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US4013751A Expired / Lapsed US ⏱️ 0.0 years remaining

Fibrils and processes for the manufacture thereof

Assignee: Gulf Research and Development Co
•
Filing: 1974-06-14
•
Granted: 1977-03-22
•
Expires: 1994-06-14
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Abstract

Abstract A process for producing a mass of entangled solvent swollen polymer filaments which can be converted into paper-making fibrils by subsequent refining. An olefin polymer such as polyethylene having an inherent viscosity of at least 3.5 is dissolved in a hot solvent. The hot polymer solution is subjected to timed sequential steps in which the polymer solution first is sheared and attenuated into fine polymer streams. The hot polymer streams then are cooled to precipitate the polymer which is recovered as a mass of entangled solvent swollen filaments. These filaments can be beaten in a non-solvent liquid such as isopropanol to prepare fibrils having diameters on the order of about 5 to 30 microns and lengths of about 1 to 15 millimeters.

Inventors

  • 👤 Joseph C. Davis
  • 👤 Francis R. Galiano
  • 👤 Robert W. Hill

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 22:55
CPC Classifications
D; D01; D01D; D01D5/00; D01D5/11; D01D5/40; D21; D21H; D21H13/00; D21H13/10; D21H13/12; D21H13/14; D21H5/00; D21H5/12; D21H5/20; D21H5/202

