US3738924A - Process for the solvent casting of cellulose films using radiation,and products thereof - Google Patents

Process for the solvent casting of cellulose films using radiation,and products thereof Download PDF

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Publication number
US3738924A
US3738924A US00160131A US3738924DA US3738924A US 3738924 A US3738924 A US 3738924A US 00160131 A US00160131 A US 00160131A US 3738924D A US3738924D A US 3738924DA US 3738924 A US3738924 A US 3738924A
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United States
Prior art keywords
film
dope
cellulose ester
cast
solvent
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Expired - Lifetime
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US00160131A
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English (en)
Inventor
R Williams
B Dotson
E Morrison
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Eastman Kodak Co
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Eastman Kodak Co
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    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03CPHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00Photosensitive materials
    • G03C1/76Photosensitive materials characterised by the base or auxiliary layers
    • G03C1/795Photosensitive materials characterised by the base or auxiliary layers the base being of macromolecular substances

Definitions

  • the present invention relates to improved processes for manufacturing film materials containing, as a major component, at least one lower fatty acid ester of cellulose. More particularly, this invention relates to a method for significantly increasing the maximum rates at which film materials containing such cellulose esters can be manufactured via the so-called solvent casting method or procedure.
  • the drying or curing zone must conventionally be fairly long because of the necessity to remove from the film a very large proportion (i.e., generally about percent or more) of the total amount of organic volatile solvents that had originally been present in the dope solution.
  • solvent casting processes for manufacturing films composed mainly of cellulose lower fatty acid esters can be markedly shortened in an economical way by (a) incorporating into the solvent portion of the dope an effective amount of a compatible organic monomer (which not only can serve as a solvent or co-solvent for the cellulose ester film former in the dope, but also can be polymerized via a free radical procedure) and (b) subjecting the layer of cast dope, While it remains on the coating web and before it has developed sufiicient integral strength to be satisfactorily strippable, to a sufficient amount of ionizing radation to cause the free radical polymerization of the monomer(s) in the cast layer, said amount of ionizing radiation being less than that which causes the cellulose ester in the cast layer to degrade excessively.
  • a compatible organic monomer which not only can serve as a solvent or co-solvent for the cellulose ester film former in the dope, but also can be polymerized via a free radical procedure
  • This amoun of ionizing radiation will preferably be from about 0.3 to about 10 megarads. Still further preferred dosage, in the presence of sensitizers, for example, is from about 0.5 to about 3 megarads.
  • An additional advantage that can result from practicing the present improved processes is that relatively smaller amounts of organic solvent-(s) need be recovered from the drying and curing steps, thereby resulting in less total demand upon solvent collection and purification equipment (which presently represent a large necessary investment in conjunction with the conventional film solvent casting equipment described above).
  • the compatible monomers referred to above are those well-known organic compounds
  • Typical non-limiting examples of such compatible monomers are the lower alkyl acrylics such as methyl methacrylate, ethyl acrylate, ethyl methacrylate, acrylonitrile, butylene dimethacrylates, ethylene glycol dimethacrylate, and the like, as well as other unsaturated monomers such as acrylic acid, acrylamide, diacetone acrylamide, diallyl phthalates, styrene, vinyl acetate, vinyl butyrate, and the like.
  • lower alkyl acrylics such as methyl methacrylate, ethyl acrylate, ethyl methacrylate, acrylonitrile, butylene dimethacrylates, ethylene glycol dimethacrylate, and the like
  • unsaturated monomers such as acrylic acid, acrylamide, diacetone acrylamide, diallyl phthalates, styrene, vinyl acetate, vinyl butyrate, and the like.
  • the polymeric products that result from practicing the processes of this invention are apparently copolymeric in nature, (rather than a simple admixture of cellulose ester and polymerized monomers, as would be expected), involving the apparent multiple grafting of polymerized monomer to the cellulosic material.
  • the products that result from practicing the present processes have unique and unexpected properties. For example, practically none of the polystyrene portion can be extracted from the film product from Example I, below even after prolonged treatment in boiling toluene.
  • the compatible monomer(s) that are used in the formulation of the various cellulose ester dopes should generally be present in the solvent fraction of the dopes (i.e., that portion that can be evaporated from the dopes in a circulating air oven at a temperature of 105 C. and at atmospheric pressure) in an amount equal to at least about 5 weight percent and will preferably represent from about 15 to about 80 weight percent of said volatile solvent fraction.
  • the compatible monomers should be used in amounts equal to at least about weight percent of the cellulose esters in these compositions, but should not be used in amounts higher than twice the amount of cellulose ester(s) in the present dope compositions.
