US2758943A - Process of superficially saponifying a strip of cellulose ester - Google Patents
Process of superficially saponifying a strip of cellulose ester Download PDFInfo
- Publication number
- US2758943A US2758943A US481714A US48171455A US2758943A US 2758943 A US2758943 A US 2758943A US 481714 A US481714 A US 481714A US 48171455 A US48171455 A US 48171455A US 2758943 A US2758943 A US 2758943A
- Authority
- US
- United States
- Prior art keywords
- strip
- aqueous
- fatty acid
- baths
- treatment
- 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 - Lifetime
Links
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/76—Photosensitive materials characterised by the base or auxiliary layers
- G03C1/795—Photosensitive materials characterised by the base or auxiliary layers the base being of macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/22—Post-esterification treatments, including purification
- C08B3/24—Hydrolysis or ripening
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
- Y10T428/2495—Thickness [relative or absolute]
Definitions
- This invention relates to an improved method of making cellulosic and more particularly to cellulosic films which are to be subsequently impregnated with ig se itive system containing'a di'afzoniumcompound, and is 'a division of our 'co-pen'ding application, ,Ser. No; 230,- I-2 45,1fi1ed June 6, 19 1, new U Pat n No- 2,704,262.
- One of theafter-treatments containsan anti-peeling agent which shrinksan'int'ermg diate partially 'saponified layer such that upon subsequent immersion of the strip in an aqueous solution, for instance when impregnating the strip with 'a water-soluble lightsensitive system no stresses are created in the saponified layer which would cause it to peel from the underlying unsaponified portion of the strip.
- the invention is particularly applicable to cellulose diesters which are subject to peeling after saponification.
- a fatty ester of cellulose containing more than 1.5 and less than 3.0 fatty acid radicals per glucose residue after superficial saponification i. e. by immersion of a strip of this material in a saponifying bath for a given period of time to saponify at least one side of the strip to a desired depth, is immersed in a bath containing an anti-peeling agent which is capable of shrinking a layer intermediate the outer surface of the strip and the unsaponified portion of the strip which contains 0.5 to 1.5 fatty acid radicals per glucose residue.
- Anti-peeling agents suitable for the aforesaid purposes are: primary saturated alcohols having a main chain of from 4 to 11 carbon atoms, such as butanol-l; a mixture of about one part of butanol-l and about one part of either benzene or toluene; a mixture of about one part of butanol-l and about one part of tetrahydronaphthalene; a mixture of about one part of butanol-l and about one part of diethyl ether; a solution of about 1.5 n phosphoric acid and butanol-l.
- salt of a 'sulphated hy droxycarbdni c acid having at least 10 carbon atoms for example, nium'or sodiunisalts of ricinolic acid 'esterified with s'ul ⁇ phu iC a id, in additionsodium oleate, the sodium s'altof pfoctylbenzenesulphonic acid, cationegenou's dispersion agents such as dodecylaminehydrochloride or compo nds derived therefrom and in addition nc'm-ion forming persion agentasuch as polyethers, derived from methylene for ethylene oxide, which at the end of the chain,'ar e eisterified, for example, witha lauryl alcohol.
- nc'm-ion forming persion agenta such as polyethers, derived from methylene for ethylene oxide, which at the end of the chain,'ar e eisterified
- An after-treatment bath may contain both an antipeeling ag'ent for partially esterified cellulose containing from 0.5 to 1.5 radicals of fattyacid per glucose residue and a solvent for the plasticiser. It must be noted that'ja great number of non-ion-form'ing shrinking a'gent's'also have a dissolvingefiect on plasticisers. l
- the thickness of the regenerated cellulose layer is 10 n and that of the intermediate layer 4 ,u.
- the adhesion of the saponified layer to the non-saponified substratum is excellent.
- the butanol-toluene mixture may be replaced with equally satisfactory results by a mixture of butanol-l with benzene or with tetrahydronaphthalene or with diethyl-ether.
- Example II A web ,u. thick and made of cellulose acetate having an acetic acid content of 53.3% is passed mechanically at 23.5 C. at the rate of 60 seconds per bath in succession through the following baths:
- the web is then sprayed with water for 30 seconds and after skimming at 90 C. dried with a warm flow of air.
- the thickness of the regenerated cellulose layer is a and that of the intermediate layer 3
- the adhesion of the saponified layer to the substratum is excellent.
- the concentration of phosphoric acid should not be excessive since otherwise the surface of the saponified layer, which in itself is readily adhesive, tends to become slightly shrivelled.
- a process of superficially saponifying a strip of cellulose ester containing between 1.5 and 3.0 radicals of fatty acid per glucose residue which comprises the steps of immersing said strip in a saponifying bath containing at least 0.1 normal solution of an alkali hydroxide and an alcoholic solvent to effect rapid saponification of said strip for a time sufficient to produce a partially saponified layer in said strip containing between 0.5 and 1.5 fatty acid radicals per glucose residue, and thereafter immersing said strip for at least 45 seconds in butanol-l.