Claims Analysis

Total Claims: 43
Claim 1
Independent Claim 223 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. subjecting said heated polymer solution to shearing forces and attenuating said solution into liquid streams to orient the solute polymer molecules in said liquid streams while maintaing said polymer solution at a temperature sufficiently high to maintain substantially all of said polymer in solution; c. feeding said liquid streams into a cooling zone in which said streams are cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; and d. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containng at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene; 2.
Claim 2
Dependent Claim 223 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. subjecting said heated polymer solution to shearing forces and attenuating said solution into liquid streams to orient the solute polymer molecules in said liquid streams while maintaing said polymer solution at a temperature sufficiently high to maintain substantially all of said polymer in solution; c. feeding said liquid streams into a cooling zone in which said streams are cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; and d. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containng at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene; 2.
Claim 3
Dependent Claim 38 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble
Claim 4
Dependent Claim 38 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble
Claim 5
Dependent Claim 52 words
at 100° C. in the solvent employed in step (a). 2. The process of claim 1 in which the olefin polymer employed in the process is an ethylene polymer containing, on a weight basis, at least 90% of polymerized ethylene with any monomer copolymerized therewith being a C-4 or higher olefin hydrocarbon.
Claim 6
Dependent Claim 34 words
The process of claim 1 in which the olefin polymer employed therein is a propylene polymer containing, on a weight basis, at least 50% of polymerized propylene and any monomer copolymerized therewith being ethylene.
Claim 7
Dependent Claim 22 words
The process of claim 1 in which the olefin polymer employed in the process constitutes the sole polymer employed in the process.
Claim 8
Dependent Claim 22 words
The process of claim 4 in which the ethylene polymer employed in the process constitutes the sole polymer employed in the process.
Claim 9
Dependent Claim 22 words
The process of claim 5 in which the propylene polymer employed in the process constitutes the sole polymer employed in the process.
Claim 10
Dependent Claim 71 words
The process of claim 1 in which the polymer employed in the process consists of a polymer mixture containing, on a weight basis, (a) at least 20% of an ethylene polymer containing, on a weight basis, at least 90% of polymerized ethylene with any monomer copolymerized therewith being a C-4 or higher olefin hydrocarbon, and (b) the balance a copolymer of ethylene with an alkyl ester of acrylic or methacrylic acid.
Claim 11
Dependent Claim 116 words
The process of claim 1 in which the polymer employed in the process consists of a polymer mixture containing, on a weight basis, (a) at least 20% of an olefin polymer having an inherent viscosity of at least 3.5, and (b) the balance a copolymer of ethylene with vinyl acetate; said olefin polymer being selected from the group consisting of (1) an ethylene polymer containing, on a weight basis, at least 90% of polymerized ethylene with any monomer copolymerized therewith being a C-4 or higher olefin hydrocarbon; (2) a propylene polymer containing, on a weight basis, at least 50% of polymerized propylene and any monomer copolymerized therewith being ethylene; and (3) mixtures of (1) and (2).
Claim 12
Dependent Claim 126 words
The process of claim 1 in which the polymer employed in the process consists of a polymer mixture containing, on a weight basis, (a) at least 20% of an olefin polymer having an inherent viscosity of at least 3.5, and (b) the balance a copolymer of maleic anhydride with either styrene or a mono-1-olefin containing 6 to 18 carbon atoms; said olefin polymer being selected from the group consisting of (1) an ethylene polymer containing, on a weight basis, at least 90% of polymerized ethylene with any monomer copolymerized therewith being a C-4 or higher olefin hydrocarbon; (2) a propylene polymer containing, on a weight basis, at least 50% of polymerized propylene and any monomer copolymerized therewith being ethylene; and (3) mixtures of (1) and (2).
Claim 13
Dependent Claim 192 words
The process of claim 1 in which the polymer employed in the process consists of a polymer mixture containing, on a weight basis, (a) at least 20% of an olefin polymer having an inherent viscosity of at least 3.5, and (b) the balance an alkylated N-vinyl-2-pyrrolidone/α-olefin copolymer containing, (c) polymerized monomer units conforming to the formula: ##STR3## wherein R 1 , R 2 and R 3 are independently hydrogen or an alkyl group containing 2 to about 180 carbon atoms, and (d) polymerized monomer units of the formula: ##STR4## wherein R 4 is hydrogen or an alkyl group containing 1 to about 180 carbon atoms, said unit (A) constituting from about 90 to about 99 mol % of the total of said units (A) plus (B); said olefin polymer being selected from the group consisting of (1) an ethylene polymer containing, on a weight basis, at least 90% of polymerized ethylene with any monomer copolymerized therewith being a C-4 or higher olefin hydrocarbon; (2) a propylene polymer containing, on a weight basis, at least 50% of polymerized propylene and any monomer copolymerized therewith being ethylene; and (3) mixtures of (1) and (2).
Claim 14
