US3987139A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process of forming synthetic fibers
Assignee: Fort James Corp
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Filing: 1974-07-29
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Granted: 1976-10-19
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Expires: 1994-07-29
Abstract
Abstract A process of preparing polymer fibers by adiabatically flashing an emulsion or dispersion of water or other suitable nonsolvent in molten polymer, the emulsion or dispersion including an emulsifying agent and a dispersing aid, at an elevated temperature and pressure through a narrow orifice into a region of reduced temperature and pressure. The water or other nonsolvent is present in an amount effective, in combination with the temperature and pressure employed, to cause the molten polymer to be disrupted and rapidly solidify in the form of high surface area, i.e., at least 1.0 m 2 /gram, discrete fibers. The polymer is preferably a crystalline polymer. The nonsolvent employed should have a boiling point less than the melting point of the polymer, a critical temperature greater than the melting point of the polymer, a heat of vaporization greater than the heat of fusion of the polymer, and is substantially immiscible in the polymer at the temperature of flashing.
Inventors
- 👤 John H. Kozlowski
- 👤 Robert E. Howard
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 22:21
CPC Classifications
D; D01; D01D; D01D5/00; D01D5/11
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
269 words
A process for producing discrete polymer fibers having a surface area greater than 1.0 m 2 /g, comprising the steps of: a. forming a water-in-oil emulsion consisting essentially of a continuous phase formed of a molten crystalline fiber-forming polymer, a discontinuous phase formed of from about 15 to 45% by weight, based on the weight of said molten polymer, of water, from about 0.5 to 20% by weight, based on the weight of said polymer, of at least one emulsifying agent having an HLB value less than 7.0, and from about 1.0 to 25% by weight, based on the weight of said polymer, of a solid hydrophilic dispersing aid, the molten polymer forming said continuous phase i. being substantially immiscible in water, ii. having a molecular weight such that its melt viscosity in the molten form is less than 2500 centipoises, iii. having a melting point higher than the boiling point of water, and iv. having a critical temperature lower than that of water; b. pressurizing the emulsion to at least an autogeneous level, during the formation of said emulsion, while at the same time maintaining the emulsion at a temperature above the melting point of the polymer, but below the critical temperature of the water; and c. discharging the emulsion through an orifice into a region of lower pressure to adiabatically vaporize substantially all of the water and violently disrupt the polymer thereby producing the subject high-surface-area fibers, the amount of water present being greater than the minimum amount necessary to cool the polymer to a temperature below the polymer melting point upon adiabatic evaporation of the emulsion.
Claim 2
Dependent Claim
269 words
A process for producing discrete polymer fibers having a surface area greater than 1.0 m 2 /g, comprising the steps of: a. forming a water-in-oil emulsion consisting essentially of a continuous phase formed of a molten crystalline fiber-forming polymer, a discontinuous phase formed of from about 15 to 45% by weight, based on the weight of said molten polymer, of water, from about 0.5 to 20% by weight, based on the weight of said polymer, of at least one emulsifying agent having an HLB value less than 7.0, and from about 1.0 to 25% by weight, based on the weight of said polymer, of a solid hydrophilic dispersing aid, the molten polymer forming said continuous phase i. being substantially immiscible in water, ii. having a molecular weight such that its melt viscosity in the molten form is less than 2500 centipoises, iii. having a melting point higher than the boiling point of water, and iv. having a critical temperature lower than that of water; b. pressurizing the emulsion to at least an autogeneous level, during the formation of said emulsion, while at the same time maintaining the emulsion at a temperature above the melting point of the polymer, but below the critical temperature of the water; and c. discharging the emulsion through an orifice into a region of lower pressure to adiabatically vaporize substantially all of the water and violently disrupt the polymer thereby producing the subject high-surface-area fibers, the amount of water present being greater than the minimum amount necessary to cool the polymer to a temperature below the polymer melting point upon adiabatic evaporation of the emulsion.
Claim 3
Dependent Claim
14 words
The process of claim 1, wherein the crystalline polymer does not degrade upon melting.
Claim 4
Dependent Claim
12 words
The process of claim 1, wherein the crystalline polymer is a polyolefin.
Claim 5
Dependent Claim
66 words
The process of claim 1, wherein the crystalline polymer is selected from the group consisting of polyolefins such as linear polyethylene, isotactic polypropylene, copolymers of ethylene and propylene, polymers of 1-butene, 1-pentene, 4-methyl, butene-1, cyclic and aryl-substituted olefins such as vinyl-cyclohexane and styrene, and crystalline copolymers and block polymers of said olefins, polyamides such as nylon-66, aliphatic and aromatic polyurethanes, and polyesters such as polyethylene terephthalate.
Claim 6
Dependent Claim
25 words
The process of claim 4, wherein the crystalline polyolefin is formed from an olefin selected from the group consisting of ethylene propylene, and mixtures thereof.
Claim 7
Dependent Claim
12 words
The process of claim 1, wherein the emulsifying agent is a stearate.
Claim 8
Dependent Claim
12 words
The process of claim 1, wherein the dispersing aid is a clay.
Claim 9
Dependent Claim
18 words
The process of claim 1, wherein the pressure employed is at least 100 psia greater than autogenous pressure.
Claim 10
Dependent Claim
25 words
The process of claim 1, wherein the molten emulsion is adiabatically flashed through the orifice into a region maintained at room temperature and atmospheric pressure.
Claim 11
Dependent Claim
11 words
The process of claim 1, wherein the polymer is linear polyethylene.