  • the ratio of total compatible monomers to total cellulose ester(s) in the dope should be at most about 1 to 1, respectively, by weight.
  • the remainder of the solvent fraction can contain any desired volatile, non-polymerizable organic solvent or blend of volatile non-polymerizable organic solvents that have conventionally been employed in cellulose ester dopes heretofore. This includes, but is not limited to methanol, ethanol, isopropanol, n-propanol, butanol, methylene chloride, cyclohexane, ethylene dichloride, chloroform, and the like. As is well known in the art, sometimes blends of such solvents are more desirable in certain formulations to yield completely clear dopes.
  • the dissolved (non-volatile at 105 C.) fraction of the initial dope compositions of the present invention should consist essentially of one or more of the film-forming lower fatty acid cellulose esters described heretofore, and can also contain a relatively smaller amount [up to about 25 weight percent, based on the combined weights of plasticizer(s) and cellulose ester(s) in the dope of one (or a blend) of those materials that are known to plasticize the cellulose ester film], as well as colorants such as dyes, anti-oxidants, and stabilizers.
  • plasticizers for cellulose ester films are triphenylphosphate, methoxyethyl phthalate, diallyl phthalate (a polymerizable plasticizer), and the like. This dissolved fraction represents at least about 10 weight percent of the present dope compositions, but preferably should represent from about 15 to about 35 weight percent of the dope compositions.
  • Typical examples of the types of ionizing radiation that can be used in the successful practice of this invention include high energy electrons (see Industrial Radiation Cured Coatings Speed Product Finishing by John A. Mock, Material Engineering, October 1970, pp. 56 through 59), beta particles, gamma rays, X-rays, positive ions such as alpha particles, and ionizing radiation from decomposing radioactive materials such as radioactive cobalt, for example.
  • the particular physical manner whereby the ionizing radiation is applied to the dope layers in the practice of this invention is not critical.
  • the radiation should be of sufficient intensty or strength to penetrate through the entre thickness of the cast dope layer. Thus, it is preferred that at least half of the ionizing radiation be strong enough to pass completely through the cast dope layer.
  • the particular source of the ionizing radiation that causes the polymerization of a substantial proportion of the compatible monomer in the dope compositions of this invention is not critical, so long as the dosage level at the cast dope layer is at least about 0.3 megarads.
  • the ionizing radiation must be directed onto the cast dope layer while the layer remains on the initial casting Web.
  • a high enegy electron beam can be directed onto the dope layer shortly, or practically immediately, after the dope layer is cast, thereby causing an immediate, very large increase in the integral strength of the layer and enabling the partially cured layer to be stripped successfully from the wheel in a much shorter time than would otherwise be possible without undesirable pickoff.
  • the ionizing radiation should be applied to the wet dope layer within about three minutes of the time the layer is cast into the Web.
  • EXAMPLE 1 Ten parts of cellulose acetate (containing 43.5% acetyl and having an intrinsic viscosity of 2.40 at 25 C. in a :10 blend of methylene chloride and methanol, respectively) are dissolved in 50 parts of a 90:10 blend of methylene chloride and methanol. Twenty parts of a solution containing equal amounts of styrene monomer and the same solvent blend are then mixed with the solution of cellulose ester. The resulting dope contains equal amounts of cellulose acetate and styrene monomer. This dope is then coated at room temperature on a glass plate to a thickness of 7 mils.
  • Example 1 Percent elongation 3.8 Modulus (10 p.s.i.) 5.3 Tear (grams) 13
  • Example 1 is repeated using 1,3-butylene dimethacrylate as the monomer in place of the styrene monomer.
  • the resulting dried/cured film has the following properties:
  • step (c) thereafter stripping said partially dried film from said web and passing said partially dried film through a drying zone to thereby remove at least half of the organic solvent material remaining in said partially dried film; the improvement which comprises (i) incorporating into said solvent portion at least about 5 weight percent of a soluble, compatible unsaturated monomer, and (ii) subjecting said wet film to ionizing radiation in an amount equal to at least about 0.3 megarad prior to step (c); said compatible unsaturated monomer having a molecular weight of at most about 300 and being capable of free radical polymerization.
  • cellulose lower fatty acid ester is selected from the group consisting of cellulose acetate, cellulose acetate butyrate, cellulose acetate propionate, and cellulose butyrate film formers having intrinsic viscosities of at least about 1.
  • a clear film product containing at least about 50 weight percent of lower fatty acid ester of cellulose and at least about 10 weight percent of polymerized compatible monomer unsaturated copolymerized therewith; said film product having been manufactured according to the process of claim 1.
  • a film product as in claim 11, wherein said polymerized compatible unsaturated monomer is polystyrene.
  • a film product as in claim 11, wherei said polymerized compatible unsaturated monomer is poly(methylmethacrylate) 14.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Polymerisation Methods In General (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Moulding By Coating Moulds (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Graft Or Block Polymers (AREA)
US00160131A 1971-07-06 1971-07-06 Process for the solvent casting of cellulose films using radiation,and products thereof Expired - Lifetime US3738924A (en)