Dependent Claim 401 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding said heated polymer solution to the inlet of a centrifugal spinning apparatus including therein: i. a housing, ii. a stationary disc-shaped plate attached to said housing, iii. a rotatable disc-shaped plate within said housing positioned closely adjacent to and parallel to but spaced from said stationary plate, iv. an inlet in the stationary disc-shaped plate adapted to feed liquid onto the rotatable disc-shaped plate, v. a plurality of flails pivotally attached to the circumference of said rotatable plate, vi. means for rotating said rotatable disc-shaped plate, and vii. an outlet in said housing; c. rotating said rotatable disc-shaped plate at a speed such that said flails are extended so as to define an annulus about the circumference of said rotating plate and said rotating plate has a tangential velocity of at least 100 cm/sec at the position where said polymer solution contacts said rotating disc-shaped plate so that said polymer solution is subjected to shearing forces, attenuated into liquid streams, and said liquid streams are fed into the annulus defined by said flails; d. feeding a coolant liquid into said housing and about said flails so as to contact the liquid polymer streams entering said annulus defined by said flails so as to cool said polymer streams to a temperature to precipitate substantially all said solute polymer as solvent swollen polymer filaments, the weight of said coolant liquid fed to said housing exceeding the weight of the polymer solution fed to the apparatus in step (b); and e. recovering a mass of entangled solvent swollen polymer filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and
Claim 15
Dependent Claim 401 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding said heated polymer solution to the inlet of a centrifugal spinning apparatus including therein: i. a housing, ii. a stationary disc-shaped plate attached to said housing, iii. a rotatable disc-shaped plate within said housing positioned closely adjacent to and parallel to but spaced from said stationary plate, iv. an inlet in the stationary disc-shaped plate adapted to feed liquid onto the rotatable disc-shaped plate, v. a plurality of flails pivotally attached to the circumference of said rotatable plate, vi. means for rotating said rotatable disc-shaped plate, and vii. an outlet in said housing; c. rotating said rotatable disc-shaped plate at a speed such that said flails are extended so as to define an annulus about the circumference of said rotating plate and said rotating plate has a tangential velocity of at least 100 cm/sec at the position where said polymer solution contacts said rotating disc-shaped plate so that said polymer solution is subjected to shearing forces, attenuated into liquid streams, and said liquid streams are fed into the annulus defined by said flails; d. feeding a coolant liquid into said housing and about said flails so as to contact the liquid polymer streams entering said annulus defined by said flails so as to cool said polymer streams to a temperature to precipitate substantially all said solute polymer as solvent swollen polymer filaments, the weight of said coolant liquid fed to said housing exceeding the weight of the polymer solution fed to the apparatus in step (b); and e. recovering a mass of entangled solvent swollen polymer filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and
Claim 16
Dependent Claim 39 words
a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 17
Dependent Claim 39 words
a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 18
Dependent Claim 342 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding the heated polymer solution to the inlet of a rotatable centrifugal spinning device including therein; i. a housing, ii. an outer basket mounted within said housing, iii. means for cooling said outer basket, iv. a perforated inner drum mounted for rotation within said outer basket and spaced therefrom, v. an inlet in the housing communicating with the inner drum, and vi. an outlet in the housing; c. rotating said inner drum at a speed to centrifugally throw said polymer solution outwardly therefrom with a centrifugal acceleration of at least 25 times that of gravity so that said polymer solution is subjected to shearing forces and attenuated into liquid streams which impinge upon said outer basket; d. cooling the outer basket so that said polymer solution impinging thereon is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; and e. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 19
Dependent Claim 342 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding the heated polymer solution to the inlet of a rotatable centrifugal spinning device including therein; i. a housing, ii. an outer basket mounted within said housing, iii. means for cooling said outer basket, iv. a perforated inner drum mounted for rotation within said outer basket and spaced therefrom, v. an inlet in the housing communicating with the inner drum, and vi. an outlet in the housing; c. rotating said inner drum at a speed to centrifugally throw said polymer solution outwardly therefrom with a centrifugal acceleration of at least 25 times that of gravity so that said polymer solution is subjected to shearing forces and attenuated into liquid streams which impinge upon said outer basket; d. cooling the outer basket so that said polymer solution impinging thereon is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; and e. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 20
Dependent Claim 256 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. forcing said heated polymer solution through an elongated die to shear said solution and thereby orient the polymer molecules therein; c. feeding the stream of polymer solution from said die into a cooling zone in which the stream of polymer solution is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; and d. recovering said polymer as a mass of entangled solvent swollen fine filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms. iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 21
Dependent Claim 256 words
A process for producing a mass of entangled solvent swollen filaments from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. forcing said heated polymer solution through an elongated die to shear said solution and thereby orient the polymer molecules therein; c. feeding the stream of polymer solution from said die into a cooling zone in which the stream of polymer solution is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; and d. recovering said polymer as a mass of entangled solvent swollen fine filaments from said solvent; said polymer being selected from the group consisting of: 1. an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms. iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 22