Claim 12
Dependent Claim
247 words
A process for producing discrete polymer fibers having a surface area greater than 1.0 m 2 /g, comprising: a. forming a water-in-oil emulsion consisting essentially of i. a continuous phase formed of a solid fiber-forming crystalline polymer that can form a melt without carbonization or degradation, having a molecular weight such that the viscosity in the melt is less than 2500 centipoises, having a melting point higher than the boiling point and lower than the critical temperature of water, having a heat of fusion less than the heat of vaporization of water, and being substantially immiscible in water, ii. a discontinuous phase formed of from about 15% to about 45% by weight of water, based on the weight of said polymer. iii. from about 0.5 to 20% by weight, based on the weight of said fiber-forming polymer, of at least one emulsifying agent having an HLB value less than 7.0, and iv. from about 1to 25% by weight, based on the weight of said fiber-forming polymer, of a solid hydrophilic dispersing aid; b. heating the emulsion to a temperature above the melting point of said continuous polymer phase and below the critical temperature of the discontinuous water phase; c. pressurizing the emulsion to at least an autogenous level; d. adiabatically vaporizing substantially all of the water by discharging the water-in-oil emulsion through an orifice into a region of lower pressure than previously imparted to the emulsion, causing the polymer phase to disrupt and form discrete high-surface-area fibers.
Claim 13
Dependent Claim
247 words
A process for producing discrete polymer fibers having a surface area greater than 1.0 m 2 /g, comprising: a. forming a water-in-oil emulsion consisting essentially of i. a continuous phase formed of a solid fiber-forming crystalline polymer that can form a melt without carbonization or degradation, having a molecular weight such that the viscosity in the melt is less than 2500 centipoises, having a melting point higher than the boiling point and lower than the critical temperature of water, having a heat of fusion less than the heat of vaporization of water, and being substantially immiscible in water, ii. a discontinuous phase formed of from about 15% to about 45% by weight of water, based on the weight of said polymer. iii. from about 0.5 to 20% by weight, based on the weight of said fiber-forming polymer, of at least one emulsifying agent having an HLB value less than 7.0, and iv. from about 1to 25% by weight, based on the weight of said fiber-forming polymer, of a solid hydrophilic dispersing aid; b. heating the emulsion to a temperature above the melting point of said continuous polymer phase and below the critical temperature of the discontinuous water phase; c. pressurizing the emulsion to at least an autogenous level; d. adiabatically vaporizing substantially all of the water by discharging the water-in-oil emulsion through an orifice into a region of lower pressure than previously imparted to the emulsion, causing the polymer phase to disrupt and form discrete high-surface-area fibers.
Claim 14
Dependent Claim
30 words
The process of claim 11, wherein the crystalline polymer, prior to forming said emulsion, is finely divided so that substantially all of the divided polymer will pass a 50-mesh screen.
Claim 15
Dependent Claim
20 words
The process of claim 12, wherein the dispersing aid is in finely divided form less than about 50-mesh in size.
Claim 16
Dependent Claim
22 words
The process of claim 11, wherein the emulsion components are uniformly blended prior to heating above the melting point of the polymer.
Claim 17
Dependent Claim
180 words
A process of preparing discrete polyethylene fibers comprising the steps of: a. uniformly blending to form a water-in-oil emulsion consisting essentially of i. finely divided solid linear polyethylene having a melt viscosity of less than 2500 centipoises, ii. about 0.5 to 20% by weight, based on the weight of polyethylene, of at least one emulsifying agent having an HLB value less than 7.0, iii. about 1.0 to 20% by weight, based on the weight of said polyethylene, of a solid hydrophilic dispersing aid, and, iv. about 15 to 45% by weight of water, based on the weight of polyethylene; b. heating the resultant emulsion to a temperature of between about 180° and 250° C.; c. pressurizing the resulting emulsion to a pressure at least 100 psia higher than autogenous pressure with an inert gas; and d. discharging the emulsion through an orifice into a region of reduced pressure to adiabatically vaporize substantially all of the water from the emulsion and disrupting the heated polyethylene and forming discrete polyethylene fibers having a surface area of at least 1.0 m 2 /g.
Claim 18
Dependent Claim
180 words
A process of preparing discrete polyethylene fibers comprising the steps of: a. uniformly blending to form a water-in-oil emulsion consisting essentially of i. finely divided solid linear polyethylene having a melt viscosity of less than 2500 centipoises, ii. about 0.5 to 20% by weight, based on the weight of polyethylene, of at least one emulsifying agent having an HLB value less than 7.0, iii. about 1.0 to 20% by weight, based on the weight of said polyethylene, of a solid hydrophilic dispersing aid, and, iv. about 15 to 45% by weight of water, based on the weight of polyethylene; b. heating the resultant emulsion to a temperature of between about 180° and 250° C.; c. pressurizing the resulting emulsion to a pressure at least 100 psia higher than autogenous pressure with an inert gas; and d. discharging the emulsion through an orifice into a region of reduced pressure to adiabatically vaporize substantially all of the water from the emulsion and disrupting the heated polyethylene and forming discrete polyethylene fibers having a surface area of at least 1.0 m 2 /g.
Claim 19
Dependent Claim
21 words
The process of claim 15, wherein a solid hydrophillic dispersing aid having a particle size less than about 50-mesh is employed.
Claim 20
Dependent Claim
12 words
The process of claim 15, wherein the dispersing aid is a clay.
Claim 21
Dependent Claim
12 words
The process of claim 15, wherein the dispersing aid is bentonite clay.
References Cited (Backward Citations)
US2728753A
Cited
US3703502A
Cited
US3674736A
Cited
US3808091A
Cited
US3770856A
Cited
US3774387A
Cited
US3885014A
Cited
US3730918A
Cited
US3848027A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-10-19 | 1980-04-19 | 1980-10-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-10-19 | 1984-04-19 | 1984-10-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-10-19 | 1988-04-19 | 1988-10-19 | $7700.00 | Window Closed / Lapsed |