least with the present state of the art. Also a general maintenance of a heat source surrounding the orifices at a substantially higher temperature is known to adversely affect strand control in hitherto known extrusion systems. However, apparently the amount and manner of the coolant system provided for in the aforementioned process of which this invention represents an improvement thereover, permits a transfer of heat from the adjacent orifice surfaces without adversely affecting the condition and hence control over the emerging strand. Accordingly a prime feature of the present invention is the maintenance of areas surrounding the orifices at a temperature substantially higher than the softening temperature range of the polymer passing therethrough; however, the effects of this higher temperature are not transferred to the polymer necessarily in terms of added heat to adversely raise its temperature since the highly effective coolant system removes not only heat from the poly mer itself to cool such and form at least a cooled exterior shell thereon but further serves to remove the heat transferred to the orifice by the surrounding heat source. The above steady state conditions are present so long as the polymer continues its flow through the particular orifice under consideration and in the particular manner above described and the coolant flow between such polymer and the interior surfaces of such orifice is maintained. However, when the polymer flow ceases as by the formation of a freeze-off, the thermal reserve brought about by the proximity of the high temperature heat source is immediately available for melting said frozen polymer. In order not to deplete the heat reservoir during normal steady-state operation, however, it has been found useful to reduce or limit the rate at which the heat from the area surrounding the orifices i.e., the heat reservoir is available to the outer surface of the orifice walls and accordingly in turn available to the strand or rodlike form of material as it either passes through the orifice 12 or is stationary therein as when freeze-offs occur. Referring now to
Fig. 2, an insert 22a surrounding an orifice 12 is positioned partially within the outer region 24a of the body portion 24 so as to project outwardly therefrom. In juxtaposition with the body region 24a is an outer plate-like heat reservoir 26 positioned as by spacers or other conventional means which may be provided about the periphery thereof, so as to be spaced apart from the outer surface of the region 24a thereby providing an air gap 29 therebetween. Such air gap 29 not only extends along the front face of the region 24a but also surrounds the inserts 22a for a major extent thereof and in such a way reduces the rate at which the heat from the high temperature heat reservoir 26 is available to the material extrusion orifice 12 by at least partially insulating such therefrom. However, the continual radiation exchange of heat between the heat reservoir 26 across the insulative air gap 29 into contact with a major extent of the insert 22, although at a slower rate than would take place with conductive transfer allows the forzen polymer plug to be melted and extrusion started again. The provision of such a high temperature heat reservoir further enables preheating of the extrusion orifices to a higher temperature than hitherto available during the start-up of the extrusion apparatus.
It should be noted that separate heating means (not shown) are maintained within the heat reservoir 26 so as to enable its temperature to be maintained separately and at a substantially higher temperature than that of the remainder of the die 10. Preferably, the heat reservoir is maintained at a temperature of at least 500-2000F above the softening temperature range of the polymer. The heat reservoir 26 as shown in Fig. 2 may also be provided with a boss 30 in physical contact and conductive heating relationship to the sleeve 22a so as to provide an increased rate of heat passage in those cases where such is necessary and preferably proximal to the exit face of the die inasmuch as such area tends to be exposed to more variations in ambient temperatures and as such could cause greater strand variation to the polymer passing therethrough. Such boss 30 by reason of its minor extent in relationship to the overall extent of the extrusion orifice 12 within the heat reservoir 26 minimizes the extent of efficient heat coupling between the die components and accordingly reduces the heat exchange from the reservoir 26 to the extrusion sleeve 12 and in turn minimizes the increased load in which combination lubrication and coolant film present in the system is required to absorb without materially reducing its lubrication and cooling effects upon the material being extruded.
Turning now to Fig. 3 of the drawing, a similar plate-like heat reservoir 26b is depicted. Such reservoir 26b is spaced from the insert 22a by means of a cermaic insert 32 which as depicted, may be of two piece construction, that is, a planar portion adapted to fit against the region 24a and a cylindrical extension adapted to surround the insert 22a.