Dependent Claim 189 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. subjecting said heated polymer solution to shearing forces and attenuating said solution into liquid streams to orient the solute polymer molecules in said liquid streams while maintaining said polymer solution at a temperature sufficiently high to maintain substantially all of said polymer in solution; c. feeding said liquid streams into a cooling zone in which said streams are cooled to a temperature to precipitate substantially all said solute polymer as solvent swollen polymer filaments; d. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; e. beating said filaments in a liquid which is a non-solvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and f. separating said fibrils from said non-solvent liquid; said polymer being selected from the group consisting of:
Claim 23
Dependent Claim 189 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. subjecting said heated polymer solution to shearing forces and attenuating said solution into liquid streams to orient the solute polymer molecules in said liquid streams while maintaining said polymer solution at a temperature sufficiently high to maintain substantially all of said polymer in solution; c. feeding said liquid streams into a cooling zone in which said streams are cooled to a temperature to precipitate substantially all said solute polymer as solvent swollen polymer filaments; d. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; e. beating said filaments in a liquid which is a non-solvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and f. separating said fibrils from said non-solvent liquid; said polymer being selected from the group consisting of:
Claim 24
Dependent Claim 69 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms. iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene,
Claim 25
Dependent Claim 69 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms. iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene,
Claim 26
Dependent Claim 48 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 27
Dependent Claim 48 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 28
Dependent Claim 360 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding said heated polymer solution to the inlet of a centrifugal spinning apparatus including therein: i. a housing, ii. a stationary disc-shaped plate attached to said housing, iii. a rotatable disc-shaped plate within said housing positioned closely adjacent to and parallel to but spaced from said stationary plate, iv. an inlet in the stationary disc-shaped plate adapted to feed liquid onto the rotatable disc-shaped plate, v. a plurality of flails pivotally attached to the circumference of said rotatable plate, vi. means for rotating said rotatable disc-shaped plate, and vii. an outlet in said housing; c. rotating said rotatable disc-shaped plate at a speed such that said flails are extended so as to define an annulus about the circumference of said rotating plate and said rotating plate has a tangential velocity of at least 100 cm/sec at the position where said polymer solution contacts said rotating disc-shaped plate so that said polymer solution is subjected to shearing forces, attenuated into liquid streams, and said liquid streams are fed into the annulus defined by said flails; d. feeding a coolant liquid into said housing and about said flails so as to contact the liquid polymer streams entering said annulus defined by said flails so as to cool said polymer streams to a temperature to precipitate substantially all said solute polymer as solvent swollen polymer filaments, the weight of said coolant liquid fed to said housing exceeding the weight of the polymer solution fed to the apparatus in step (b); e. recovering a mass of entangled solvent swollen polymer filaments from said solvent; f. beating said filaments in a liquid which is a nonsolvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and g. separating said fibrils from said nonsolvent liquid; said polymer being selected from the group consisting of:
Claim 29
Dependent Claim 360 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding said heated polymer solution to the inlet of a centrifugal spinning apparatus including therein: i. a housing, ii. a stationary disc-shaped plate attached to said housing, iii. a rotatable disc-shaped plate within said housing positioned closely adjacent to and parallel to but spaced from said stationary plate, iv. an inlet in the stationary disc-shaped plate adapted to feed liquid onto the rotatable disc-shaped plate, v. a plurality of flails pivotally attached to the circumference of said rotatable plate, vi. means for rotating said rotatable disc-shaped plate, and vii. an outlet in said housing; c. rotating said rotatable disc-shaped plate at a speed such that said flails are extended so as to define an annulus about the circumference of said rotating plate and said rotating plate has a tangential velocity of at least 100 cm/sec at the position where said polymer solution contacts said rotating disc-shaped plate so that said polymer solution is subjected to shearing forces, attenuated into liquid streams, and said liquid streams are fed into the annulus defined by said flails; d. feeding a coolant liquid into said housing and about said flails so as to contact the liquid polymer streams entering said annulus defined by said flails so as to cool said polymer streams to a temperature to precipitate substantially all said solute polymer as solvent swollen polymer filaments, the weight of said coolant liquid fed to said housing exceeding the weight of the polymer solution fed to the apparatus in step (b); e. recovering a mass of entangled solvent swollen polymer filaments from said solvent; f. beating said filaments in a liquid which is a nonsolvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and g. separating said fibrils from said nonsolvent liquid; said polymer being selected from the group consisting of:
Claim 30
Dependent Claim 69 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene,
Claim 31
Dependent Claim 69 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene,
Claim 32
Dependent Claim 48 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 33