- a process of superficially saponifying a strip of cellulose ester containing between 1.5 and 3.0 radicals of fatty acid per glucose residue which comprises the steps of immersing said strip in a saponifying bath containing at least 0.1 normal solution of an alkali hydroxide and I,
- a process of superficially saponifying a strip of cellulose ester containing between 1.5 and 3.0 radicals of fatty acid per glucose residue which comprises the steps of immersing said strip in a saponifying bath containing at least 0.1 normal solution of an alkali hydroxide and an alcoholic solvent to effect rapid saponification of said strip for a time sufiicient to produce a partially saponified intermediate layer in said strip containing between 0.5 and 1.5 fatty acid radicals per glucose residue, and thereafter immersing said strip for at least 45 seconds in a mixture of about one part of butanol-l and about one part of tetrahydronaphthalene.
- a process of superficially saponifying a strip of cellulose ester containing between 1.5 and 3.0 radicals :of fatty acid per glucose residue which comprises the steps of immersing said strip in a saponifying bath containing at least 0.1 normal solution of an alkali hydroxide and an alcoholic solvent to effect rapid saponification of said strip for a time sufiicient to produce a partially saponified intermediate layer in said strip containing between 0.5 and 1.5 fatty acid radicals per glucose residue, and thereafter immersing said strip for atleast 45 seconds in a mix-v ture of about one part of butanol-l and about one part of diethyl ether.
- a process of superficially saponifying a strip of cellulose ester containing between 1.5 and 3.0 radicals of fatty acid per glucose residue which comprises the steps of immersing said strip in a saponifying bath containing at least 0.1 normal solution of an alkali hydroxide and an alcoholic solvent to efiect rapid saponification of said strip for a time sufficient to produce a partially saponified intermediate layer in said strip containing between 0.5 and 1.5 fatty acid radicals per glucose residue, and thereafter immersing said strip for at least seconds in a solution of about 1.5 n phosphoric acid in butanol-l.
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- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- General Physics & Mathematics (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BE503729D BE503729A (fr) | 1950-06-06 | ||
NL76311D NL76311C (fr) | 1950-06-06 | ||
GB13077/51A GB696103A (en) | 1950-06-06 | 1951-06-01 | Improvements in or relating to methods of producing superficially saponified films or the like of fatty acid cellulose esters |
FR1045757D FR1045757A (fr) | 1950-06-06 | 1951-06-04 | Procédé de fabrication de feuilles, pellicules et articles analogues saponifiés superficiellement |
US230245A US2704262A (en) | 1950-06-06 | 1951-06-06 | Method of superficially saponifying a cellulose ester film |
US481714A US2758943A (en) | 1950-06-06 | 1955-01-13 | Process of superficially saponifying a strip of cellulose ester |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NL696103X | 1950-06-06 | ||
US230245A US2704262A (en) | 1950-06-06 | 1951-06-06 | Method of superficially saponifying a cellulose ester film |
US481714A US2758943A (en) | 1950-06-06 | 1955-01-13 | Process of superficially saponifying a strip of cellulose ester |
Publications (1)
Publication Number | Publication Date |
---|---|
US2758943A true US2758943A (en) | 1956-08-14 |
Family
ID=32303331
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US481714A Expired - Lifetime US2758943A (en) | 1950-06-06 | 1955-01-13 | Process of superficially saponifying a strip of cellulose ester |
Country Status (5)
Country | Link |
---|---|
US (1) | US2758943A (fr) |
BE (1) | BE503729A (fr) |
FR (1) | FR1045757A (fr) |
GB (1) | GB696103A (fr) |
NL (1) | NL76311C (fr) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3078178A (en) * | 1960-03-02 | 1963-02-19 | Polaroid Corp | Method of hydrolizing and polishing surface of cellulose ester substrate and photographic product produced therefrom |
US3969541A (en) * | 1971-03-26 | 1976-07-13 | Fuji Photo Film Co., Ltd. | Diffusion transfer image receptive materials |
US20100316861A1 (en) * | 2006-10-30 | 2010-12-16 | Lofo High Tech Film Gmbh | Plasticizer for protective films |
-
0
- BE BE503729D patent/BE503729A/xx unknown
- NL NL76311D patent/NL76311C/xx active
-
1951
- 1951-06-01 GB GB13077/51A patent/GB696103A/en not_active Expired
- 1951-06-04 FR FR1045757D patent/FR1045757A/fr not_active Expired
-
1955
- 1955-01-13 US US481714A patent/US2758943A/en not_active Expired - Lifetime
Non-Patent Citations (1)
Title |
---|
None * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3078178A (en) * | 1960-03-02 | 1963-02-19 | Polaroid Corp | Method of hydrolizing and polishing surface of cellulose ester substrate and photographic product produced therefrom |
US3969541A (en) * | 1971-03-26 | 1976-07-13 | Fuji Photo Film Co., Ltd. | Diffusion transfer image receptive materials |
US20100316861A1 (en) * | 2006-10-30 | 2010-12-16 | Lofo High Tech Film Gmbh | Plasticizer for protective films |
Also Published As
Publication number | Publication date |
---|---|
GB696103A (en) | 1953-08-26 |
NL76311C (fr) | |
FR1045757A (fr) | 1953-12-01 |
BE503729A (fr) |
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