Applications Claiming Priority (1)

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US16013171A 1971-07-06 1971-07-06

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US3738924A true US3738924A (en) 1973-06-12

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Country Status (6)

Country Link
US (1) US3738924A (show.php)
JP (1) JPS5510618B1 (show.php)
CA (1) CA959188A (show.php)
DE (1) DE2233027C3 (show.php)
FR (1) FR2144818B1 (show.php)
GB (1) GB1381762A (show.php)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3878139A (en) * 1972-01-31 1975-04-15 Nippon Paint Co Ltd Acrylate and styrene graft copolymers of mercapto-group-containing cellulose derivatives and coating composition containing same
US4057657A (en) * 1973-12-13 1977-11-08 John Lyndon Garnett Curable pre-polymer compositions, method of making and method of coating articles therewith
US5686036A (en) * 1996-01-11 1997-11-11 Eastman Kodak Company Process for making a cellulose triacetate photographic film base
US20060130227A1 (en) * 2002-01-30 2006-06-22 Belford Gary P Arm rest massage feature for whirlpool tubs

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI66624C (fi) * 1983-11-02 1984-11-12 Neste Oy Foerfarande foer framstaellning av cellulosakarbamatfibrer eller -filmer

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3878139A (en) * 1972-01-31 1975-04-15 Nippon Paint Co Ltd Acrylate and styrene graft copolymers of mercapto-group-containing cellulose derivatives and coating composition containing same
US4057657A (en) * 1973-12-13 1977-11-08 John Lyndon Garnett Curable pre-polymer compositions, method of making and method of coating articles therewith
US5686036A (en) * 1996-01-11 1997-11-11 Eastman Kodak Company Process for making a cellulose triacetate photographic film base
US20060130227A1 (en) * 2002-01-30 2006-06-22 Belford Gary P Arm rest massage feature for whirlpool tubs

Also Published As

Publication number Publication date
GB1381762A (en) 1975-01-29
FR2144818A1 (show.php) 1973-02-16
FR2144818B1 (show.php) 1974-12-27
DE2233027C3 (de) 1974-10-03
JPS5510618B1 (show.php) 1980-03-18
CA959188A (en) 1974-12-10
DE2233027A1 (de) 1973-01-25
DE2233027B2 (de) 1974-02-21

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