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US4115492A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for preparing microporous polyethylene hollow fibers

Assignee: Dow Chemical Co
•
Filing: 1977-01-28
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Granted: 1978-09-19
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Expires: 1997-01-28
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Abstract

Abstract Normally hydrophobic, polyethylene hollow fibers having contiguous microporosity are prepared by extruding a heated solution of a polyethylene and an ester from a hollow fiber spinnerette, simultaneously cooling and drawing the forming fibers to a ratio of up to 40 to 1, drawing the gelled fibers to an overall ratio of from about 1.5/1 to 800/1 and then removing the ester. The maximum pore radius ranges up to about 50A, and the fibers have gas permeabilities approaching 10 -2 cc (STP) per cm 2 per second per cm. Hg. transmembrane pressure differential. A significant increase in permeability over polyethylene hollow fibers made according to the teachings of the prior art is achieved.

Inventors

  • 👤 Robert D. Mahoney
  • 👤 Stephen E. Schneider

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-04 19:54
CPC Classifications
D; D01; D01D; D01D5/00; D01D5/24; B; B01; B01D; B01D67/00; B01D67/0002; B01D67/0023; B01D67/0025; B01D67/0027; B01D67/003; B01D69/00; B01D69/08; B01D71/00; B01D71/06; B01D71/26; B01D71/261; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2913; Y10T428/2973; Y10T428/2975

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 313 words
A process for preparing a hollow fiber which consists essentially of polyethylene and is a microporous hollow fiber in which the porosity is contiguous and the O 2 gas permeability is at least 2×10 -5 cc (STP) per cm 2 per second per cm Hg transmembrane pressure differential, said process comprising: (a) providing a polyethylene/ester mixture of which about 20 to about 80 weight percent consists essentially of polyethylene and the balance consists essentially of an ester or a mixture of esters, of the formula R 1 (COOR 2 ) n , wherein n is 1 or 2, R 1 is a mono- or divalent hydrocarbon radical, optionally interrupted by one or two --O-- or --S-- links, and containing from 1 to 32 carbons, each R 2 independently is an aliphatic hydrocarbon radical of 2-26 carbon atoms or consists of two aliphatic hydrocarbon moieties joined by an --O-- or --S-- link and containing a total of from 3 to 20 carbons; (b) heating said polyethylene/ester mixture to a temperature at which it is a homogeneous liquid but below the boiling or decomposition temperature thereof, and extruding it from a spinnerette in the form of a hollow fiber; (c) cooling the issuing extrudate to solidify it while maintaining sufficient tension on the forming fiber to achieve a draw ratio of from about 1.0/1 to about 40/1; (d) at a temperature above the melting point of the ester, but at least 10° below the cloud point of said homogeneous liquid, post-spin drawing the solidified fiber under sufficient tension to achieve an overall draw ratio of from about 1.5/1 to about 800/1; and (e) contacting the post-spin drawn fiber with a liquid ester-removal medium, at a temperature intermediate of the freezing point of the medium and the flow point of the polyethylene, until at least a major proportion of the ester is removed from the fiber.
Claim 2
Dependent Claim 313 words
A process for preparing a hollow fiber which consists essentially of polyethylene and is a microporous hollow fiber in which the porosity is contiguous and the O 2 gas permeability is at least 2×10 -5 cc (STP) per cm 2 per second per cm Hg transmembrane pressure differential, said process comprising: (a) providing a polyethylene/ester mixture of which about 20 to about 80 weight percent consists essentially of polyethylene and the balance consists essentially of an ester or a mixture of esters, of the formula R 1 (COOR 2 ) n , wherein n is 1 or 2, R 1 is a mono- or divalent hydrocarbon radical, optionally interrupted by one or two --O-- or --S-- links, and containing from 1 to 32 carbons, each R 2 independently is an aliphatic hydrocarbon radical of 2-26 carbon atoms or consists of two aliphatic hydrocarbon moieties joined by an --O-- or --S-- link and containing a total of from 3 to 20 carbons; (b) heating said polyethylene/ester mixture to a temperature at which it is a homogeneous liquid but below the boiling or decomposition temperature thereof, and extruding it from a spinnerette in the form of a hollow fiber; (c) cooling the issuing extrudate to solidify it while maintaining sufficient tension on the forming fiber to achieve a draw ratio of from about 1.0/1 to about 40/1; (d) at a temperature above the melting point of the ester, but at least 10° below the cloud point of said homogeneous liquid, post-spin drawing the solidified fiber under sufficient tension to achieve an overall draw ratio of from about 1.5/1 to about 800/1; and (e) contacting the post-spin drawn fiber with a liquid ester-removal medium, at a temperature intermediate of the freezing point of the medium and the flow point of the polyethylene, until at least a major proportion of the ester is removed from the fiber.
Claim 3
Dependent Claim 54 words
The process of claim 1 in which said ester has the formula R 1 --COOR 2 , in which R 1 is a monovalent radical defined as in claim 1 and R 2 consists of two aliphatic hydrocarbon moieties joined by an --O-- link and containing a total of from 3 to 20 carbons.
Claim 4
Dependent Claim 19 words
The process of claim 1 in which R 1 is an aliphatic radical containing from 10 to 24 carbons.
Claim 5
Dependent Claim 42 words
The process of claim 1 in which said ester has the formula R 1 --COOR 2 , in which R 1 is a monovalent radical defined as in claim 1 and R 2 is an aliphatic hydrocarbon radical of 2-20 carbon atoms.
Claim 6
Dependent Claim 15 words
The process of claim 2 in which said ester is butyl stearate or 2-butoxyethyl oleate.
Claim 7
Dependent Claim 12 words
The process of claim 2 in which said ester is 2-butoxyethyl oleate.
Claim 8
Dependent Claim 32 words
The process of claim 1 in which said post-spin drawn fiber is contacted with methylene chloride or ethanol until the residual content of said solvent therein is less than 5 weight percent.
Claim 9
Dependent Claim 22 words
The process of claim 1 in which said overall draw ratio is within the range of from about 20/1 to about 500/1.

References Cited (Backward Citations)

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US3228896A Cited
US3423491A Cited
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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) 1981-09-18 1982-03-20 1982-09-19 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-09-18 1986-03-20 1986-09-19 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-09-18 1990-03-20 1990-09-19 $7700.00 Window Closed / Lapsed

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