Dependent Claim 48 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 34
Dependent Claim 261 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding the heated polymer solution to the inlet of a rotatable centrifugal spinning device including therein; i. a housing, ii. an outer basket mounted within said housing, iii. means for cooling said outer basket, iv. a perforated inner drum mounted for rotation within said outer basket and spaced therefrom, v. an inlet in the housing communicating with the inner drum, and vi. an outlet in the housing; c. rotating said inner drum at a speed to centrifugally throw said polymer solution outwardly therefrom with a centrifugal acceleration of at least 25 times that of gravity so that said polymer solution is subjected to shearing forces and attenuated into liquid streams which impinge upon said outer basket; d. cooling the outer basket so that said polymer solution impinging thereon is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; e. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; f. beating said filaments in a liquid which is a non-solvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and g. separating said fibrils from said non-solvent liquid; said polymer being selected from the group consisting of:
Claim 35
Dependent Claim 261 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving said polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. feeding the heated polymer solution to the inlet of a rotatable centrifugal spinning device including therein; i. a housing, ii. an outer basket mounted within said housing, iii. means for cooling said outer basket, iv. a perforated inner drum mounted for rotation within said outer basket and spaced therefrom, v. an inlet in the housing communicating with the inner drum, and vi. an outlet in the housing; c. rotating said inner drum at a speed to centrifugally throw said polymer solution outwardly therefrom with a centrifugal acceleration of at least 25 times that of gravity so that said polymer solution is subjected to shearing forces and attenuated into liquid streams which impinge upon said outer basket; d. cooling the outer basket so that said polymer solution impinging thereon is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; e. recovering said polymer as a mass of entangled solvent swollen filaments from said solvent; f. beating said filaments in a liquid which is a non-solvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and g. separating said fibrils from said non-solvent liquid; said polymer being selected from the group consisting of:
Claim 36
Dependent Claim 69 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene,
Claim 37
Dependent Claim 69 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene,
Claim 38
Dependent Claim 48 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight percent of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 39
Dependent Claim 48 words
a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight percent of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 40
Dependent Claim 185 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving a polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. forcing said heated polymer solution through an elongated die to shear said solution and thereby orient the polymer molecules therein; c. feeding the stream of polymer solution from said die into a cooling zone in which the stream of polymer solution is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; d. recovering said polymer as a mass of entangled solvent swollen fine filaments from said solvent; e. chopping said solvent swollen filaments into discrete lengths; f. beating said chopped filaments in a liquid which is a nonsolvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and g. separating said fibrils from said nonsolvent liquid; said polymer being selected from the group consisting of:
Claim 41
Dependent Claim 185 words
A process for producing fibrils suitable for the manufacture of water leaves from a high molecular weight polymer consisting essentially of the sequential steps of: a. dissolving a polymer in a solvent at a temperature above 100° C. to prepare a solution thereof having a viscosity of at least about 50 centipoises; b. forcing said heated polymer solution through an elongated die to shear said solution and thereby orient the polymer molecules therein; c. feeding the stream of polymer solution from said die into a cooling zone in which the stream of polymer solution is cooled to a temperature to precipitate substantially all of said solute polymer as solvent swollen polymer filaments; d. recovering said polymer as a mass of entangled solvent swollen fine filaments from said solvent; e. chopping said solvent swollen filaments into discrete lengths; f. beating said chopped filaments in a liquid which is a nonsolvent for the polymer for a time sufficient to break down said filaments into a plurality of individual fibrils; and g. separating said fibrils from said nonsolvent liquid; said polymer being selected from the group consisting of:
Claim 42
Dependent Claim 118 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).
Claim 43
Dependent Claim 118 words
an olefin polymer having an inherent viscosity of at least 3.5 and selected from the group consisting of: i. an ethylene homopolymer, ii. a copolymer containing at least 90 weight % of polymerized ethylene and the balance a polymerized olefin hydrocarbon containing at least 4 carbon atoms, iii. a propylene homopolymer, and iv. a copolymer containing at least 50 weight % of polymerized propylene and the balance polymerized ethylene, 2. a mixture of olefin polymers of (1), and 3. a mixture of polymers containing at least 20 weight % of an olefin polymer of (1) and up to 80 weight % of a diluent polymer that is soluble at 100° C. in the solvent employed in step (a).

References Cited (Backward Citations)

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1980-03-21 1980-09-20 1981-03-22 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1984-03-21 1984-09-20 1985-03-22 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1988-03-21 1988-09-20 1989-03-22 $7700.00 Window Closed / Lapsed

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