In such alternative embodiment, heat reservoir 26b may also be provided with an inwardly extending boss 30 to provide a portion of conductive and more efficient heat transfer between the heat reservoir and the material being extruded; the common feature between both embodiments being the insulative feature which reduces the rate of heat transfer in order to conserve energy requirements.
The following is an example of the aboveillustrative and described improved extrusion process wherein polypropylene having a melt flow index of 5 and with the midpoint of its workable melting temperature range about 450"F. was extruded at a rate of approximately 2,500 Ibs./hr. through a two-stage 400 H.P. extruder available from Johnson
Plastics Machinery Co., Chippewa Falls,
Wisconsin, U.S.A., coupled to a die face cutter as described in the previously referred to patent. The outer plate i.e., the heat reservoir was maintained at temperatures varying from 500"F. to 600"F. Water coolant was introduced under high pressure via open cell sintered metal inserts surrounding each orifice as taught by the previously referred to applications at a rate wherein the rods of polymer emerging from the die face exhibited an outer hardened cooled polymer shell which when cut produced individual pellets without evidence of smearing.
The equipment and process utilized as above related to polypropylene was conducted with commercially available ABS polymer having an approximate midpoint melting temperature range workable for extrusion of 425"F. at the same rates as above indicated but wherein the outer plate or heat reservoir was maintained at a temperature of approximately 555"F. Again polymer rods exhibiting a cooled outer shell which when cut produced discrete pellets without evidence of smearing were produced.
WHAT WE CLAIM IS:- 1. A method of extruding thermoplastics material, comprising heating the material to make it fluid; conveying the material into the inlet end of an extrusion orifice in an extrusion die; forcing the material through the orifice and outward from an outlet end thereof in rod or strand-like form of which an outer wall structure at least is solidified; directing a liquid coolant under pressure into the extrusion orifice at a location intermediate the ends thereof to contact the outer surface of the material passing therethrough while at least partially vaporizing said coolant simultaneously to form said solidified wall structure and to provide a lubricating film between the inner wall of the orifice and the material to facilitate passage of material through the orifice; providing a heat reservoir adjacent the outlet end of the orifice downstream from said location at a significantly higher temperature than the softening temperature range of the material and maintaining the partially vaporized coolant between the outer wall structure and the inner wall of the orifice whereby said structure is thermally insulated from the reservoir while the extrusion continues and in thermal contact there with when the coolant flow is discontinued by a material freeze-off at the outlet end of the orifice.
2. A method according to Claim 1, wherein the heat reservoir is maintained at a temperature of at least 500-2000F above the softening temperature range of the material and wherein said coolant is water.
3. A method according to Claim 1 or
Claim 2, including cutting said rods into discrete pellets as they emerge from the outlet end of the extrusion orifice.
4. A method according to any one of the preceding claims, wherein the heat reservoir extends from the outlet end of the orifice over a longitudinal region of the extrusion orifice, the rate of heat transfer from the reservoir to the orifice being arranged to be greatest at the outlet end of the orifice.
5. A method according to Claim 4, wherein heat transfer from the reservoir to the orifice is by conduction over a minor portion of said longitudinal region adjacent the outlet end and by convection and radiation over the remainder of said longitudinal region.
6. A method according to Claim 4, wherein insulating material is disposed between the orifice and the heat reservoir over a major portion of said longitudinal portion remote from the outlet end of the orifice.
7. A method of extruding thermoplastics material, substantially as hereinbefore described with reference to and as shown in
Figure 2 or Figure 3 of the accompanying drawings.
**WARNING** end of DESC field may overlap start of CLMS **.
Claims (7)
1. A method of extruding thermoplastics material, comprising heating the material to make it fluid; conveying the material into the inlet end of an extrusion orifice in an extrusion die; forcing the material through the orifice and outward from an outlet end thereof in rod or strand-like form of which an outer wall structure at least is solidified; directing a liquid coolant under pressure into the extrusion orifice at a location intermediate the ends thereof to contact the outer surface of the material passing therethrough while at least partially vaporizing said coolant simultaneously to form said solidified wall structure and to provide a lubricating film between the inner wall of the orifice and the material to facilitate passage of material through the orifice; providing a heat reservoir adjacent the outlet end of the orifice downstream from said location at a significantly higher temperature than the softening temperature range of the material and maintaining the partially vaporized coolant between the outer wall structure and the inner wall of the orifice whereby said structure is thermally insulated from the reservoir while the extrusion continues and in thermal contact there with when the coolant flow is discontinued by a material freeze-off at the outlet end of the orifice.
2. A method according to Claim 1, wherein the heat reservoir is maintained at a temperature of at least 500-2000F above the softening temperature range of the material and wherein said coolant is water.
3. A method according to Claim 1 or
Claim 2, including cutting said rods into discrete pellets as they emerge from the outlet end of the extrusion orifice.
4. A method according to any one of the preceding claims, wherein the heat reservoir extends from the outlet end of the orifice over a longitudinal region of the extrusion orifice, the rate of heat transfer from the reservoir to the orifice being arranged to be greatest at the outlet end of the orifice.
5. A method according to Claim 4, wherein heat transfer from the reservoir to the orifice is by conduction over a minor portion of said longitudinal region adjacent the outlet end and by convection and radiation over the remainder of said longitudinal region.
6. A method according to Claim 4, wherein insulating material is disposed between the orifice and the heat reservoir over a major portion of said longitudinal portion remote from the outlet end of the orifice.
7. A method of extruding thermoplastics material, substantially as hereinbefore described with reference to and as shown in
Figure 2 or Figure 3 of the accompanying drawings.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US05/727,155 US4112039A (en) | 1975-02-12 | 1976-09-27 | Pelletizing process |
Publications (1)
Publication Number | Publication Date |
---|---|
GB1590281A true GB1590281A (en) | 1981-05-28 |
Family
ID=24921545
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB34202/77A Expired GB1590281A (en) | 1976-09-27 | 1977-08-15 | Method of and apparatus for extruding thermoplastics material |
Country Status (11)
Country | Link |
---|---|
JP (1) | JPS5342253A (en) |
BE (1) | BE858442A (en) |
BR (1) | BR7706266A (en) |
CA (1) | CA1104780A (en) |
CH (1) | CH618381A5 (en) |
DE (1) | DE2741256A1 (en) |
FR (1) | FR2365431A1 (en) |
GB (1) | GB1590281A (en) |
IT (1) | IT1090860B (en) |
NL (1) | NL7710467A (en) |
SE (1) | SE7710208L (en) |
-
1977
- 1977-08-15 GB GB34202/77A patent/GB1590281A/en not_active Expired
- 1977-08-17 CA CA284,876A patent/CA1104780A/en not_active Expired
- 1977-09-06 BE BE180704A patent/BE858442A/en unknown
- 1977-09-07 FR FR7727146A patent/FR2365431A1/en active Granted
- 1977-09-08 IT IT69004/77A patent/IT1090860B/en active
- 1977-09-12 CH CH1112777A patent/CH618381A5/en not_active IP Right Cessation
- 1977-09-12 SE SE7710208A patent/SE7710208L/en not_active Application Discontinuation
- 1977-09-14 DE DE19772741256 patent/DE2741256A1/en not_active Withdrawn
- 1977-09-20 BR BR7706266A patent/BR7706266A/en unknown
- 1977-09-26 NL NL7710467A patent/NL7710467A/en not_active Application Discontinuation
- 1977-09-27 JP JP11522877A patent/JPS5342253A/en active Pending
Also Published As
Publication number | Publication date |
---|---|
SE7710208L (en) | 1978-03-28 |
NL7710467A (en) | 1978-03-29 |
BR7706266A (en) | 1978-05-30 |
DE2741256A1 (en) | 1978-03-30 |
BE858442A (en) | 1978-01-02 |
CA1104780A (en) | 1981-07-14 |
IT1090860B (en) | 1985-06-26 |
CH618381A5 (en) | 1980-07-31 |
FR2365431B3 (en) | 1980-06-06 |
JPS5342253A (en) | 1978-04-17 |
FR2365431A1 (en) | 1978-04-21 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
PS | Patent sealed [section 19, patents act 1949] | ||
PCNP | Patent ceased through non-payment of renewal fee |